CN105321726B - High magnification active carbon/Activated Graphite alkene combination electrode material and preparation method thereof - Google Patents
High magnification active carbon/Activated Graphite alkene combination electrode material and preparation method thereof Download PDFInfo
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- CN105321726B CN105321726B CN201410348689.7A CN201410348689A CN105321726B CN 105321726 B CN105321726 B CN 105321726B CN 201410348689 A CN201410348689 A CN 201410348689A CN 105321726 B CN105321726 B CN 105321726B
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Abstract
The present invention relates to a kind of high magnification active carbon/Activated Graphite alkene hybrid supercapacitor electrode materials and preparation method thereof.It is characterized by: evenly spreading to active carbon in the graphene oxide solution containing activator; heating removes moisture therein; then obtained mixture is restored and is activated at a certain temperature in protective atmosphere; finally product is washed again, filtered and is dried, obtains active carbon/Activated Graphite alkene combination electrode material.Active carbon provided by the present invention/Activated Graphite alkene combination electrode material has high specific capacity and excellent high rate performance, and specific capacitance is stablized in 250F/g in the current density range of 2~10A/g.And the active carbon/Activated Graphite alkene composite material preparation method has many advantages, such as that technical process is simple, time saving, at low cost and be easily achieved large-scale industrial production.
Description
Technical field
The present invention relates to electric chemical super capacitor technical fields, and in particular to a kind of high magnification active carbon/Activated Graphite
Alkene hybrid supercapacitor electrode material and preparation method thereof.
Background technique
Supercapacitor (Supercapacitor), also known as electrochemical capacitance (ultracapacitor), electrochemical capacitor
(Electrochemical Capacitor, EC), electric chemical super capacitor (Electrochemical
Supercapacitor), it is a kind of new type of energy storage device, can completes to charge in seconds.Furthermore supercapacitor also has
There is the features such as output power density is high, operating temperature range is wide, has extended cycle life, is economic and environment-friendly.Supercapacitor is renewable
There are huge application value and market potential in the fields such as using energy source, traffic, electric power, communication, national defence.Especially wind-force, light
Volt power generation and the rise of electric vehicle are so that the research and development of this novel energy-storing technology of supercapacitor are paid more and more attention.
Graphene (graphene) be one kind by carbon atom with sp2The hexangle type honeycomb crystal lattice structure of hybridized orbit composition
Crystal, it is considered to be the basic structural unit of fullerene, carbon nanotube and graphite.Graphene has unique physical characteristic,
As (theoretical specific surface area is up to 2630m to higher specific surface area2/ g) and very high conductivity (resistivity is about 10-6Ω·
cm).Graphene is a kind of energy storage material with broad prospect of application, as graphene-based material may be used as supercapacitor
Electrode material.The preparation method of graphene has micromechanics stripping method, surface growth method (epitaxial growth, vapor deposition etc.), chemistry
Stripping method, chemical synthesis (organic precursor synthesis and solvent-thermal process) etc..Wherein chemical synthesis is most adapted on a large scale
Produce grapheme material.It is most importantly chemical reduction method in chemical synthesis, for example is carried out using strong reductants such as hydrazine hydrates
Reduction, high-temperature heating reduction, microwave irradiation reduction, electrochemical reduction etc., can obtain with high conductivity high-specific surface area
Grapheme material.
Although the theoretical specific surface area of graphene is very high, since piece stacking is stamped, the specific surface of the graphene of chemical method preparation
Product is relatively low as the attainable specific capacitance of electrode material for super capacitor institute well below theoretical value.It lives to graphene
Change processing, can increase substantially its specific surface area and specific capacitance.
Currently, the preparation method of Activated Graphite alkene has physical activation method and chemical activation method, physical activation method is in high temperature
Under, under the effect of the catalyst, carbon therein reacts graphene raw material with oxidizing gas, part carbon gasification and be made have height
The Activated Graphite alkene of specific surface area.Common activator has alkali metal, iron, carbonate etc..Chemical activation method is in activator
Under effect, hydrogen or oxygen in graphene raw material are partly or entirely removed, while carrying out carbonization-activation to it.Common activator
There are phosphoric acid, zinc chloride, potassium hydroxide or part heavy metal.
