CN105321726A - High-magnification active carbon and active graphene composite electrode material and preparation method thereof - Google Patents
High-magnification active carbon and active graphene composite electrode material and preparation method thereof Download PDFInfo
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- CN105321726A CN105321726A CN201410348689.7A CN201410348689A CN105321726A CN 105321726 A CN105321726 A CN 105321726A CN 201410348689 A CN201410348689 A CN 201410348689A CN 105321726 A CN105321726 A CN 105321726A
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Abstract
The invention relates to a high-magnification active carbon and active graphene composite electrode material and a preparation method thereof. The material is characterized in that active carbon is uniformly dispersed into an activator-contained oxidized graphene solution and heated to remove moisture therein, an obtained mixture is reduced and activated at certain temperature in the protective atmosphere, and a product is washed, filtered and dried to obtain the active carbon and active graphene composite electrode material. The active carbon and active graphene composite electrode material provided by the invention is high in the specific capacity and magnification, and the specific capacitive of the material is kept in 250F/g in the current density range of 2-10A/g; and the preparation method of the material is simple in technical process, saves time, is low in cost and is easy to realize large-scale industrial production.
Description
Technical field
The present invention relates to electric chemical super capacitor technical field, be specifically related to a kind of high magnification active carbon/Activated Graphite alkene hybrid supercapacitor electrode material and preparation method thereof.
Background technology
Ultracapacitor (Supercapacitor), be also called electrochemical capacitance (ultracapacitor), electrochemical capacitor (ElectrochemicalCapacitor, EC), electric chemical super capacitor (ElectrochemicalSupercapacitor), be a kind of novel energy-storing device, it in seconds can complete charging.In addition ultracapacitor also have that output power density is high, operating temperature range is wide, have extended cycle life, the feature such as economic environmental protection.Ultracapacitor has huge using value and market potential in fields such as renewable energy utilization, traffic, electric power, communication, national defence.Particularly the rise of wind-force, photovoltaic generation and electric motor car makes the research and development of this novel energy-storing technology of ultracapacitor day by day come into one's own.
Graphene (graphene) be a kind of by carbon atom with sp
2the crystal of the cellular lattice structure of hexangle type of hybridized orbit composition, is considered to the basic structural unit of fullerene, carbon nano-tube and graphite.Graphene has unique physical characteristic, and as higher specific area, (theoretical specific surface area is up to 2630m
2/ g) and very high conductance (resistivity is about 10
-6Ω cm).Graphene is a kind of energy storage material with broad prospect of application, as graphene-based material can be used as the electrode material of ultracapacitor.The preparation method of Graphene has micromechanics stripping method, superficial growth method (epitaxial growth, vapour deposition etc.), chemical stripping method, chemical synthesis (organic precursor synthesis and solvent-thermal process) etc.Wherein chemical synthesis is adapted to large-scale production grapheme material most.Most importantly chemical reduction method in chemical synthesis, such as utilize the strong reductants such as hydrazine hydrate to carry out reducing, high-temperature heating reduction, microwave irradiation reduction, electrochemical reduction etc., the grapheme material with high conductivity high-specific surface area can be obtained.
Although the theoretical specific surface area of Graphene is very high, stamp because sheet is stacked, the specific area of Graphene prepared by chemical method is well below theoretical value, and the ratio capacitance that can reach as electrode material for super capacitor is also lower.Activation processing is carried out to Graphene, its specific area and ratio capacitance can be increased substantially.
At present, the preparation method of Activated Graphite alkene has physical activation method and chemical activation method, and physical activation method is at high temperature, and Graphene raw material is under the effect of catalyst, carbon wherein and oxidizing gas react, part carbon gasification and the obtained Activated Graphite alkene with high-specific surface area.Conventional activator has alkali metal, iron, carbonate etc.Chemical activation method is under the effect of activator, and the hydrogen in Graphene raw material or oxygen are partly or entirely removed, and carry out carbonization-activation to it simultaneously.Conventional activator has 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 advantage such as specific area is large.Because conductivity is poor, the chemical property of commercial activated charcoal can along with the increase of current density rapid decay.And no matter be in water system or in organic system electrolyte solution, the characteristic such as high conductivity, high-specific surface area, height ratio capacity, high rate capability of Activated Graphite alkene material is a kind of the supplementing well to absorbent charcoal material.Active carbon and Activated Graphite alkene are carried out the ratio capacitance value that compound can not only improve electrode material, and composite material exhibits can be made to go out high high rate performance.
