CN105244175A - N-doped graphene/cobaltosic oxide nanocomposite - Google Patents
N-doped graphene/cobaltosic oxide nanocomposite Download PDFInfo
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- CN105244175A CN105244175A CN201510598098.XA CN201510598098A CN105244175A CN 105244175 A CN105244175 A CN 105244175A CN 201510598098 A CN201510598098 A CN 201510598098A CN 105244175 A CN105244175 A CN 105244175A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses an N-doped graphene/cobaltosic oxide nanocomposite and preparation method and application thereof. The method comprises the steps: adding ammonium hydroxide in oxidized graphene aqueous solution as a nitrogen source; carrying out predoping; carrying out the mixing with cobalt acetate solution; and preparing the N-doped graphene/cobaltosic oxide nanocomposite through employing a hydrothermal method. The predoping greatly improves the N doping amount of graphene, enables the conductivity of the composite material to be increased, facilitates the load of cobaltosic oxide nanoparticles, and enables obtained nanoparticles to be uniform in size (80 nm). The nanocomposite has a dualistic multistage structure, facilitates the sufficient use of active materials, and can be used as the electrode material of a supercapacitor.
Description
Technical field
The invention belongs to nano material and electrochemical field, be specifically related to a kind of nitrogen-doped graphene/cobaltosic oxide nano composite material and its preparation method and application.
Background technology
Graphene as one by carbon atom with sp
2hybridized orbit composition hexangle type is the two-dimensional material of honeycomb lattice, relative to other material with carbon elements, as zero dimension fullerene, one dimension carbon nano-tube, has higher conductivity and specific area.The physical property of its uniqueness and chemical property, cause the great interest of researchers.The application of Graphene in ultracapacitor obtains to be studied widely.Noticeable, there is a lot of defect and greatly reduce its conductivity in Graphene prepared by chemical oxidation, and its electric double layer capacitance shown, cannot meet the application requirement of people to ultracapacitor simultaneously.
Introducing hetero-atoms carries out promoting the performance of Graphene doped with being beneficial to, in addition on the one hand by with fake capacitance material, such as transition metal oxide and conducting polymer, compound improves the ratio capacitance of material.Therefore the present invention's load fake capacitance material while adulterating to Graphene, prepares high performance composite material and just seems very urgent to meet the requirement of people to super electric capacitor.
Summary of the invention
The object of the present invention is to provide a kind of nitrogen-doped graphene/cobaltosic oxide nano composite material and its preparation method and application, by introducing hetero-atoms nitrogen, adulterate to Graphene, improve conductivity, the fake capacitance of load simultaneously material cobaltosic oxide is to obtain larger ratio capacitance.
For achieving the above object, the present invention adopts following technical scheme:
(1) graphene oxide water solution is prepared
Adopt the Hummers method improved, first natural flake graphite is slowly added sulfuric acid/phosphoric acid mixing acid (H
2sO
4: H
3pO
4=9:1, v/v) in solution, subsequently potassium permanganate is added wherein, after mixing, system temperature is risen to 50 DEG C, reaction 12h.Product is used respectively hydrochloric acid, deionized water centrifuge washing, until pH is to neutral, is disperseed after freeze drying in deionized water, obtain graphene oxide water solution, its concentration control 4mg/mL.
(2) by the above-mentioned graphene aqueous solution (60mL) prepared and proper ammonia at 80 DEG C of return stirring certain hours, realize pre-doping;
(3) weigh a certain amount of cobalt acetate, be dissolved in 40mL deionized water in advance, then join in above-mentioned mixed system, carry out hydro-thermal reaction.The concentration of cobalt acetate controls at 0.01 ~ 1mg/mL, and reaction temperature controls at 120 ~ 180 DEG C, and the reaction time controlled at 4 ~ 16 hours.
(4) products therefrom spends deionized water, and 60 DEG C of vacuumizes can obtain nitrogen-doped graphene/cobaltosic oxide nano composite material.
Described nitrogen-doped graphene/cobaltosic oxide composite material is made up of at graphenic surface the cobaltosic oxide uniform particles load of about 80nm, has excellent performance, can be used for electrode material for super capacitor.
