CN105895384A - Method for preparing graphene/ superfine cobalt oxide granule compound electrode material - Google Patents
Method for preparing graphene/ superfine cobalt oxide granule compound electrode material Download PDFInfo
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- CN105895384A CN105895384A CN201610302686.9A CN201610302686A CN105895384A CN 105895384 A CN105895384 A CN 105895384A CN 201610302686 A CN201610302686 A CN 201610302686A CN 105895384 A CN105895384 A CN 105895384A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- 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
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Abstract
The invention discloses a liquid laser irradiation/ ablation preparation method of a graphene/ superfine Co3O4 granule compound electrode material. The method specifically comprises the following steps: sufficiently mixing graphene oxide and a precursor of Co3O4 in different proportions in different solvents, and then preparing the graphene/ superfine Co3O4 granule compound material under different pulse laser conditions. The graphene/ superfine Co3O4 granule compound material shows excellent specific volumetric capacity as a super-capacitor electrode material. The preparation method has the advantages of novelty, simplicity in operation, low preparation cost, high product purity and the like.
Description
Technical field
The present invention relates to the preparation method of a kind of combination electrode material, particularly relate to a kind of Graphene/ultra micro Co3O4Particles dispersed electrode material preparation method；Belong to field of nanometer material technology.
Background technology
Cobaltosic oxide (Co3O4) as a kind of typical battery-type electrode chose material, there are high theoretical capacity (3560 Fg-1), the feature such as excellent redox active, good environment compatibility and abundant raw material sources, simultaneously compared to the cell type metal oxides such as Fe, Ni base, Co3O4There is more preferable stability, therefore it is considered to be one of the most promising electrode material for super capacitor.But, intrinsic Co3O4Electrical conductivity relatively low (10-4～10-2 Scm-1), and in charge and discharge process, Volume Changes is notable, seriously hinders its application in high-performance super capacitor.
In order to improve Co3O4Electric conductivity and stability, by itself and have superior electrical conductivity can and the Graphene of mechanical performance carry out being combined and obtain the favor of scientific research personnel.At present, domestic and international researcher obtains Graphene/Co by various preparation methods (such as hydro-thermal method/solvent-thermal method, sol-gel process, simple liquid phase reactor, chemical vapor deposition (CVD) etc.)3O4Composite, but wherein most preparation method still suffers from Graphene/Co3O4The problems such as nano material micro-structural is wayward and preparation condition is harsh.Ujjain et al. ( Electrochim.Acta , 2015,169:276-282) and utilize water heat transfer graphene nanobelt/Co3O4Nano particle composite material, Co3O4Nano particle (～60 nm) is dispersed on graphene nanobelt；At 5 mVs-1Sweep speed under, the specific capacity of this composite is 525 Fg-1.Although graphene nanobelt/Co3O4Nano particle composite material is than synthesized simple Co3O4Specific capacity have bigger lifting, but due to electrolyte diffusion length in electrode material shorter (20 nm), so bigger Co3O4Nano particle can not be by fully effective utilization in electrochemical reaction process.Liao et al. ( ACS Nano , 2015,9:5310-5317) and on carbon cloth, synthesize vertical orientated Graphene/Co by microwave plasma enhanced chemical gaseous phase deposition (MPECVD) and follow-up hydrothermal method3O4The composite of nano particle；At 1 mVs-1Sweep speed under, its volume and capacity ratio is up to 950 Fcm-3.Vertical-growth Graphene on carbon cloth result in the space that the internal existence of this combination electrode material is bigger.Therefore, in electrode material unit volume, contained active electrode material is restricted, and defines so-called " dead volume ".
Liquid laser irradiation/ablation is existing relevant report in terms of preparing high connductivity Graphene and ultramicro powder.As Huang et al. ( Carbon , 2011,49 (7): 2431-2436) and by pulse laser irradiation graphene oxide water solution, by graphene oxide in-situ reducing and obtain high conductivity.James et al. ( ACS Catal. , 2013,3:2497-2500) and utilize liquid laser ablation to obtain small size (2.5 nm) Co being evenly distributed3O4Nano particle.But, prepare aspect at the graphene-based combination electrode material of ultracapacitor, liquid laser irradiation/ablation preparation yet there are no relevant report.Therefore those skilled in the art are devoted to develop a kind of Graphene/ultra micro Co3O4Liquid laser irradiation/ablation the preparation method of Particles dispersed electrode material, the method will have important scientific research meaning and using value.
Summary of the invention
Present invention aim to overcome that the deficiency of above-mentioned existing technology of preparing, it is provided that a kind of simple, novel Graphene/ultra micro Co3O4The preparation method of Particles dispersed electrode material.When combination electrode material prepared by the method is used as electrode material for super capacitor, improves the volume capacity of this electrode greatly, solve conventional method and be difficult to high volume capacity a difficult problem for high-purity preparation.