By the end of at present, the research of active carbon and Activated Graphite alkene Material cladding is less.Only there is the report about active carbon and Graphene compound.According to the literature, the people such as Zhang Kai utilizes the method for collosol and gel that Graphene and phenolic resin-based activated carbon are carried out In-situ reaction to prepare active carbon/graphene combination electrode material.And the sol-gel process that it adopts is consuming time longer, the carbonization process environmental pollution of carbon source used is serious.In addition, also have report active carbon and Graphene being carried out mechanical mixture and prepare combination electrode material, but adopt the method to be difficult to dispersed at activated carbon surface of guarantee Graphene.
The present invention aims to provide a kind of Activated Graphite alkene carries out modification method to merchandise active carbon.The feature of the method be active carbon first with graphene oxide and activator mix, then at high temperature realize the reduction of wherein graphene oxide, activation and the compound with absorbent charcoal material thereof.The preparation method of this active carbon/Activated Graphite alkene hybrid supercapacitor electrode material have technical process simple, save time, cost is low and be easy to realize the advantage of large-scale industrial production.
Summary of the invention
The object of this invention is to provide a kind of high magnification active carbon/Activated Graphite alkene hybrid supercapacitor electrode material and preparation method thereof.This active carbon/Activated Graphite alkene composite material exhibits goes out the high rate performance more excellent than conventional carbon, adopts active carbon and graphene oxide and activator mix and is at high temperature prepared the method that graphene oxide wherein carries out reducing Yu activating.
The present invention specifically provides a kind of high magnification active carbon/Activated Graphite alkene hybrid supercapacitor electrode material; it is characterized in that: in protective atmosphere; the mixture of active carbon, graphene oxide and activator carried out under certain temperature range reduce and activate; and then product is carried out washing, filtering and drying; obtain active carbon/Activated Graphite alkene combination electrode material, wherein activator is one or both in the concentrated sulfuric acid, SPA.
The preparation method of high magnification active carbon of the present invention/Activated Graphite alkene hybrid supercapacitor electrode material, is characterized in that, comprise the steps:
(1) adopt chemical method to prepare graphite oxide, then the graphite oxide obtained is distributed in strong acid solution, and carries out ultrasonic process, obtain graphene oxide dispersion; Described chemical method is Brodie method, Staudenmaier method or Hummers method; When adopting Hummers legal system for graphite oxide, without the need to being separated from reaction system by the graphite oxide obtained, but directly ultrasonic process being carried out to it, obtaining graphene oxide dispersion.In graphene oxide dispersion, the remaining concentrated sulfuric acid directly can be used as activator.Adopt additive method when preparing graphite oxide, graphite oxide need be distributed to dried up in, then add activator, ultrasonic process, obtains graphene oxide dispersion.Described activator is one or both in the concentrated sulfuric acid, SPA.Described ultrasonic time is 1 ~ 10h (preferred 8h).
(2) active carbon is joined in above-mentioned graphene oxide dispersion, fully stir, obtain active carbon/graphene oxide dispersion; Wherein, the quality of described active carbon and graphene oxide is 100:1 ~ 1:100 (preferred 1:1) than scope; Mixing time is 0.5 ~ 10h (being preferably 6h).
(3) remove the solvent in active carbon/graphene oxide dispersion, obtain active carbon/graphene oxide/strong acid mixture; Wherein, the method for the solvent in described removal active carbon/graphene oxide dispersion is: active carbon/graphene oxide dispersion is toasted 0.5 ~ 48h under heat lamp, or in drying box dry 0.5 ~ 24h at 30 ~ 150 DEG C.
(4) in an inert atmosphere, active carbon/graphene oxide/strong acid mixture is heated to uniform temperature and is incubated the regular hour and carry out reducing and activation processing, graphene oxide is wherein reduced sufficiently, reduzate Graphene activate by strong acid, obtain powerful active carbon/Activated Graphite alkene hybrid supercapacitor electrode material head product.Wherein inert gas is: one or more in nitrogen, helium and argon gas, and inert gas flow velocity is 40 ~ 500mlmin
-1.Reduction and activation temperature 100 ~ 1000 DEG C (being preferably 100 ~ 800 DEG C), reduction and soak time are 0.5 ~ 12h.
