CN105449210A - Preparation method for porous graphene micro-sheet - Google Patents
Preparation method for porous graphene micro-sheet Download PDFInfo
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- CN105449210A CN105449210A CN201510794125.0A CN201510794125A CN105449210A CN 105449210 A CN105449210 A CN 105449210A CN 201510794125 A CN201510794125 A CN 201510794125A CN 105449210 A CN105449210 A CN 105449210A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method for a porous graphene micro-sheet. The preparation method is characterized by comprising the following steps: 1) pretreatment of graphite: putting graphite into a mixed solution consisting of an oxidizing agent and intercalator, performing ultrasonic stirring for 3-5h; washing, filtering and drying the obtained product, and putting the product into a muffle furnace, and processing the product in nitrogen atmosphere at a high temperature of 600-1,200 DEG C for 2-6h to obtain an expanded graphite product for use; and 2) preparation of the porous graphene micro-sheet: dissolving the expanded graphite obtained in the above step into a certain amount of deionized water, adding 0.1-2wt% of surfactant, performing ultrasonic stirring for 0.5-2h, and then adding a certain amount of pore forming agent, and putting into the muffle furnace under the N2 protective atmosphere for processing for 1-3h; washing the obtained product by dilute acid or dilute alkali and the deionized water solution for multiple times; drying the product in a vacuum drying oven for 2-6h to obtain the porous graphene micro-sheet. The porous graphene micro-sheet prepared by the preparation method provided by the invention is relatively high in specific surface area (850-1,000 m2/g); and due to the porous structure, the diffusion rate of the lithium ions can be improved, and a relatively better electrochemical performance can be obtained.
Description
Technical field
The present invention relates to field of graphene technology, a kind of preparation method of porous graphene microplate is particularly provided.
Background technology
The special two-dimension plane structure of Graphene gives the electronic conductance ability of its excellence, and the electron mobility on its face can reach 2.5 × 105cm2/V, is 100 times of silicon.And it can tolerate the current density of 1 ~ 2 × 108A/cm2.These performances all make it have application prospect widely at high performance electronics and battery material field.For lithium ion battery, its high electron mobility is conducive to the transmission of electronics, but its stable planar structure limits the transmission of Li+ between graphene planes, effective three-dimensional lithium ion tunnel cannot be formed, therefore there is lower lithium ionic mobility, limit the performance of battery capacity and high rate performance etc.Therefore preparation has the Graphene of special appearance, makes it have the important way that excellent lithium ion transport passage is Development of Novel lithium ion battery material.The invention provides a kind of low cost preparation method of porous graphene microplate, the Graphene impurity content of gained is few, and the number of plies is lower 1 ~ 10 layer, and thickness is about 0.3 ~ 5nm.
Summary of the invention
In view of this, the present invention is directed to the disappearance of prior art existence, the object of the present invention is to provide a kind of preparation method of porous graphene microplate, the porous graphene microplate obtained by it has good electric conductivity.
For achieving the above object, the present invention adopts following technical scheme: a kind of preparation method of porous graphene microplate, includes following steps:
1) pre-treatment of graphite:
Graphite is placed in the mixed solution be made up of oxidant and intercalator, ultrasonic agitation process 3 ~ 5h at 20 ~ 60 DEG C, the product obtained is placed in Muffle furnace through washing, filtration, drying, processes 2 ~ 6h, obtain expanded graphite product for subsequent use in nitrogen atmosphere and under 600 ~ 1200 DEG C of high temperature;
2) preparation of porous graphene microplate:
Upper step products therefrom expanded graphite is dissolved in a certain amount of deionized water, add the surfactant of 0.1 ~ 2wt%, ultrasonic agitation 0.5 ~ 2h, add a certain amount of pore creating material again, the mass ratio of pore creating material and expanded graphite is: 0.1 ~ 1:1, continue ultrasonic agitation 1 ~ 5h, then solvent flashing at 100 DEG C of temperature, is placed in N by gained solid
2in Muffle furnace under atmosphere protection, under 600 ~ 1200 DEG C of high temperature, process 1 ~ 3h, products therefrom, after diluted acid or diluted alkaline and deionized water solution repeatedly wash, with the temperature drying 2 ~ 6h of 30 ~ 50 DEG C in vacuum drying oven, obtains porous graphene microplate.
