CN107026259A - A kind of graphene combination electrode material and preparation method and application - Google Patents
A kind of graphene combination electrode material and preparation method and application Download PDFInfo
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- CN107026259A CN107026259A CN201610069008.2A CN201610069008A CN107026259A CN 107026259 A CN107026259 A CN 107026259A CN 201610069008 A CN201610069008 A CN 201610069008A CN 107026259 A CN107026259 A CN 107026259A
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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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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 kind of graphene combination electrode material and preparation method and application.Graphene combination electrode material of the present invention is made up of lithium ion battery electrode material and the surface coated graphene of the lithium ion battery electrode material；The thickness of the graphene is between 0.3~5nm.Its preparation method, comprises the following steps：1) lithium ion cell electrode raw material is calcined, calcining cools after finishing；2) by step 1) processing the lithium ion battery electrode material heating, then pass to carbon source carry out chemical vapour deposition reaction, that is, obtain the graphene combination electrode material.Preparation method of the present invention is simple, and controllability is high, is adapted to industrial continuous production.
Description
Technical field
The present invention relates to a kind of graphene combination electrode material and preparation method and application, belong to Material Field.
Background technology
Lithium ion battery is a kind of common electrochemical energy storing device, due to its stable cycle performance, high-energy-density,
The advantage such as environment friendly and security, is widely used in electric consumers.The ultimate of lithium ion battery will
Seeking Truth light weight, small volume, long lifespan, and can quickly discharge and recharge, and in extreme conditions can also
Use.However, traditional lithium ion battery is difficult to meet such demand, accordingly, it would be desirable to seek new electrode material
To meet the demand of energy storage.Due to the capacity of superelevation, metal oxide, tin, the emerging negative material such as silicon draws
Increasing concern has been played, however, these electrode active materials are electric insulations, has been unfavorable for the transmission of electronics, and
And higher capacity also brings the cycle performance of difference.
The content of the invention
It is an object of the invention to provide a kind of graphene combination electrode material and preparation method and application.It is prepared by the present invention
Method is simple, and controllability is high, is adapted to industrial continuous production.
The graphene combination electrode material that the present invention is provided, it is by lithium ion battery electrode material and the lithium ion battery
The graphene composition of electrode material surface cladding；
The thickness of the graphene is 0.3~10nm.
In above-mentioned electrode material, the lithium ion battery electrode material is silicon monoxide, silica, silicon, oxidation
At least one of titanium, manganese oxide, tin oxide and iron oxide；
The number of plies of the graphene can be 1~10 layer.
Present invention also offers the preparation method of above-mentioned electrode material, comprise the following steps：1) by lithium ion battery battery
Pole raw material calcining, calcining cools after finishing；
2) by step 1) processing the lithium ion battery electrode material heating, then pass to carbon source carry out chemical gaseous phase
Deposition reaction, that is, obtain the graphene combination electrode material.
In above-mentioned method, the lithium ion cell electrode raw material is silicon monoxide, silica, titanium oxide, oxidation
At least one of manganese, tin oxide and iron oxide；
The calcining uses tube furnace.
In above-mentioned method, the temperature of the calcining can be 50~1300 DEG C, concretely 100 DEG C, 200 DEG C, 1200 DEG C,
100~200 DEG C, 200~1200 DEG C or 100~1200 DEG C；
The time of the calcining can be 30~300min, concretely 60min, 300min or 60~300min；
The atmosphere of the calcining is at least one of air, argon gas, hydrogen and nitrogen atmosphere；
Temperature after the cooling is room temperature, and the room temperature is generally referred to as 10~30 DEG C, concretely 25 DEG C, 10~25 DEG C
Or 25~30 DEG C.
In above-mentioned method, the tube furnace is atmospheric pipe still equipment or low-pressure tube type furnace apparatus；
When using the low-pressure tube type furnace apparatus, the vacuum of the calcining can be 1~1000Pa.
In above-mentioned method, step 2) in, the speed of the heating can be 5~100 DEG C/min, concretely 20 DEG C
/min；Temperature after the heating can for 200~1300 DEG C, concretely 600 DEG C, 800 DEG C, 1000 DEG C or
600~1000 DEG C；
The carbon source is methane, ethene, propylene, acetylene, alcohol vapor or benzoic acid steam；
The chemical vapour deposition reaction is carried out in an inert atmosphere；
The chemical vapour deposition reaction is using aumospheric pressure cvd equipment, low pressure chemical vapor deposition equipment or waits
Gas ions strengthen chemical vapor depsotition equipment.
In the present invention, the inert atmosphere inputs the carbon source to the chemical gaseous phase as the carrier gas of the carbon source
In the equipment of deposition reaction.