(5) reduction obtained and activation products carried out wash, filter, dry, obtain active carbon/Activated Graphite alkene combination electrode material, cleaning fluids is deionized water, washing standard is the pH of filtrate is 6 ~ 7, and baking temperature is 30 ~ 150 DEG C (being preferably 100 ~ 150 DEG C).
Advantage of the present invention: active carbon provided by the invention/Activated Graphite alkene hybrid supercapacitor electrode material has higher specific capacity and is better than the high rate performance (ratio capacitance is stabilized in 250F/g in the current density range of 2 ~ 10A/g) of traditional activated carbon electrode material.By having height ratio capacity, the Activated Graphite alkene of high stable performance is incorporated in absorbent charcoal material, and the two also can produce synergy, on the basis of improving active carbon specific capacity, can improve its high rate performance by a relatively large margin.Therefore, active carbon and Activated Graphite alkene are carried out compound, the distinct electrical of bi-material chemistry capacitance characteristic can be made to be given full play to.The preparation method of active carbon of the present invention/Activated Graphite alkene composite material, have technical process simple, save time, cost is low and be easy to realize the advantages such as large-scale industrial production.
Accompanying drawing explanation
Fig. 1 is the XRD figure of active carbon/Activated Graphite alkene composite material prepared by the embodiment of the present invention 1;
Fig. 2 is the cyclic voltammetry curve figure that the active carbon/Activated Graphite alkene composite material prepared with the embodiment of the present invention 1 does the electrode of super capacitor of active material;
Fig. 3 is the electrochemical impedance spectroscopy that the active carbon/Activated Graphite alkene composite material prepared with the embodiment of the present invention 1 does the electrode of super capacitor of active material;
Fig. 4 is the constant current charge-discharge curve that the active carbon/Activated Graphite alkene composite material prepared with the embodiment of the present invention 1 does the electrode of super capacitor of active material;
Fig. 5 is the multiplying power property curve of electrode material and the active carbon obtained after the embodiment of the present invention 1 PROCESS FOR TREATMENT;
Fig. 6 is the cyclic voltammetry curve figure of active carbon/Activated Graphite alkene composite material prepared by the embodiment of the present invention 2;
Fig. 7 is the constant current charge-discharge curve chart of active carbon/Activated Graphite alkene composite material prepared by the embodiment of the present invention 3;
Fig. 8 is the cyclic voltammetry curve figure of active carbon/Activated Graphite alkene composite material prepared by the embodiment of the present invention 4.
Embodiment
The following examples will be further described the present invention, but not thereby limiting the invention.
Embodiment 1
0.3681g325 object powdered graphite and 0.184g sodium nitrate powder are evenly spread in the concentrated sulfuric acid solution of 9.57ml, stirs 2h to obtain homodisperse mixture solution.Notice that this process will be carried out in ice bath or ice-water bath, to prevent this mixture temperature too high.To above-mentioned dispersed have in the sulfuric acid solution of powdered graphite and sodium nitrate powder slowly add 1.1g potassium permanganate powder to form suspension-turbid liquid, and then add 17.68ml deionized water in above-mentioned suspension-turbid liquid.Heating this suspension-turbid liquid makes it experience 35 DEG C and 98 DEG C of pyroreaction stages, finally obtains graphite oxide.Without the need to the graphite oxide obtained is separated from reaction system, but directly joined in 250ml beaker, measuring 100ml distilled water with graduated cylinder pours into wherein, then ultrasonic 8h is carried out to it, obtain graphene oxide dispersion, mix subsequently to the active carbon adding 14.715g in graphene oxide dispersion, after stirring, drying is carried out to mixed liquor.Desciccate is warming up in a nitrogen atmosphere 400 DEG C and carries out reduction activation, insulation 6h, after cooling, the head product obtained is carried out washing (pH=6 ~ 7), filtration, drying, obtain end product.