As a kind of preferred version, described surfactant is CTAB, neopelex, polyethylene glycol (PEG), polyvinylpyrrolidone or Pluronic series of products.
As a kind of preferred version, described pore creating material is H
3pO
4, KOH or ZnCl
2.
As a kind of preferred version, described oxidant includes hydrogen peroxide, potassium permanganate, ammonium persulfate; Described intercalator includes sulfuric acid, acetic acid, nitric acid, formic acid, phosphoric acid, perchloric acid.
The present invention compared with prior art has obvious advantage and beneficial effect, is specially: the porous graphene microplate that the inventive method is prepared has higher specific area (850 ~ 1000m
2/ g), loose structure is conducive to the diffusion rate improving lithium ion, therefore as lithium ion battery negative material, has higher ionic conductance, thus has good chemical property; The inventive method technique is simple, abundant raw material, easy to operate, and production equipment is few, thus reduces costs further, easy to utilize, is suitable for large-scale production.
Embodiment
Embodiment 1
A preparation method for porous graphene microplate, includes following steps:
1) pre-treatment of graphite:
Graphite is placed in the mixed solution be made up of oxidant and intercalator, ultrasonic agitation process 5h at 20 DEG C, the product obtained is placed in Muffle furnace through washing, filtration, drying, processes 6h, obtain expanded graphite product for subsequent use in nitrogen atmosphere and under 1200 DEG C of high temperature; This oxidant is hydrogen peroxide; This intercalator is sulfuric acid.
2) preparation of porous graphene microplate:
Upper step products therefrom expanded graphite is dissolved in a certain amount of deionized water, add the surfactant of 0.1wt%, ultrasonic agitation 0.5h, add a certain amount of pore creating material again, the mass ratio of pore creating material and expanded graphite is: 0.1:1, continue ultrasonic agitation 5h, then solvent flashing at 100 DEG C of temperature, is placed in N by gained solid
2in Muffle furnace under atmosphere protection, under 1200 DEG C of high temperature, process 1h, products therefrom is after diluted acid or diluted alkaline and deionized water solution repeatedly wash, and with the dry 6h of the temperature of 30 DEG C in vacuum drying oven, obtain porous graphene microplate, its specific area is 850m
2/ g.This surfactant is CTAB; This pore creating material is H
3pO
4.
Embodiment 2
A preparation method for porous graphene microplate, includes following steps:
1) pre-treatment of graphite:
Graphite is placed in the mixed solution be made up of oxidant and intercalator, ultrasonic agitation process 3h at 60 DEG C, the product obtained is placed in Muffle furnace through washing, filtration, drying, processes 6h, obtain expanded graphite product for subsequent use in nitrogen atmosphere and under 600 DEG C of high temperature; This oxidant is potassium permanganate; This intercalator is acetic acid.
2) preparation of porous graphene microplate:
Upper step products therefrom expanded graphite is dissolved in a certain amount of deionized water, add the surfactant of 2wt%, ultrasonic agitation 2h, add a certain amount of pore creating material again, the mass ratio of pore creating material and expanded graphite is: 1:1, continue ultrasonic agitation 1h, then solvent flashing at 100 DEG C of temperature, is placed in N by gained solid
2in Muffle furnace under atmosphere protection, under 600 DEG C of high temperature, process 3h, products therefrom is after diluted acid or diluted alkaline and deionized water solution repeatedly wash, and with the dry 2h of the temperature of 50 DEG C in vacuum drying oven, obtain porous graphene microplate, its specific area is 900m
2/ g.This surfactant is neopelex; This pore creating material is KOH.