The invention has the advantages that: introduce ammoniacal liquor as nitrogenous source, by carrying out pre-doping at 80 DEG C, substantially increase the doping of nitrogen-atoms, then by the fake capacitance electrode material cobaltosic oxide nano particle of hydro thermal method load simultaneously high capacitance, greatly improve the performance of composite material, can be used for super electric capacitor electrode material, the ratio capacitance of final composite material can reach 355.9F/g(0.2A/g).
Accompanying drawing explanation
Fig. 1 is the SEM figure of nitrogen-doped graphene/cobaltosic oxide composite material prepared by the embodiment of the present invention 3;
Fig. 2 is the constant current charge-discharge curve of nitrogen-doped graphene/cobaltosic oxide composite material prepared by the embodiment of the present invention 3.
Embodiment
The present invention's the following example further illustrates the present invention, but protection scope of the present invention is not limited to the following example.
Nano composite material of a kind of nitrogen-doped graphene/cobaltosic oxide and preparation method thereof, its detailed process is:
(1) graphene oxide water solution is prepared
Adopt the Hummers method improved, first natural flake graphite is slowly added sulfuric acid/phosphoric acid mixing acid (H
2sO
4: H
3pO
4=9:1, v/v) in solution, subsequently potassium permanganate is added wherein, after mixing, system temperature is risen to 50 DEG C, reaction 12h, product is used respectively hydrochloric acid, deionized water centrifuge washing, until pH is to neutral, disperseed after freeze drying in deionized water, obtain graphene oxide water solution, its concentration control 4mg/mL.
(2) by the above-mentioned graphene aqueous solution (60mL) prepared and proper ammonia at 80 DEG C of return stirring certain hours, realize pre-doping;
(3) weigh a certain amount of cobalt acetate, be dissolved in 40mL deionized water in advance, then join in above-mentioned mixed system, carry out hydro-thermal reaction.The concentration of cobalt acetate controls at 0.01 ~ 1mg/mL, and reaction temperature controls at 120 ~ 180 DEG C, and the reaction time controlled at 4 ~ 16 hours.
(4) products therefrom spends deionized water, and 60 DEG C of vacuumizes can obtain nitrogen-doped graphene/cobaltosic oxide nano composite material.
embodiment 1
(1) graphene oxide water solution is prepared
Adopt the Hummers method improved, first natural flake graphite is slowly added sulfuric acid/phosphoric acid mixing acid (H
2sO
4: H
3pO
4=9:1, v/v) in solution, subsequently potassium permanganate is added wherein, after mixing, system temperature is risen to 50 DEG C, reaction 12h, product is used respectively hydrochloric acid, deionized water centrifuge washing, until pH is to neutral, disperseed after freeze drying in deionized water, obtain graphene oxide water solution, its concentration control 4mg/mL.
(2) by the above-mentioned graphene aqueous solution (60mL) prepared and 1mL concentrated ammonia liquor at 80 DEG C of return stirring certain hours, realize pre-doping;
(3) weigh a certain amount of cobalt acetate, be dissolved in 40mL deionized water in advance, then join in above-mentioned mixed system, carry out hydro-thermal reaction.The concentration of cobalt acetate controls at 0.2mg/mL, and reaction temperature controls at 180 DEG C, and the reaction time controlled at 12 hours.
(4) products therefrom spends deionized water, and 60 DEG C of vacuumizes can obtain nitrogen-doped graphene/cobaltosic oxide nano composite material.
embodiment 2
(1) graphene oxide water solution is prepared
Adopt the Hummers method improved, first natural flake graphite is slowly added sulfuric acid/phosphoric acid mixing acid (H
2sO
4: H
3pO
4=9:1, v/v) in solution, subsequently potassium permanganate is added wherein, after mixing, system temperature is risen to 50 DEG C, reaction 12h, product is used respectively hydrochloric acid, deionized water centrifuge washing, until pH is to neutral, disperseed after freeze drying in deionized water, obtain graphene oxide water solution, its concentration control 4mg/mL.
(2) by the above-mentioned graphene aqueous solution (60mL) prepared and 2mL concentrated ammonia liquor at 80 DEG C of return stirring certain hours, realize pre-doping;
(3) weigh a certain amount of cobalt acetate, be dissolved in 40mL deionized water in advance, then join in above-mentioned mixed system, carry out hydro-thermal reaction.The concentration of cobalt acetate controls at 0.2mg/mL, and reaction temperature controls at 180 DEG C, and the reaction time controlled at 12 hours.