Above-mentioned end product, preserves, for the test of chemical property after the air dry oven inner drying of 100 DEG C.The XRD test result of active carbon/Activated Graphite alkene composite powder as shown in Figure 1.XRD test result shows that graphene oxide has been reduced and has activated, active carbon/Activated Graphite alkene compound.By composite material according to active material: conductive agent: the ratio of binding agent=85:10:5 mixes, and makes electrode slice, then in 6MKOH electrolyte, carry out cyclic voltammetry, test result as shown in Figure 2.100mV/s sweep speed under, the cyclic voltammetry curve shape of this electrode, still close to rectangle, illustrates and adopts active carbon/Activated Graphite alkene composite material of preparing of the inventive method still to show good capacitance characteristic under this potential scan rate.Ac impedance measurement shown in Fig. 3 shows that this electrode has lower ohmmic drop.Constant current charge-discharge result shows that active carbon/Activated Graphite alkene combination electrode material has height ratio capacity (Fig. 4).The ratio capacitance of composite material under the current density of 0.05A/g reaches 332.77F/g, and the ratio capacitance under the current density of 5A/g reaches 243.42F/g.Figure 5 shows that the multiplying power property curve adopting galvanostatic charge/discharge to test the active carbon/Activated Graphite alkene combination electrode material obtained.From figure, compared with active carbon, composite material is along with the increase of discharge current density, and ratio capacitance declines slowly.Particularly when current density brings up to 6000mA/g from 2000mA/g, the ratio capacitance of composite material does not almost reduce, and illustrates that the active carbon/Activated Graphite alkene prepared by the present embodiment has excellent high rate performance.
Embodiment 2
Made for embodiment 1 graphite oxide is joined in 250ml beaker, measuring 100ml distilled water with graduated cylinder pours into wherein, then ultrasonic 8h is carried out to it, obtain graphene oxide dispersion, mix subsequently to the active carbon adding 8.645g in graphene oxide dispersion, after stirring, drying is carried out to mixed liquor.Desciccate is warming up in a nitrogen atmosphere 400 DEG C and carries out reduction activation, insulation 6h, after cooling, the head product obtained is carried out washing (pH=6 ~ 7), filtration, drying, obtain end product.
Above-mentioned end product, preserves, for the test of chemical property after the air dry oven inner drying of 100 DEG C.By composite material according to active material: conductive agent: the ratio of binding agent=85:10:5 mixes, and makes electrode slice, then in 6MKOH electrolyte, carry out cyclic voltammetry, test result as shown in Figure 6.100mV/s sweep speed under, the cyclic voltammetry curve shape of this electrode, still close to rectangle, illustrates and adopts active carbon/Activated Graphite alkene composite material of preparing of the inventive method still to show good capacitance characteristic under this potential scan rate.Constant current charge-discharge test result shows that active carbon/Activated Graphite alkene combination electrode material has height ratio capacity, high rate capability, and the ratio capacitance of composite material under the current density of 5A/g reaches 206.04F/g.
Embodiment 3
Made for embodiment 1 graphite oxide is joined in 250ml beaker, measuring 100ml distilled water with graduated cylinder pours into wherein, then ultrasonic 8h is carried out to it, obtain graphene oxide dispersion, mix subsequently to the active carbon adding 4.095g in graphene oxide dispersion, after stirring, drying is carried out to mixed liquor.Desciccate is warming up in a nitrogen atmosphere 400 DEG C and carries out reduction activation, insulation 6h, after cooling, the head product obtained is carried out washing (pH=6 ~ 7), filtration, drying, obtain end product.
Above-mentioned end product, preserves, for the test of chemical property after the air dry oven inner drying of 100 DEG C.By composite material according to active material: conductive agent: the ratio of binding agent=85:10:5 mixes, and makes electrode slice, then in 6MKOH electrolyte, carry out constant current charge-discharge test, test result as shown in Figure 7.Constant current charge-discharge result shows that active carbon/Activated Graphite alkene combination electrode material has height ratio capacity, and the ratio capacitance of composite material under the current density of 5A/g reaches 193.61F/g.100mV/s sweep speed under, the cyclic voltammetry curve shape of this electrode, still close to rectangle, illustrates that to adopt active carbon/Activated Graphite alkene composite material capacitance characteristic under this potential scan rate of preparing of the inventive method good.
Embodiment 4
Made for embodiment 1 graphite oxide is joined in 250ml beaker, measuring 100ml distilled water with graduated cylinder pours into wherein, then ultrasonic 8h is carried out to it, obtain graphene oxide dispersion, mix subsequently to the active carbon adding 2.575g in graphene oxide dispersion, after stirring, drying is carried out to mixed liquor.Desciccate is warming up in a nitrogen atmosphere 400 DEG C of insulation 6h and carries out reduction activation, after cooling, the head product obtained is carried out washing (pH=6 ~ 7), filtration, drying, obtain end product.