For achieving the above object, the invention provides a kind of Graphene/ultra micro Co3O4Liquid laser irradiation/ablation the preparation method of Particles dispersed electrode material.The technical solution of the present invention is: by graphene oxide and the Co of different proportion3O4Presoma mixing, under the conditions of different pulse lasers prepare Graphene/ultra micro Co3O4Particulate composite.
Above-mentioned Graphene/ultra micro Co3O4The preparation method of Particles dispersed electrode material, specifically comprises the following steps that
(1) by Co3O4Nano particle presoma and graphene oxide press different proportion ultrasonic disperse in different solvents, Co3O4Nano particle with graphene oxide ratio is: 0.1%～10%:90%～99.9%.
(2) using above-mentioned mixed solution as liquid phase target, magnetic stirring apparatus continuously stirred under, by pulse laser irradiation/ablation liquid phase target, the condition of work of laser is: wavelength 248 nm～the laser of 1064 nm, frequency 1～30 Hz, energy density is 0.1～10 J pulse-1cm-2, exposure time is 10～1000 min, has reacted rear centrifuge washing and i.e. can get Graphene/Co3O4Particles dispersed electrode material.
Graphene oxide and Co is disperseed in being embodied as of the present invention3O4Presoma used by liquid flux be water, ethanol.
In a preferred embodiment of the invention for laser, described frequency is preferably 1～10 Hz, and energy density is 0.1～0.8 J pulse-1cm-2, exposure time is 20～100 min.
Compared with prior art, the invention have the benefit that
(1) preparation process of the present invention has only to laser irradiation/ablation graphene oxide and Co3O4The liquid solution of precursor, it is not necessary to other redox condition and reagent and the experimental provision of complexity, condition is easily-controllable, and technique is simple, low cost, solves conventional manufacturing process complicated and be difficult to control to the difficult problem of composite micro-structure and purity.
(2) Graphene/Co prepared by the inventive method3O4In Particles dispersed electrode material, Co3O4It is tightly combined with Graphene, and is dispersed on Graphene, Co simultaneously3O4Pattern, the equal controllable of size.
(3) Graphene/Co prepared by the present invention3O4Particles dispersed electrode material has good electric conductivity and high tap density, can improve this electrode material greatly as volume capacity during electrode of super capacitor.
Below with reference to accompanying drawing, the technique effect of the design of the present invention, concrete material structure and generation is described further, to be fully understood from the purpose of the present invention, feature and effect.
Accompanying drawing explanation
Fig. 1 is the Graphene/ultra micro Co of the embodiment of the present invention 1 preparation3O4The XRD spectrum of particulate composite；
Fig. 2 is the Graphene/ultra micro Co of the embodiment of the present invention 1 preparation3O4The transmission electron microscope picture of particulate composite；
Fig. 3 is the Graphene/ultra micro Co of the embodiment of the present invention 1 preparation3O4The high-resolution-ration transmission electric-lens figure of particulate composite；
Fig. 4 is the Graphene/ultra micro Co of the embodiment of the present invention 1 preparation3O4Particulate composite constant current charge-discharge curve under different current densities.
Claims (6)
1. Graphene/ultra micro Co3O4Liquid laser irradiation/ablation the preparation method of Particles dispersed electrode material, it is characterised in that specifically comprise the following steps that
(1) different proportion is pressed by Co3O4Nano particle presoma and graphene oxide are sufficiently mixed in different solvents；
(2) using above-mentioned gained mixed solution as liquid phase target, under the conditions of different pulse lasers, carry out irradiation/ablation, prepare Graphene/ultra micro Co3O4Particulate composite.
Preparation method the most according to claim 1, it is characterised in that Co used in step (1)3O4Nano particle presoma is commercialization Co3O4Particle, the Co of laboratory synthesis3O4Particle.
Preparation method the most according to claim 1, it is characterised in that solvent used in step (1) is: water, ethanol.
Preparation method the most according to claim 1, it is characterised in that Co in step (1)3O4Nano particle with graphene oxide ratio is: 0.1%～10%:90%～99.9%.
Preparation method the most according to claim 1, it is characterised in that in step (2), the condition of work of laser is: wavelength 248 nm～1064 nm, frequency 1～30 Hz, energy density is 0.1～10 J pulse-1cm-2, exposure time is 10～1000 min.