Absorbent charcoal material has that production cost is low, manufacturing process is simple and the advantages such as large specific surface area.Due to electric conductivity compared with
Difference, the chemical property of commercial activated charcoal can with the increase of current density rapid decay.Regardless of be in water system or
In organic system electrolyte solution, the high conductivity of Activated Graphite alkene material, high-specific surface area, height ratio capacity, high rate capability
Etc. characteristics be a kind of good supplement to absorbent charcoal material.Active carbon and Activated Graphite alkene are carried out compound to improve electricity
The specific capacitance value of pole material, and composite material exhibits can be made to go out high high rate performance.
By the end of currently, the research of active carbon and Activated Graphite alkene Material cladding is less.Only about active carbon and graphite
The compound report of alkene.According to the literature, Zhang Kai et al. utilizes the method for collosol and gel by graphene and phenolic resin-based activated carbon
In-situ reaction is carried out to prepare active carbon/graphene combination electrode material.And the sol-gel process that it is used takes a long time, institute
It is serious with the carbonization process environmental pollution of carbon source.In addition, compound there are also active carbon is prepared with graphene progress mechanical mixture
The report of electrode material, but using the method it is difficult to ensure that graphene is in the evenly dispersed of activated carbon surface.
The present invention is intended to provide a kind of method being modified with Activated Graphite alkene to merchandise active carbon.The characteristics of this method
It is that active carbon is mixed with graphene oxide and activator first, then realizes the reduction, work of wherein graphene oxide at high temperature
Change and its compound with absorbent charcoal material.The active carbon/Activated Graphite alkene hybrid supercapacitor electrode material preparation method
Have the advantages that technical process is simple, time saving, at low cost and be easily achieved large-scale industrial production.
Summary of the invention
The object of the present invention is to provide a kind of high magnification active carbon/Activated Graphite alkene hybrid supercapacitor electrode material and
Preparation method.This active carbon/Activated Graphite alkene composite material exhibits go out the high rate performance more excellent than conventional carbon,
It is mixed using active carbon with graphene oxide and activator and graphene oxide therein is restored and activated at high temperature
Method prepared.
The present invention specifically provides a kind of high magnification active carbon/Activated Graphite alkene hybrid supercapacitor electrode material,
Be characterized in that: in protective atmosphere, by the mixture of active carbon, graphene oxide and activator under certain temperature range into
Row reduction and activation, then product is washed again, filtered and is dried, obtain active carbon/Activated Graphite alkene combination electrode material
Material, wherein activator is one or both of the concentrated sulfuric acid, concentrated phosphoric acid.
High magnification active carbon of the present invention/Activated Graphite alkene hybrid supercapacitor electrode material preparation method,
It is characterized in that, includes the following steps:
(1) graphite oxide is prepared using chemical method, then obtained graphite oxide is distributed in strong acid solution, and carries out
Ultrasonic treatment, obtains graphene oxide dispersion；The chemical method is Brodie method, Staudenmaier method or Hummers
Method；When preparing graphite oxide using Hummers method, it is not necessary that obtained graphite oxide is separated from reaction system, but
Directly it is ultrasonically treated, obtains graphene oxide dispersion.The remaining concentrated sulfuric acid can be in graphene oxide dispersion
It is directly used as activator.When preparing graphite oxide using other methods, graphite oxide need to be distributed to from water, add work
Agent, ultrasonic treatment, obtains graphene oxide dispersion.The activator is one or both of the concentrated sulfuric acid, concentrated phosphoric acid.
The ultrasonic time is 1~10h (preferably 8h).
(2) active carbon is added in above-mentioned graphene oxide dispersion, is sufficiently stirred, obtain active carbon/graphite oxide
Alkene dispersion liquid；Wherein, the quality of the active carbon and graphene oxide is 100:1~1:100 (preferably 1:1) than range；Stirring
Time is 0.5~10h (preferably 6h).