Above-mentioned end product, preserves, for the test of chemical property after the air dry oven inner drying of 100 DEG C.By composite material according to active material: conductive agent: the ratio of binding agent=85:10:5 mixes, make electrode slice, then in 6MKOH electrolyte, cyclic voltammetry is carried out, test result as shown in Figure 8,100mV/s sweep speed under, the cyclic voltammetry curve shape of this electrode, still close to rectangle, illustrates that the active carbon/Activated Graphite alkene composite material adopting the inventive method to prepare still shows good capacitance characteristic under this potential scan rate.
Embodiment 5
0.3681g325 object powdered graphite and 0.184g sodium nitrate powder are evenly spread in the concentrated sulfuric acid solution of 9.57ml, stirs 2h to obtain homodisperse mixture solution.Notice that this process will be carried out in ice bath or ice-water bath, to prevent this mixture temperature too high.To above-mentioned dispersed have in the sulfuric acid solution of powdered graphite and sodium nitrate powder slowly add 1.1g potassium permanganate powder to form suspension-turbid liquid, and then add 17.68ml deionized water in above-mentioned suspension-turbid liquid.Heating this suspension-turbid liquid makes it experience 35 DEG C and 98 DEG C of pyroreaction stages, finally obtains graphite oxide.Without the need to the graphite oxide obtained is separated from reaction system, but directly joined in 250ml beaker, measuring 100ml distilled water with graduated cylinder pours into wherein, then ultrasonic 8h is carried out to it, obtain graphene oxide dispersion, mix subsequently to the active carbon adding 14.715g in graphene oxide dispersion, after stirring, drying is carried out to mixed liquor.Desciccate is warming up in a nitrogen atmosphere 100 DEG C and carries out reduction activation, insulation 6h, after cooling, the head product obtained is carried out washing (pH=6 ~ 7), filtration, drying, obtain end product.
Above-mentioned end product, preserves, for the test of chemical property after the air dry oven inner drying of 100 DEG C.By composite material according to active material: conductive agent: the ratio of binding agent=85:10:5 mixes, make electrode slice, then in 6MKOH electrolyte, cyclic voltammetry is carried out, 100mV/s sweep speed under, the cyclic voltammetry curve shape of this electrode, still close to rectangle, illustrates that the active carbon/Activated Graphite alkene composite material adopting the inventive method to prepare still shows good capacitance characteristic under this potential scan rate.
Embodiment 6
0.3681g325 object powdered graphite and 0.184g sodium nitrate powder are evenly spread in the concentrated sulfuric acid solution of 9.57ml, stirs 2h to obtain homodisperse mixture solution.Notice that this process will be carried out in ice bath or ice-water bath, to prevent this mixture temperature too high.To above-mentioned dispersed have in the sulfuric acid solution of powdered graphite and sodium nitrate powder slowly add 1.1g potassium permanganate powder to form suspension-turbid liquid, and then add 17.68ml deionized water in above-mentioned suspension-turbid liquid.Heating this suspension-turbid liquid makes it experience 35 DEG C and 98 DEG C of pyroreaction stages, finally obtains graphite oxide.Without the need to the graphite oxide obtained is separated from reaction system, but directly joined in 250ml beaker, measuring 100ml distilled water with graduated cylinder pours into wherein, then ultrasonic 8h is carried out to it, obtain graphene oxide dispersion, mix subsequently to the active carbon adding 14.715g in graphene oxide dispersion, after stirring, drying is carried out to mixed liquor.Desciccate is warming up in a nitrogen atmosphere 1000 DEG C and carries out reduction activation, insulation 6h, after cooling, the head product obtained is carried out washing (pH=6 ~ 7), filtration, drying, obtain end product.
Above-mentioned end product, preserves, for the test of chemical property after the air dry oven inner drying of 100 DEG C.By composite material according to active material: conductive agent: the ratio of binding agent=85:10:5 mixes, make electrode slice, then in 6MKOH electrolyte, cyclic voltammetry is carried out, test result be presented at 5 ~ 100mV/s sweep speed under, the cyclic voltammetry curve shape of this electrode still keeps rectangle, illustrates that the active carbon/Activated Graphite alkene composite material adopting the inventive method to prepare still shows good capacitance characteristic under this corresponding potential scan rate.