(4) products therefrom spends deionized water, and 60 DEG C of vacuumizes can obtain nitrogen-doped graphene/cobaltosic oxide nano composite material.
embodiment 3
(1) graphene oxide water solution is prepared
Adopt the Hummers method improved, first natural flake graphite is slowly added sulfuric acid/phosphoric acid mixing acid (H
2sO
4: H
3pO
4=9:1, v/v) in solution, subsequently potassium permanganate is added wherein, after mixing, system temperature is risen to 50 DEG C, reaction 12h, product is used respectively hydrochloric acid, deionized water centrifuge washing, until pH is to neutral, disperseed after freeze drying in deionized water, obtain graphene oxide water solution, its concentration control 4mg/mL.
(2) by the above-mentioned graphene aqueous solution (60mL) prepared and 5mL concentrated ammonia liquor at 80 DEG C of return stirring certain hours, realize pre-doping;
(3) weigh a certain amount of cobalt acetate, be dissolved in 40mL deionized water in advance, then join in above-mentioned mixed system, carry out hydro-thermal reaction.The concentration of cobalt acetate controls at 0.4mg/mL, and reaction temperature controls at 180 DEG C, and the reaction time controlled at 12 hours.
(4) products therefrom spends deionized water, and 60 DEG C of vacuumizes can obtain nitrogen-doped graphene/cobaltosic oxide nano composite material.
Carry out SEM sign to composite material, as can be seen from Figure 1 nano-cobaltic-cobaltous oxide uniform particles is distributed in graphenic surface, and its size is 80-100nm.When as electrode material, it shows excellent invertibity, as shown in Figure 2.315.6F/g is reached by the ratio capacitance calculating combination electrode material.
embodiment 4
(1) graphene oxide water solution is prepared
Adopt the Hummers method improved, first natural flake graphite is slowly added sulfuric acid/phosphoric acid mixing acid (H
2sO
4: H
3pO
4=9:1, v/v) in solution, subsequently potassium permanganate is added wherein, after mixing, system temperature is risen to 50 DEG C, reaction 12h, product is used respectively hydrochloric acid, deionized water centrifuge washing, until pH is to neutral, disperseed after freeze drying in deionized water, obtain graphene oxide water solution, its concentration control 4mg/mL.
(2) by the above-mentioned graphene aqueous solution (60mL) prepared and 5mL concentrated ammonia liquor at 80 DEG C of return stirring certain hours, realize pre-doping;
(3) weigh a certain amount of cobalt acetate, be dissolved in 40mL deionized water in advance, then join in above-mentioned mixed system, carry out hydro-thermal reaction.The concentration of cobalt acetate controls at 0.8mg/mL, and reaction temperature controls at 180 DEG C, and the reaction time controlled at 12 hours.
(4) products therefrom spends deionized water, and 60 DEG C of vacuumizes can obtain nitrogen-doped graphene/cobaltosic oxide nano composite material.
embodiment 5
(1) graphene oxide water solution is prepared
Adopt the Hummers method improved, first natural flake graphite is slowly added sulfuric acid/phosphoric acid mixing acid (H
2sO
4: H
3pO
4=9:1, v/v) in solution, subsequently potassium permanganate is added wherein, after mixing, system temperature is risen to 50 DEG C, reaction 12h, product is used respectively hydrochloric acid, deionized water centrifuge washing, until pH is to neutral, disperseed after freeze drying in deionized water, obtain graphene oxide water solution, its concentration control 4mg/mL.
(2) by the above-mentioned graphene aqueous solution (60mL) prepared and 5mL concentrated ammonia liquor at 80 DEG C of return stirring certain hours, realize pre-doping;
(3) weigh a certain amount of cobalt acetate, be dissolved in 40mL deionized water in advance, then join in above-mentioned mixed system, carry out hydro-thermal reaction.The concentration of cobalt acetate controls at 0.4mg/mL, and reaction temperature controls at 180 DEG C, and the reaction time controlled at 12 hours.