(3) solvent in active carbon/graphene oxide dispersion is removed, active carbon/graphene oxide/strong acid mixing is obtained
Object；Wherein, the method for the solvent in the removal active carbon/graphene oxide dispersion are as follows: by active carbon/graphene oxide point
Dispersion liquid toasts 0.5~48h under heat lamp, or in drying box dry 0.5 at 30~150 DEG C~for 24 hours.
(4) in an inert atmosphere, active carbon/graphene oxide/strong acid mixture is heated to certain temperature and keeps the temperature one
The fixed time is restored and is activated, and graphene oxide therein is reduced sufficiently, and reduzate graphene is by strong acid
It is activated, obtains powerful active carbon/Activated Graphite alkene hybrid supercapacitor electrode material head product.Wherein inert gas
Are as follows: one of nitrogen, helium and argon gas are a variety of, and inert gas flow velocity is 40~500mlmin-1.Reduction and activation temperature
100~1000 DEG C (preferably 100~800 DEG C), reduction is 0.5~12h with activation time.
(5) obtained reduction washed with activation products, filtered, dried, it is compound to obtain active carbon/Activated Graphite alkene
Electrode material, cleaning fluids are deionized water, and washing standard is that the pH of filtrate is 6~7, and drying temperature is 30~150 DEG C (excellent
It is selected as 100~150 DEG C).
Advantages of the present invention: active carbon provided by the invention/Activated Graphite alkene hybrid supercapacitor electrode material has
Higher specific capacity and better than traditional activated carbon electrode material high rate performance (in the current density range internal ratio electricity of 2~10A/g
Hold and stablize in 250F/g).Activated Graphite alkene with height ratio capacity, high stability energy is introduced into absorbent charcoal material, the two
Synergistic effect can be also generated, its high rate performance can be improved by a relatively large margin on the basis of improving active carbon specific capacity.Therefore,
Active carbon and the progress of Activated Graphite alkene is compound, unique electrochemical capacitor characteristic of two kinds of materials can be enable to give full play to.
Active carbon of the present invention/Activated Graphite alkene composite material preparation method, have technical process it is simple, it is time saving, at low cost and
The advantages that being easily achieved large-scale industrial production.
Detailed description of the invention
Fig. 1 is active carbon/Activated Graphite alkene composite material XRD diagram prepared by the embodiment of the present invention 1；
Fig. 2 is the super electricity that the active carbon/Activated Graphite alkene composite material prepared with the embodiment of the present invention 1 does active material
The cyclic voltammetry curve figure of container electrode；
Fig. 3 is the super electricity that the active carbon/Activated Graphite alkene composite material prepared with the embodiment of the present invention 1 does active material
The electrochemical impedance spectroscopy of container electrode；
Fig. 4 is the super electricity that the active carbon/Activated Graphite alkene composite material prepared with the embodiment of the present invention 1 does active material
The constant current charge-discharge curve of container electrode；
Fig. 5 be 1 process of the embodiment of the present invention after obtained electrode material and active carbon multiplying power property curve；
Fig. 6 is active carbon/Activated Graphite alkene composite material cyclic voltammetry curve figure prepared by the embodiment of the present invention 2；
Fig. 7 is active carbon/Activated Graphite alkene composite material constant current charge-discharge curve graph prepared by the embodiment of the present invention 3；
Fig. 8 is active carbon/Activated Graphite alkene composite material cyclic voltammetry curve figure prepared by the embodiment of the present invention 4.
Specific embodiment
The following examples will be further described the present invention, but not thereby limiting the invention.
Embodiment 1
The concentrated sulfuric acid that the powdered graphite of 0.3681g325 mesh and 0.184g sodium nitrate powder are evenly spread to 9.57ml is molten
In liquid, 2h is stirred to obtain evenly dispersed mixture solution.Notice that this process will carry out in ice bath or ice-water bath, to prevent
The mixture temperature is excessively high.1.1g is slowly added into the above-mentioned evenly dispersed sulfuric acid solution for having powdered graphite and sodium nitrate powder
Then 17.68ml deionized water is added to form suspension in potassium permanganate powder into above-mentioned suspension again.Heat the suspension
35 DEG C and 98 DEG C of pyroreaction stages are subjected to, graphite oxide is finally obtained.Without by obtained graphite oxide from reactant
It is separated, but is directly added it in 250ml beaker in system, measured 100ml distilled water with graduated cylinder and pour into wherein, then
Ultrasonic 8h is carried out to it, obtains graphene oxide dispersion, then to the activity that 14.715g is added in graphene oxide dispersion
Charcoal is mixed, and mixed liquor is dried after mixing evenly.Desciccate is warming up to 400 DEG C in a nitrogen atmosphere to be gone back
Original activation keeps the temperature 6h, and obtained head product is washed (pH=6~7) after cooling, is filtered, dry, final product is obtained.