Embodiment 7
0.3681g325 object powdered graphite and 0.184g sodium nitrate powder are evenly spread in the concentrated sulfuric acid solution of 9.57ml, stirs 2h to obtain homodisperse mixture solution.Notice that this process will be carried out in ice bath or ice-water bath, to prevent this mixture temperature too high.To above-mentioned dispersed have in the sulfuric acid solution of powdered graphite and sodium nitrate powder slowly add 1.1g potassium permanganate powder to form suspension-turbid liquid, and then add 17.68ml deionized water in above-mentioned suspension-turbid liquid.Heating this suspension-turbid liquid makes it experience 35 DEG C and 98 DEG C of pyroreaction stages, finally obtains graphite oxide.Without the need to the graphite oxide obtained is separated from reaction system, but directly joined in 250ml beaker, measuring 100ml distilled water with graduated cylinder pours into wherein, then ultrasonic 8h is carried out to it, obtain graphene oxide dispersion, mix subsequently to the active carbon adding 14.715g in graphene oxide dispersion, after stirring, drying is carried out to mixed liquor.Desciccate is warming up in a nitrogen atmosphere 400 DEG C and carries out reduction activation, insulation 0.5h, after cooling, the head product obtained is carried out washing (pH=6 ~ 7), filtration, drying, obtain end product.
Above-mentioned end product, preserves, for the test of chemical property after the air dry oven inner drying of 100 DEG C.By composite material according to active material: conductive agent: the ratio of binding agent=85:10:5 mixes, make electrode slice, then in 6MKOH electrolyte, cyclic voltammetry is carried out, test result be presented at 100mV/s sweep speed under, the cyclic voltammetry curve shape of this electrode, still close to rectangle, illustrates that the active carbon/Activated Graphite alkene composite material adopting the inventive method to prepare still shows good capacitance characteristic under this potential scan rate.
Embodiment 8
0.3681g325 object powdered graphite and 0.184g sodium nitrate powder are evenly spread in the concentrated sulfuric acid solution of 9.57ml, stirs 2h to obtain homodisperse mixture solution.Notice that this process will be carried out in ice bath or ice-water bath, to prevent this mixture temperature too high.To above-mentioned dispersed have in the sulfuric acid solution of powdered graphite and sodium nitrate powder slowly add 1.1g potassium permanganate powder to form suspension-turbid liquid, and then add 17.68ml deionized water in above-mentioned suspension-turbid liquid.Heating this suspension-turbid liquid makes it experience 35 DEG C and 98 DEG C of pyroreaction stages, finally obtains graphite oxide.Without the need to the graphite oxide obtained is separated from reaction system, but directly joined in 250ml beaker, measuring 100ml distilled water with graduated cylinder pours into wherein, then ultrasonic 8h is carried out to it, obtain graphene oxide dispersion, mix subsequently to the active carbon adding 14.715g in graphene oxide dispersion, after stirring, drying is carried out to mixed liquor.Desciccate is warming up in a nitrogen atmosphere 400 DEG C and carries out reduction activation, insulation 12h, after cooling, the head product obtained is carried out washing (pH=6 ~ 7), filtration, drying, obtain end product.
Above-mentioned end product, preserves, for the test of chemical property after the air dry oven inner drying of 100 DEG C.By composite material according to active material: conductive agent: the ratio of binding agent=85:10:5 mixes, make electrode slice, then in 6MKOH electrolyte, cyclic voltammetry is carried out, test result be presented at 5 ~ 100mV/s sweep speed under, the cyclic voltammetry curve shape of this electrode, close to rectangle, illustrates that the active carbon/Activated Graphite alkene composite material adopting the inventive method to prepare shows good capacitance characteristic under this corresponding potential scan rate.
Above-described embodiment, only for technical conceive of the present invention and feature are described, its object is to person skilled in the art can be understood content of the present invention and implement according to this, can not limit the scope of the invention with this.All equivalences done according to Spirit Essence of the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (9)
1. high magnification active carbon/Activated Graphite alkene hybrid supercapacitor electrode material; it is characterized in that: in protective atmosphere; the mixture of active carbon, graphene oxide and activator carried out under certain temperature range reduce and activate; and then product is carried out washing, filtering and drying; obtain active carbon/Activated Graphite alkene combination electrode material, wherein activator is one or both in the concentrated sulfuric acid, SPA.