Embodiment 3
A preparation method for porous graphene microplate, includes following steps:
1) pre-treatment of graphite:
Graphite is placed in the mixed solution be made up of oxidant and intercalator, ultrasonic agitation process 5h at 30 DEG C, the product obtained is placed in Muffle furnace through washing, filtration, drying, processes 3h, obtain expanded graphite product for subsequent use in nitrogen atmosphere and under 1000 DEG C of high temperature; This oxidant is ammonium persulfate; Described intercalator is nitric acid.
2) preparation of porous graphene microplate:
Upper step products therefrom expanded graphite is dissolved in a certain amount of deionized water, add the surfactant of 1wt%, ultrasonic agitation 1h, add a certain amount of pore creating material again, the mass ratio of pore creating material and expanded graphite is: 0.5:1, continue ultrasonic agitation 3h, then solvent flashing at 100 DEG C of temperature, is placed in N by gained solid
2in Muffle furnace under atmosphere protection, under 800 DEG C of high temperature, process 2h, products therefrom is after diluted acid or diluted alkaline and deionized water solution repeatedly wash, and with the dry 4h of the temperature of 40 DEG C in vacuum drying oven, obtain porous graphene microplate, its specific area is 980m
2/ g.This surfactant polyethylene (PEG); This pore creating material is ZnCl
2.
Embodiment 4
A preparation method for porous graphene microplate, includes following steps:
1) pre-treatment of graphite:
Graphite is placed in the mixed solution be made up of oxidant and intercalator, ultrasonic agitation process 4h at 50 DEG C, the product obtained is placed in Muffle furnace through washing, filtration, drying, processes 4h, obtain expanded graphite product for subsequent use in nitrogen atmosphere and under 800 DEG C of high temperature; This oxidant is hydrogen peroxide; Described intercalator includes formic acid.
2) preparation of porous graphene microplate:
Upper step products therefrom expanded graphite is dissolved in a certain amount of deionized water, add the surfactant of 1.3wt%, ultrasonic agitation 1.5h, add a certain amount of pore creating material again, the mass ratio of pore creating material and expanded graphite is: 0.8:1, continue ultrasonic agitation 4h, then solvent flashing at 100 DEG C of temperature, is placed in N by gained solid
2in Muffle furnace under atmosphere protection, under 1000 DEG C of high temperature, process 2h, products therefrom is after diluted acid or diluted alkaline and deionized water solution repeatedly wash, and with the dry 5h of the temperature of 35 DEG C in vacuum drying oven, obtain porous graphene microplate, its specific area is 1000m
2/ g.This surfactant is polyvinylpyrrolidone; This pore creating material is ZnCl
2.
Of the present inventionly to focus on: the porous graphene microplate that the inventive method is prepared has higher specific area (850 ~ 1000m
2/ g), loose structure is conducive to the diffusion rate improving lithium ion, therefore as lithium ion battery negative material, has higher ionic conductance, thus has good chemical property; The inventive method technique is simple, abundant raw material, easy to operate, and production equipment is few, thus reduces costs further, easy to utilize, is suitable for large-scale production.