Above-mentioned final product saves, the test for chemical property after dry in 100 DEG C of air dry oven.It is living
Test results are shown in figure 1 by property charcoal/Activated Graphite alkene composite powder XRD.XRD test result shows graphene oxide
It is reduced and activates, active carbon/Activated Graphite alkene is compound.By composite material according to active material: conductive agent: binder=
The ratio of 85:10:5 is mixed, and electrode slice is made, and cyclic voltammetry, test knot are then carried out in 6M KOH electrolyte
Fruit is as shown in Figure 2.100mV/s sweep speed under, the cyclic voltammetry curve shape of the electrode illustrates still close to rectangle using this hair
It is special that active carbon/Activated Graphite alkene composite material of bright method preparation still shows good capacitor under this potential scan rate
Property.Ac impedance measurement shown in Fig. 3 shows that the electrode has lower ohmmic drop.Constant current charge-discharge the result shows that active carbon/
Activated Graphite alkene combination electrode material has height ratio capacity (Fig. 4).Specific capacitance of the composite material under the current density of 0.05A/g
Up to 332.77F/g, the specific capacitance under the current density of 5A/g reaches 243.42F/g.Fig. 5 is shown using galvanostatic charge/discharge
Test obtained active carbon/Activated Graphite alkene combination electrode material multiplying power property curve.From figure it is found that compared with active carbon,
Composite material is with the increase of discharge current density, and specific capacitance decline is slowly.Especially when current density is improved from 2000mA/g
When to 6000mA/g, the specific capacitance of composite material illustrates active carbon/Activated Graphite prepared by the present embodiment almost without reduction
Alkene has excellent high rate performance.
Embodiment 2
The made graphite oxide of embodiment 1 is added in 250ml beaker, 100ml distilled water is measured with graduated cylinder and pours into wherein,
Then ultrasonic 8h is carried out to it, obtains graphene oxide dispersion, then to addition 8.645g in graphene oxide dispersion
Active carbon is mixed, and mixed liquor is dried after mixing evenly.Desciccate is warming up in a nitrogen atmosphere 400 DEG C into
Row reduction activation keeps the temperature 6h, and obtained head product is washed (pH=6~7), filtering, drying after cooling, is finally produced
Object.
Above-mentioned final product saves, the test for chemical property after dry in 100 DEG C of air dry oven.It will
Composite material is according to active material: conductive agent: binder=85:10:5 ratio is mixed, and electrode slice is made, then in 6M
Cyclic voltammetry is carried out in KOH electrolyte, test results are shown in figure 6.100mV/s sweep speed under, the circulation of the electrode
Volt-ampere curve shape illustrates the active carbon/Activated Graphite alkene composite material prepared using the method for the present invention herein still close to rectangle
Good capacitance characteristic is still shown under potential scan rate.Constant current charge-discharge test is the result shows that active carbon/Activated Graphite alkene
Combination electrode material has height ratio capacity, high rate capability, and specific capacitance of the composite material under the current density of 5A/g reaches
206.04F/g。
Embodiment 3
The made graphite oxide of embodiment 1 is added in 250ml beaker, 100ml distilled water is measured with graduated cylinder and pours into wherein,
Then ultrasonic 8h is carried out to it, obtains graphene oxide dispersion, then to addition 4.095g in graphene oxide dispersion
Active carbon is mixed, and mixed liquor is dried after mixing evenly.Desciccate is warming up in a nitrogen atmosphere 400 DEG C into
Row reduction activation keeps the temperature 6h, and obtained head product is washed (pH=6~7), filtering, drying after cooling, is finally produced
Object.