(4) products therefrom spends deionized water, and 60 DEG C of vacuumizes can obtain nitrogen-doped graphene/cobaltosic oxide nano composite material.
embodiment 6
(1) graphene oxide water solution is prepared
Adopt the Hummers method improved, first natural flake graphite is slowly added sulfuric acid/phosphoric acid mixing acid (H
2sO
4: H
3pO
4=9:1, v/v) in solution, subsequently potassium permanganate is added wherein, after mixing, system temperature is risen to 50 DEG C, reaction 12h, product is used respectively hydrochloric acid, deionized water centrifuge washing, until pH is to neutral, disperseed after freeze drying in deionized water, obtain graphene oxide water solution, its concentration control 4mg/mL.
(2) by the above-mentioned graphene aqueous solution (60mL) prepared and 10mL concentrated ammonia liquor at 80 DEG C of return stirring certain hours, realize pre-doping;
(3) weigh a certain amount of cobalt acetate, be dissolved in 40mL deionized water in advance, then join in above-mentioned mixed system, carry out hydro-thermal reaction.The concentration of cobalt acetate controls at 0.8mg/mL, and reaction temperature controls at 180 DEG C, and the reaction time controlled at 12 hours.
(4) products therefrom spends deionized water, and 60 DEG C of vacuumizes can obtain nitrogen-doped graphene/cobaltosic oxide nano composite material.
embodiment 7
(1) graphene oxide water solution is prepared
Adopt the Hummers method improved, first natural flake graphite is slowly added sulfuric acid/phosphoric acid mixing acid (H
2sO
4: H
3pO
4=9:1, v/v) in solution, subsequently potassium permanganate is added wherein, after mixing, system temperature is risen to 50 DEG C, reaction 12h, product is used respectively hydrochloric acid, deionized water centrifuge washing, until pH is to neutral, disperseed after freeze drying in deionized water, obtain graphene oxide water solution, its concentration control 4mg/mL.
(2) by the above-mentioned graphene aqueous solution (60mL) prepared and 10mL concentrated ammonia liquor at 80 DEG C of return stirring certain hours, realize pre-doping;
(3) weigh a certain amount of cobalt acetate, be dissolved in 40mL deionized water in advance, then join in above-mentioned mixed system, carry out hydro-thermal reaction.The concentration of cobalt acetate controls at 0.2mg/mL, and reaction temperature controls at 180 DEG C, and the reaction time controlled at 16 hours.
(4) products therefrom spends deionized water, and 60 DEG C of vacuumizes can obtain nitrogen-doped graphene/cobaltosic oxide nano composite material.
The foregoing is only preferred embodiment of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (9)
1. nitrogen-doped graphene/cobaltosic oxide nano composite material, is characterized in that: be distributed in the cobaltosic oxide nano uniform particles of size uniformity nitrogen-doped graphene surface and form the composite material with binary multilevel hierarchy.
2. nitrogen-doped graphene/cobaltosic oxide nano composite material according to claim 1, is characterized in that: cobaltosic oxide nano particle is of a size of 50-100nm.
3. nitrogen-doped graphene/cobaltosic oxide nano composite material according to claim 1, is characterized in that: in nitrogen-doped graphene, the doping of nitrogen element is more than 11%.
4. prepare the method for nitrogen-doped graphene/cobaltosic oxide nano composite material as claimed in claim 1 for one kind, it is characterized in that: in graphene oxide water solution, introduce ammoniacal liquor as nitrogenous source, carry out pre-doping, then mix with cobalt acetate solution, adopt hydro thermal method to obtain nitrogen-doped graphene/cobaltosic oxide nano composite material:
Comprise the following steps:
(1) graphene oxide water solution that concentration is 4mg/mL is prepared;
(2) return stirring at 80 DEG C by graphene oxide water solution and ammoniacal liquor, carries out pre-doping;
(3) add cobalt acetate solution, carry out hydro-thermal reaction;
(4) products therefrom spends deionized water, 60 DEG C of vacuumizes.
5. method according to claim 4, is characterized in that: in step (2), the volume of ammoniacal liquor is 1 ~ 10mL.
6. method according to claim 4, is characterized in that: in step (2), the reaction time is 2 ~ 12 hours.
7. method according to claim 4, is characterized in that: in step (3), the concentration of cobalt acetate solution is 0.01 ~ 1mg/mL.