The above, it is only preferred embodiment of the present invention, not technical scope of the present invention is imposed any restrictions, thus every according to technical spirit of the present invention to any trickle amendment made for any of the above embodiments, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
Claims (4)
1. a preparation method for porous graphene microplate, is characterized in that: include following steps:
1) pre-treatment of graphite:
Graphite is placed in the mixed solution be made up of oxidant and intercalator, ultrasonic agitation process 3 ~ 5h at 20 ~ 60 DEG C, the product obtained is placed in Muffle furnace through washing, filtration, drying, processes 2 ~ 6h, obtain expanded graphite product for subsequent use in nitrogen atmosphere and under 600 ~ 1200 DEG C of high temperature;
2) preparation of porous graphene microplate:
Upper step products therefrom expanded graphite is dissolved in a certain amount of deionized water, add the surfactant of 0.1 ~ 2wt%, ultrasonic agitation 0.5 ~ 2h, add a certain amount of pore creating material again, the mass ratio of pore creating material and expanded graphite is: 0.1 ~ 1:1, continue ultrasonic agitation 1 ~ 5h, then solvent flashing at 100 DEG C of temperature, is placed in N by gained solid
2in Muffle furnace under atmosphere protection, under 600 ~ 1200 DEG C of high temperature, process 1 ~ 3h, products therefrom, after diluted acid or diluted alkaline and deionized water solution repeatedly wash, with the temperature drying 2 ~ 6h of 30 ~ 50 DEG C in vacuum drying oven, obtains porous graphene microplate.
2. the preparation method of a kind of porous graphene microplate according to claim 1, is characterized in that: described surfactant is CTAB, neopelex, polyethylene glycol (PEG), polyvinylpyrrolidone or Pluronic series of products.
3. the preparation method of a kind of porous graphene microplate according to claim 1, is characterized in that: described pore creating material is H
3pO
4, KOH or ZnCl
2.
4. the preparation method of a kind of porous graphene microplate according to claim 1, is characterized in that: described oxidant includes hydrogen peroxide, potassium permanganate, ammonium persulfate; Described intercalator includes sulfuric acid, acetic acid, nitric acid, formic acid, phosphoric acid, perchloric acid.
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Cited By (8)
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CN106025202A (en) * | 2016-05-25 | 2016-10-12 | 福建翔丰华新能源材料有限公司 | Preparation method of silicon-graphene compound conductive paste |
CN106129340A (en) * | 2016-08-12 | 2016-11-16 | 长兴聚优电源有限公司 | A kind of preparation method of lead carbon battery negative pole |
CN107394158A (en) * | 2017-07-21 | 2017-11-24 | 张娟 | A kind of method that the compound lithium cell cathode material of silicon-carbon is prepared based on expanded graphite |
CN107403916A (en) * | 2017-07-14 | 2017-11-28 | 贵州鼎玺烯材高科技有限公司 | A kind of positive material for lithium-sulfur battery with the more lithium sulfides of graphene conductive network constraint |
CZ307072B6 (en) * | 2016-11-24 | 2017-12-27 | Masarykova Univerzita | A method of preparing graphenoids and a graphhenoid obtainable by this method |
CN109256547A (en) * | 2018-09-05 | 2019-01-22 | 合肥国轩电池材料有限公司 | A kind of preparation method of porous graphene-lithium iron phosphate positive material |
CN110575848A (en) * | 2019-09-19 | 2019-12-17 | 燕山大学 | preparation method of catalyst for catalyzing ozone to oxidize volatile organic compounds |
CN113200541A (en) * | 2021-03-29 | 2021-08-03 | 中南大学 | Method for recycling graphite negative electrode of waste battery |
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CN107394158A (en) * | 2017-07-21 | 2017-11-24 | 张娟 | A kind of method that the compound lithium cell cathode material of silicon-carbon is prepared based on expanded graphite |
CN109256547A (en) * | 2018-09-05 | 2019-01-22 | 合肥国轩电池材料有限公司 | A kind of preparation method of porous graphene-lithium iron phosphate positive material |
CN110575848A (en) * | 2019-09-19 | 2019-12-17 | 燕山大学 | preparation method of catalyst for catalyzing ozone to oxidize volatile organic compounds |
CN110575848B (en) * | 2019-09-19 | 2020-11-27 | 燕山大学 | Preparation method of catalyst for catalyzing ozone to oxidize volatile organic compounds |
CN113200541A (en) * | 2021-03-29 | 2021-08-03 | 中南大学 | Method for recycling graphite negative electrode of waste battery |
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Application publication date: 20160330 |