Above-mentioned final product saves, the test for chemical property after dry in 100 DEG C of air dry oven.It will
Composite material is according to active material: conductive agent: binder=85:10:5 ratio is mixed, and electrode slice is made, then in 6M
Constant current charge-discharge test is carried out in KOH electrolyte, test results are shown in figure 7.Constant current charge-discharge is the result shows that active carbon/activity
Graphene combination electrode material has height ratio capacity, and specific capacitance of the composite material under the current density of 5A/g reaches 193.61F/g.
100mV/s sweep speed under, the cyclic voltammetry curve shape of the electrode still close to rectangle, illustrate using the method for the present invention preparation
Active carbon/Activated Graphite alkene composite material capacitance characteristic under this potential scan rate is good.
Embodiment 4
The made graphite oxide of embodiment 1 is added in 250ml beaker, 100ml distilled water is measured with graduated cylinder and pours into wherein,
Then ultrasonic 8h is carried out to it, obtains graphene oxide dispersion, then to addition 2.575g in graphene oxide dispersion
Active carbon is mixed, and mixed liquor is dried after mixing evenly.Desciccate is warming up to 400 DEG C of guarantors in a nitrogen atmosphere
Warm 6h carries out reduction activation, and obtained head product is washed (pH=6~7), filtering, drying after cooling, is finally produced
Object.
Above-mentioned final product saves, the test for chemical property after dry in 100 DEG C of air dry oven.It will
Composite material is according to active material: conductive agent: binder=85:10:5 ratio is mixed, and electrode slice is made, then in 6M
Cyclic voltammetry is carried out in KOH electrolyte, test results are shown in figure 8,100mV/s sweep speed under, the circulation of the electrode
Volt-ampere curve shape illustrates the active carbon/Activated Graphite alkene composite material prepared using the method for the present invention herein still close to rectangle
Good capacitance characteristic is still shown under potential scan rate.
Embodiment 5
The concentrated sulfuric acid that the powdered graphite of 0.3681g325 mesh and 0.184g sodium nitrate powder are evenly spread to 9.57ml is molten
In liquid, 2h is stirred to obtain evenly dispersed mixture solution.Notice that this process will carry out in ice bath or ice-water bath, to prevent
The mixture temperature is excessively high.1.1g is slowly added into the above-mentioned evenly dispersed sulfuric acid solution for having powdered graphite and sodium nitrate powder
Then 17.68ml deionized water is added to form suspension in potassium permanganate powder into above-mentioned suspension again.Heat the suspension
35 DEG C and 98 DEG C of pyroreaction stages are subjected to, graphite oxide is finally obtained.Without by obtained graphite oxide from reactant
It is separated, but is directly added it in 250ml beaker in system, measured 100ml distilled water with graduated cylinder and pour into wherein, then
Ultrasonic 8h is carried out to it, obtains graphene oxide dispersion, then to the activity that 14.715g is added in graphene oxide dispersion
Charcoal is mixed, and mixed liquor is dried after mixing evenly.Desciccate is warming up to 100 DEG C in a nitrogen atmosphere to be gone back
Original activation keeps the temperature 6h, and obtained head product is washed (pH=6~7) after cooling, is filtered, dry, final product is obtained.
Above-mentioned final product saves, the test for chemical property after dry in 100 DEG C of air dry oven.It will
Composite material is according to active material: conductive agent: binder=85:10:5 ratio is mixed, and electrode slice is made, then in 6M
Cyclic voltammetry is carried out in KOH electrolyte, 100mV/s sweep speed under, the cyclic voltammetry curve shape of the electrode still close to
Rectangle illustrates using active carbon/Activated Graphite alkene composite material of the method for the present invention preparation the still table under this potential scan rate
Reveal good capacitance characteristic.