8. method according to claim 4, is characterized in that: in step (3), hydrothermal temperature is 120 ~ 180 DEG C, and the reaction time is 4 ~ 16 hours.
9. an application for nitrogen-doped graphene/cobaltosic oxide nano composite material as claimed in claim 1, is characterized in that: described composite material is as electrode material for super capacitor.
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Cited By (10)
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| CN105632787A (en) * | 2016-01-20 | 2016-06-01 | 安徽大学 | Preparation method of cobaltosic oxide/graphene nano composite electrode material for super capacitor |
| CN106450354A (en) * | 2016-09-30 | 2017-02-22 | 合肥工业大学 | Hydrothermal synthesis method for nitrogen-doping graphene-loaded cobalt oxygen reduction reaction electrocatalyst |
| CN106486291A (en) * | 2016-09-21 | 2017-03-08 | 浙江大学 | A kind of NiO/rGO composite nano materials and preparation method thereof |
| CN106602078A (en) * | 2016-12-30 | 2017-04-26 | 华南理工大学 | Graphene-supported, nitrogen-doped and carbon film-coated cobaltosic oxide composite material and preparation and application |
| CN106654212A (en) * | 2016-12-29 | 2017-05-10 | 吉林大学 | Preparation method and application of cobaltosic oxide/graphene composite material (Co<3>O<4>/N-RGO) |
| CN106908498A (en) * | 2017-04-07 | 2017-06-30 | 安徽工业大学 | A kind of Co4S3The preparation method and applications of/nitrogen-doped graphene composite |
| CN107746051A (en) * | 2017-10-26 | 2018-03-02 | 复旦大学 | A kind of nitrogen-doped graphene nanobelt nano-cobaltic-cobaltous oxide hybrid material and preparation method thereof |
| CN108455685A (en) * | 2018-03-07 | 2018-08-28 | 上海应用技术大学 | A kind of N/Co3O4Composite porous preparation method |
| CN113620350A (en) * | 2021-08-19 | 2021-11-09 | 珠海市科立鑫金属材料有限公司 | Preparation method of large-particle cobaltosic oxide |
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| CN105632787A (en) * | 2016-01-20 | 2016-06-01 | 安徽大学 | Preparation method of cobaltosic oxide/graphene nano composite electrode material for super capacitor |
| CN106486291A (en) * | 2016-09-21 | 2017-03-08 | 浙江大学 | A kind of NiO/rGO composite nano materials and preparation method thereof |
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| CN106654212B (en) * | 2016-12-29 | 2019-07-30 | 吉林大学 | A kind of Co3O4The preparation method and application of/N-RGO/HSAs composite material |
| CN106602078A (en) * | 2016-12-30 | 2017-04-26 | 华南理工大学 | Graphene-supported, nitrogen-doped and carbon film-coated cobaltosic oxide composite material and preparation and application |
| CN106908498A (en) * | 2017-04-07 | 2017-06-30 | 安徽工业大学 | A kind of Co4S3The preparation method and applications of/nitrogen-doped graphene composite |
| CN107746051A (en) * | 2017-10-26 | 2018-03-02 | 复旦大学 | A kind of nitrogen-doped graphene nanobelt nano-cobaltic-cobaltous oxide hybrid material and preparation method thereof |
| CN108455685A (en) * | 2018-03-07 | 2018-08-28 | 上海应用技术大学 | A kind of N/Co3O4Composite porous preparation method |
| CN108455685B (en) * | 2018-03-07 | 2020-01-31 | 上海应用技术大学 | kinds of N/Co3O4Preparation method of porous composite material |
| CN113620350A (en) * | 2021-08-19 | 2021-11-09 | 珠海市科立鑫金属材料有限公司 | Preparation method of large-particle cobaltosic oxide |
| CN115215380A (en) * | 2022-07-13 | 2022-10-21 | 四川轻化工大学 | Cobaltosic oxide/nitrogen-doped graphene oxide material, preparation method thereof and application thereof in sodium-ion battery |
| CN115215380B (en) * | 2022-07-13 | 2023-12-08 | 四川轻化工大学 | Tricobalt tetraoxide/nitrogen-doped graphene oxide material, preparation method thereof and application thereof in sodium ion battery |
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Application publication date: 20160113 |