2., according to a preparation method for high magnification active carbon described in claim 1/Activated Graphite alkene hybrid supercapacitor electrode material, it is characterized in that, comprise the steps:
(1) adopt chemical method to prepare graphite oxide, then the graphite oxide obtained is distributed in strong acid solution, and carries out ultrasonic process, obtain graphene oxide dispersion;
(2) active carbon is joined in above-mentioned graphene oxide dispersion, fully stir, obtain active carbon/graphene oxide dispersion;
(3) remove the solvent in active carbon/graphene oxide dispersion, obtain active carbon/graphene oxide/strong acid mixture;
(4) in an inert atmosphere, active carbon/graphene oxide/strong acid mixture is heated to uniform temperature and is incubated the regular hour, graphene oxide is wherein reduced sufficiently, reduzate Graphene activate by strong acid;
(5) reduction obtained and activation products carried out wash, filter, dry, obtain active carbon/Activated Graphite alkene combination electrode material.
3. according to the preparation method of high magnification active carbon described in claim 2/Activated Graphite alkene hybrid supercapacitor electrode material, it is characterized in that: in step (1), described chemical method is Brodie method, Staudenmaier method or Hummers method; Ultrasonic time is 1h ~ 10h.
4. according to the preparation method of high magnification active carbon described in claim 2/Activated Graphite alkene hybrid supercapacitor electrode material, it is characterized in that: in step (2), the mass ratio of active carbon and graphene oxide is 100:1 ~ 1:100; Mixing time is 0.5 ~ 10h.
5. according to the preparation method of high magnification active carbon described in claim 4/Activated Graphite alkene hybrid supercapacitor electrode material, it is characterized in that: the mass ratio of active carbon and graphene oxide is 1:1.
6. according to the preparation method of high magnification active carbon described in claim 2/Activated Graphite alkene hybrid supercapacitor electrode material, it is characterized in that: in step (3), the temperature range removing the solvent in active carbon/graphene oxide dispersion is: 30 ~ 150 DEG C.
7. according to the preparation method of high magnification active carbon described in claim 2/Activated Graphite alkene hybrid supercapacitor electrode material, it is characterized in that: in step (4), the reduction of active carbon/graphene oxide/strong acid mixture and active temperature range are 100 ~ 100 DEG C, and temperature retention time is 0.5 ~ 12h; Inert atmosphere is one or more the mixing in nitrogen, argon gas, helium.
8., according to the preparation method of high magnification active carbon described in claim 7/Activated Graphite alkene hybrid supercapacitor electrode material, it is characterized in that: the reduction of active carbon/graphene oxide/strong acid mixture and active temperature range are 100 ~ 800 DEG C.
9. according to the preparation method of high magnification active carbon described in claim 2/Activated Graphite alkene hybrid supercapacitor electrode material, it is characterized in that: in step (5), cleaning fluids is deionized water, and washing standard is the pH of filtrate is 6 ~ 7.
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| CN107093525A (en) * | 2017-04-05 | 2017-08-25 | 苏州海凌达电子科技有限公司 | A kind of preparation method of the electrode material of oxidized graphene aqueous solution processing |
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| CN112133571A (en) * | 2020-09-03 | 2020-12-25 | 方大炭素新材料科技股份有限公司 | Graphene cross-linked activated carbon composite membrane, preparation method and supercapacitor electrode |
| CN112670100A (en) * | 2020-12-16 | 2021-04-16 | 成都善镁渠环保科技有限公司 | Preparation method of supercapacitor electrode material |
| CN114506841A (en) * | 2022-04-19 | 2022-05-17 | 中科南京绿色制造产业创新研究院 | Biomass-graphene composite electrode material and preparation method and application thereof |
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| CN112133571A (en) * | 2020-09-03 | 2020-12-25 | 方大炭素新材料科技股份有限公司 | Graphene cross-linked activated carbon composite membrane, preparation method and supercapacitor electrode |
| CN112670100A (en) * | 2020-12-16 | 2021-04-16 | 成都善镁渠环保科技有限公司 | Preparation method of supercapacitor electrode material |
| CN114506841A (en) * | 2022-04-19 | 2022-05-17 | 中科南京绿色制造产业创新研究院 | Biomass-graphene composite electrode material and preparation method and application thereof |
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