Embodiment 6
The concentrated sulfuric acid that the powdered graphite of 0.3681g325 mesh and 0.184g sodium nitrate powder are evenly spread to 9.57ml is molten
In liquid, 2h is stirred to obtain evenly dispersed mixture solution.Notice that this process will carry out in ice bath or ice-water bath, to prevent
The mixture temperature is excessively high.1.1g is slowly added into the above-mentioned evenly dispersed sulfuric acid solution for having powdered graphite and sodium nitrate powder
Then 17.68ml deionized water is added to form suspension in potassium permanganate powder into above-mentioned suspension again.Heat the suspension
35 DEG C and 98 DEG C of pyroreaction stages are subjected to, graphite oxide is finally obtained.Without by obtained graphite oxide from reactant
It is separated, but is directly added it in 250ml beaker in system, measured 100ml distilled water with graduated cylinder and pour into wherein, then
Ultrasonic 8h is carried out to it, obtains graphene oxide dispersion, then to the activity that 14.715g is added in graphene oxide dispersion
Charcoal is mixed, and mixed liquor is dried after mixing evenly.Desciccate is warming up to 1000 DEG C of progress in a nitrogen atmosphere
Reduction activation keeps the temperature 6h, and obtained head product is washed (pH=6~7), filtering, drying after cooling, is finally produced
Object.
Above-mentioned final product saves, the test for chemical property after dry in 100 DEG C of air dry oven.It will
Composite material is according to active material: conductive agent: binder=85:10:5 ratio is mixed, and electrode slice is made, then in 6M
Carry out cyclic voltammetry in KOH electrolyte, test result is shown in the sweeping under speed of 5~100mV/s, the cyclic voltammetric of the electrode
Curve shape still keeps rectangle, illustrates corresponding herein using active carbon/Activated Graphite alkene composite material of the method for the present invention preparation
Good capacitance characteristic is still shown under potential scan rate.
Embodiment 7
The concentrated sulfuric acid that the powdered graphite of 0.3681g325 mesh and 0.184g sodium nitrate powder are evenly spread to 9.57ml is molten
In liquid, 2h is stirred to obtain evenly dispersed mixture solution.Notice that this process will carry out in ice bath or ice-water bath, to prevent
The mixture temperature is excessively high.1.1g is slowly added into the above-mentioned evenly dispersed sulfuric acid solution for having powdered graphite and sodium nitrate powder
Then 17.68ml deionized water is added to form suspension in potassium permanganate powder into above-mentioned suspension again.Heat the suspension
35 DEG C and 98 DEG C of pyroreaction stages are subjected to, graphite oxide is finally obtained.Without by obtained graphite oxide from reactant
It is separated, but is directly added it in 250ml beaker in system, measured 100ml distilled water with graduated cylinder and pour into wherein, then
Ultrasonic 8h is carried out to it, obtains graphene oxide dispersion, then to the activity that 14.715g is added in graphene oxide dispersion
Charcoal is mixed, and mixed liquor is dried after mixing evenly.Desciccate is warming up to 400 DEG C in a nitrogen atmosphere to be gone back
Original activation keeps the temperature 0.5h, and obtained head product is washed (pH=6~7) after cooling, is filtered, dry, is finally produced
Object.
Above-mentioned final product saves, the test for chemical property after dry in 100 DEG C of air dry oven.It will
Composite material is according to active material: conductive agent: binder=85:10:5 ratio is mixed, and electrode slice is made, then in 6M
Carry out cyclic voltammetry in KOH electrolyte, test result is shown in the sweeping under speed of 100mV/s, and the cyclic voltammetric of the electrode is bent
Wire shaped illustrates to sweep using active carbon/Activated Graphite alkene composite material of the method for the present invention preparation in this current potential still close to rectangle
It retouches and still shows good capacitance characteristic under rate.
Embodiment 8
The concentrated sulfuric acid that the powdered graphite of 0.3681g325 mesh and 0.184g sodium nitrate powder are evenly spread to 9.57ml is molten
In liquid, 2h is stirred to obtain evenly dispersed mixture solution.Notice that this process will carry out in ice bath or ice-water bath, to prevent
The mixture temperature is excessively high.1.1g is slowly added into the above-mentioned evenly dispersed sulfuric acid solution for having powdered graphite and sodium nitrate powder
Then 17.68ml deionized water is added to form suspension in potassium permanganate powder into above-mentioned suspension again.Heat the suspension
35 DEG C and 98 DEG C of pyroreaction stages are subjected to, graphite oxide is finally obtained.Without by obtained graphite oxide from reactant
It is separated, but is directly added it in 250ml beaker in system, measured 100ml distilled water with graduated cylinder and pour into wherein, then
Ultrasonic 8h is carried out to it, obtains graphene oxide dispersion, then to the activity that 14.715g is added in graphene oxide dispersion
Charcoal is mixed, and mixed liquor is dried after mixing evenly.Desciccate is warming up to 400 DEG C in a nitrogen atmosphere to be gone back
Original activation keeps the temperature 12h, and obtained head product is washed (pH=6~7) after cooling, is filtered, dry, final product is obtained.