In above-mentioned method, the temperature of the chemical vapour deposition reaction can be 300~1100 DEG C, concretely 600 DEG C,
800 DEG C, 1000 DEG C, 600~800 DEG C, 800~1000 DEG C or 600~1000 DEG C；
The time of the chemical vapour deposition reaction can be 10~360min, concretely 60min.
In above-mentioned method, the inert atmosphere is at least one of argon gas, nitrogen, carbon dioxide and hydrogen；
The percentage composition that the carbon source accounts for the cumulative volume of the carbon source and the inert atmosphere is 0.5%~30%, specifically may be used
For 0.5%, 2%, 0.5~2%, 0.5~10% or 0.5~20%；
When using low pressure chemical vapor deposition equipment, the vacuum of the chemical vapour deposition reaction is 1~1000Pa.
Graphene combination electrode material of the present invention is applied in electrochemical energy storing device.
The present invention has advantages below：
The method for the graphene coated electrode material that the present invention is provided, technical process is simple, and controllability is high, is adapted to industry
Continuous production.This method has played the advantage that conventional chemical vapor sedimentation prepares high-quality graphene, obtains high-quality
The electrode material of the graphene coated of amount, electrode material-graphene composite wood that and liquid phase method good compared to mechanical mixture is obtained
Material, the graphene quality of this method is higher, and surface is without functional group, and controllability is higher, can control the bag of graphene
The amount of covering.
Brief description of the drawings
The pictorial diagram for the combination electrode material that Fig. 1 is prepared for the present invention using silicon monoxide.
The electron scanning micrograph for silicon monoxide-graphene composite material that Fig. 2 prepares for the present invention.
The transmission electron microscope photo for silicon monoxide-graphene composite material that Fig. 3 prepares for the present invention.
The Raman spectrogram for silicon monoxide-graphene composite material that Fig. 4 prepares for the present invention.
The electric conductivity measurement for silicon monoxide-graphene composite material that Fig. 5 prepares for the present invention.
The test of the battery performance for silicon monoxide-graphene composite material that Fig. 6 (a) prepares for the present invention.Fig. 6
(b) it is check experiment, the battery performance test of silicon monoxide-absorbent charcoal composite material.
The scanning electron micrograph for titanium dioxide-graphene combination electrode material that Fig. 7 prepares for the present invention.
Embodiment
Experimental method used in following embodiments is conventional method unless otherwise specified.
Material, reagent used etc., unless otherwise specified, are commercially obtained in following embodiments.
Embodiment 1, prepare silicon monoxide-graphene combination electrode material
1) silicon monoxide powder is placed in atmospheric pipe still 1200 DEG C of precalcining 5h under an argon atmosphere so that an oxygen
Disproportionated reaction occurs for SiClx, obtains the mixed phase of silica, silicon and silica, is cooled to 25 DEG C；
2) by step 1) obtained mixed phase is put into quartz boat, and be put into chemical vapor deposition stove.This sets
It is standby to be heated to 1000 DEG C with 20 DEG C/min heating rate, methane (argon gas is then passed through under argon gas, hydrogen shield
The carrier gas of methane is also served as with the gaseous mixture of hydrogen, carbon-source gas methane accounts for carbon source and the percentage of carrier gas cumulative volume is
0.5%) reacted, methane with vapor reaction presoma precalcining silicon oxide surface carry out chemisorbed, into
Core and growth, the reaction time are 60min；
3) after reaction terminates, treat that equipment is cooled to 25 DEG C, obtain an oxygen of black powder material, i.e. graphene parcel
SiClx combination electrode material (i.e. graphene combination electrode material), as shown in Figure 1.
Silica-graphene composite material of the present invention maintains the microscopic appearance of silicon monoxide, as shown in Fig. 2 particle diameter chi
It is very little at 5 μm or so.The number of plies of graphene is within 1-10 layers, and thickness is between 0.3nm~5nm, as shown in Figure 3.
The quality of resulting graphene is as shown in Figure 4.Change of the growth time to electric conductivity caused by the regulation of graphene coated amount
Change as shown in Figure 5.
Using silicon monoxide-graphene combination electrode material of the present invention as negative pole, its performance of lithium ion battery is tested：
By silicon monoxide, conductive agent, organic solvent mix be made into slurry, be coated on copper as negative pole, using lithium piece as
Positive pole is assembled into half-cell and tests its cycle performance, presses with silicon monoxide-activated carbon composite electrode material as a control group
Photograph is assembled into half-cell with assemble method and tests its cycle performance.Ten before the battery performance of combination electrode material of the present invention
The circulation result in week is as shown in fig. 6, figure a is the lithium ion battery cyclicity of silicon monoxide-graphene combination electrode material
Can, its coulombic efficiency maintains more than 97%, and as shown in Fig. 6 (b), silicon monoxide-active carbon combined electrode material
Material, its coulombic efficiency drops to 85%, and the compound silicon monoxide electrode material cycle performance of this explanation graphene is more preferable,
Better than other kinds of combination electrode material.