Preparation method the most according to claim 2, it is characterised in that for laser in step (2), described frequency is preferably 1～10 Hz, and energy density is 0.1～0.8 J pulse-1cm-2, exposure time is 20～100 min.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106398802A (en) * | 2016-09-07 | 2017-02-15 | 济南大学 | Rapid laser preparing method for composite with graphene loaded with spherical inorganic fullerene molybdenum disulfide |
| CN106784828A (en) * | 2016-12-30 | 2017-05-31 | 尹宗杰 | A kind of layer type casting moulding Graphene metallic composite and preparation method |
| CN106784596A (en) * | 2016-11-18 | 2017-05-31 | 杭州电子科技大学 | One kind prepares binder free Graphene/SnO using laser irradiation original position2The method of combination electrode |
| CN106800292A (en) * | 2017-01-16 | 2017-06-06 | 王奉瑾 | The preparation method of graphene oxide and Graphene |
| CN107731544A (en) * | 2017-09-06 | 2018-02-23 | 济南大学 | A kind of graphene zinc ferrite combination electrode material and preparation method thereof |
| CN109179398A (en) * | 2018-10-24 | 2019-01-11 | 国家纳米科学中心 | A kind of metal oxide containing precious metals nanocomposite, preparation method and the usage |
| CN109326789A (en) * | 2018-12-11 | 2019-02-12 | 济南大学 | A kind of graphene coated cobalt acid zinc combination electrode material and preparation method thereof |
| CN109590008A (en) * | 2018-12-25 | 2019-04-09 | 天津大学 | The preparation method of Laser synthesizing Lacking oxygen is adjustable cobaltosic oxide nitrogen-doped graphene |
| CN113634255A (en) * | 2021-08-24 | 2021-11-12 | 武汉理工大学 | Loaded Co3O4Preparation method of granular nano carbon composite catalytic material |
| CN114093682A (en) * | 2021-11-12 | 2022-02-25 | 西安交通大学 | Laser preparation method and application of graphene/Co-CoO composite electrode material |
| CN115466918A (en) * | 2022-09-06 | 2022-12-13 | 哈尔滨工程大学 | Modification method of whisker/fiber surface textured nano bump structure and strengthening and toughening application thereof |
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| CN103972496A (en) * | 2014-04-10 | 2014-08-06 | 山东润昇电源科技有限公司 | Co3O4/graphene electrode material preparation method through hydro-thermal coupling spray pyrolysis |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106398802A (en) * | 2016-09-07 | 2017-02-15 | 济南大学 | Rapid laser preparing method for composite with graphene loaded with spherical inorganic fullerene molybdenum disulfide |
| CN106784596A (en) * | 2016-11-18 | 2017-05-31 | 杭州电子科技大学 | One kind prepares binder free Graphene/SnO using laser irradiation original position2The method of combination electrode |
| CN106784828A (en) * | 2016-12-30 | 2017-05-31 | 尹宗杰 | A kind of layer type casting moulding Graphene metallic composite and preparation method |
| CN106800292A (en) * | 2017-01-16 | 2017-06-06 | 王奉瑾 | The preparation method of graphene oxide and Graphene |
| CN107731544B (en) * | 2017-09-06 | 2019-06-25 | 济南大学 | A kind of graphene zinc ferrite combination electrode material and preparation method thereof |
| CN107731544A (en) * | 2017-09-06 | 2018-02-23 | 济南大学 | A kind of graphene zinc ferrite combination electrode material and preparation method thereof |
| CN109179398A (en) * | 2018-10-24 | 2019-01-11 | 国家纳米科学中心 | A kind of metal oxide containing precious metals nanocomposite, preparation method and the usage |
| CN109326789A (en) * | 2018-12-11 | 2019-02-12 | 济南大学 | A kind of graphene coated cobalt acid zinc combination electrode material and preparation method thereof |
| CN109326789B (en) * | 2018-12-11 | 2021-11-30 | 济南大学 | Graphene-coated zinc cobaltate composite electrode material and preparation method thereof |
| CN109590008A (en) * | 2018-12-25 | 2019-04-09 | 天津大学 | The preparation method of Laser synthesizing Lacking oxygen is adjustable cobaltosic oxide nitrogen-doped graphene |
| CN113634255A (en) * | 2021-08-24 | 2021-11-12 | 武汉理工大学 | Loaded Co3O4Preparation method of granular nano carbon composite catalytic material |
| CN114093682A (en) * | 2021-11-12 | 2022-02-25 | 西安交通大学 | Laser preparation method and application of graphene/Co-CoO composite electrode material |
| CN114093682B (en) * | 2021-11-12 | 2022-10-25 | 西安交通大学 | Laser preparation method and application of graphene/Co-CoO composite electrode material |
| CN115466918A (en) * | 2022-09-06 | 2022-12-13 | 哈尔滨工程大学 | Modification method of whisker/fiber surface textured nano bump structure and strengthening and toughening application thereof |
| CN115466918B (en) * | 2022-09-06 | 2024-04-16 | 哈尔滨工程大学 | Whisker/fiber surface texturing nano bump structure modification method and toughening application thereof |
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Denomination of invention: A preparation method of graphene/ultrafine cobalt tetroxide particle composite electrode material Effective date of registration: 20230828 Granted publication date: 20181123 Pledgee: Levin commercial bank Limited by Share Ltd. Ji'nan branch Pledgor: JINAN RICHNES ELECTRONIC Co.,Ltd. Registration number: Y2023980054077 |
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