Above-mentioned final product saves, the test for chemical property after dry in 100 DEG C of air dry oven.It will
Composite material is according to active material: conductive agent: binder=85:10:5 ratio is mixed, and electrode slice is made, then in 6M
Carry out cyclic voltammetry in KOH electrolyte, test result is shown in the sweeping under speed of 5~100mV/s, the cyclic voltammetric of the electrode
Curve shape illustrates corresponding electric herein using active carbon/Activated Graphite alkene composite material of the method for the present invention preparation close to rectangle
Good capacitance characteristic is shown under bit scan rate.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (6)
1. a kind of high magnification active carbon/Activated Graphite alkene hybrid supercapacitor electrode material preparation method, which is characterized in that
Active carbon is modified with Activated Graphite alkene, so that the active carbon/activity that can be used as electrode material for super capacitor be made
Graphene combination electrode material, the high rate performance of the material are as follows: specific capacitance is stablized in the current density range of 2~10A/g
250F/g；Specific preparation method includes the following steps:
(1) graphite oxide is prepared using chemical method, then obtained graphite oxide is distributed in strong acid solution, and carry out ultrasound
Processing, obtains graphene oxide dispersion；
(2) active carbon is added in above-mentioned graphene oxide dispersion, is sufficiently stirred, obtain active carbon/graphene oxide point
Dispersion liquid；
(3) solvent in active carbon/graphene oxide dispersion is removed, active carbon/graphene oxide/strong acid mixture is obtained；
(4) in an inert atmosphere, active carbon/graphene oxide/strong acid mixture is heated to certain temperature and kept the temperature centainly
Time is reduced sufficiently graphene oxide therein, and reduzate graphene is activated by strong acid；Wherein, reduction and activation
Temperature range is 100~400 DEG C, and soaking time is 0.5~12h；
(5) obtained reduction washed with activation products, filtered, dried, obtain active carbon/Activated Graphite alkene combination electrode
Material；
Wherein strong acid solution is one or both of the concentrated sulfuric acid, concentrated phosphoric acid, and the mass ratio of active carbon and graphene oxide is
100:1~1:100.
2. according to the active carbon of high magnification described in claim 1/Activated Graphite alkene hybrid supercapacitor electrode material preparation side
Method, it is characterised in that: in step (1), the chemical method is Brodie method, Staudenmaier method or Hummers method；It is super
The sound time is 1h~10h.
3. according to the active carbon of high magnification described in claim 1/Activated Graphite alkene hybrid supercapacitor electrode material preparation side
Method, it is characterised in that: in step (2), mixing time is 0.5~10h.
4. according to the active carbon of high magnification described in claim 1/Activated Graphite alkene hybrid supercapacitor electrode material preparation side
Method, it is characterised in that: in step (3), remove the temperature range of the solvent in active carbon/graphene oxide dispersion are as follows: 30
~150 DEG C.
5. according to the active carbon of high magnification described in claim 1/Activated Graphite alkene hybrid supercapacitor electrode material preparation side
Method, it is characterised in that: in step (4), inert atmosphere is one of nitrogen, argon gas, helium or a variety of mixing.
6. according to the active carbon of high magnification described in claim 1/Activated Graphite alkene hybrid supercapacitor electrode material preparation side
Method, it is characterised in that: in step (5), cleaning fluids are deionized water, and washing standard is that the pH of filtrate is 6~7.
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| CN106486295A (en) * | 2016-10-29 | 2017-03-08 | 大英聚能科技发展有限公司 | The preparation method of the Graphene of high specific capacitance/high surface carbon composite |
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