Embodiment 2, using titanium dioxide be growth substrate prepare titanium dioxide-graphene combination electrode material
1) titanium dioxide powder is placed in atmospheric pipe still 200 DEG C of precalcining 1h in air atmosphere, removes surface water
Point, it is cooled to 25 DEG C；
2) titanium dioxide powder after calcining is put into quartz boat, and be put into chemical vapor deposition stove.The equipment
800 DEG C are heated to 20 DEG C/min heating rate, being then passed through ethene under argon gas, hydrogen shield is reacted,
Ethene carries out chemisorbed, nucleation and growth, reaction with vapor reaction presoma in the titanium dioxide surface of precalcining
Time is 60min, and carbon-source gas ethene accounts for carbon source and carrier gas (mixed gas of above-mentioned argon gas and hydrogen) cumulative volume
Percentage is 2%；
3) after reaction terminates, treat that equipment is cooled to 25 DEG C, obtain the oxidation of black powder material, i.e. graphene parcel
Silicon combination electrode material (i.e. graphene combination electrode material), its pattern is as shown in Figure 7.
Embodiment 3, using nanometer grade silica powder prepare silica-graphene combination electrode material
1) silicon-dioxide powdery is placed in atmospheric pipe still 100 DEG C of precalcining 1h in air atmosphere, removes surface
Moisture, is cooled to 25 DEG C；
2) silicon-dioxide powdery after calcining is put into quartz boat, and be put into chemical vapor deposition stove.The equipment
600 DEG C are heated to 20 DEG C/min heating rate, being then passed through ethene under argon gas, hydrogen shield is reacted,
Acetylene carries out chemisorbed, nucleation and growth, reaction with vapor reaction presoma in the silica surface of precalcining
Time is 60min, and carbon-source gas acetylene accounts for the hundred of carbon source and carrier gas (gaseous mixture of above-mentioned argon gas and hydrogen) cumulative volume
Fraction is 2%；
3) after reaction terminates, treat that equipment is cooled to 25 DEG C, obtain the dioxy of black powder material, i.e. graphene parcel
SiClx combination electrode material (i.e. graphene combination electrode material).
Claims (10)
1. a kind of graphene combination electrode material, it is characterised in that：It by lithium ion battery electrode material and the lithium from
The sub- surface coated graphene composition of battery electrode material；
The thickness of the graphene is between 0.3~5nm.
2. electrode material according to claim 1, it is characterised in that：The lithium ion battery electrode material is one
At least one of silica, silica, silicon, titanium oxide, manganese oxide, tin oxide and iron oxide；
The number of plies of the graphene is 1~10 layer.
3. the preparation method of the electrode material described in claim 1 or 2, comprises the following steps：1) by lithium-ion electric
Pond electrode material calcining, calcining cools after finishing；
2) by step 1) processing the lithium ion battery electrode material heating, then pass to carbon source carry out chemical gaseous phase
Deposition reaction, that is, obtain the graphene combination electrode material.
4. method according to claim 3, it is characterised in that：The lithium ion cell electrode raw material is an oxidation
At least one of silicon, titanium oxide, manganese oxide, tin oxide and iron oxide；
The calcining uses tube furnace.
5. the method according to claim 3 or 4, it is characterised in that：The temperature of the calcining is 50~1300 DEG C；
The time of the calcining is 30~300min；
The atmosphere of the calcining is at least one of air, argon gas, hydrogen and nitrogen atmosphere；
Temperature after the cooling is room temperature.
6. the method according to any one of claim 4 or 5, it is characterised in that：The tube furnace is normal pressure pipe
Formula furnace apparatus or low-pressure tube type furnace apparatus；
When using the low-pressure tube type furnace apparatus, the vacuum of the calcining is 1~1000Pa.
7. the method according to any one of claim 3-6, it is characterised in that：Step 2) in, the heating
Speed be 5~100 DEG C/min；Temperature after the heating is 200~1300 DEG C；
The carbon source is methane, ethene, propylene, acetylene, alcohol vapor or benzoic acid steam；
The chemical vapour deposition reaction is carried out in an inert atmosphere；
The chemical vapour deposition reaction is using aumospheric pressure cvd equipment, low pressure chemical vapor deposition equipment or waits
Gas ions strengthen chemical vapor depsotition equipment.
8. the method according to any one of claim 3-7, it is characterised in that：The chemical vapour deposition reaction
Temperature be 300~1100 DEG C；
The time of the chemical vapour deposition reaction is 10~360min.
9. the method according to claim 7 or 8, it is characterised in that：The inert atmosphere be argon gas, nitrogen,
At least one of carbon dioxide and hydrogen；
The percentage composition that the carbon source accounts for the cumulative volume of the carbon source and the inert atmosphere is 0.5%~30%；
When using low pressure chemical vapor deposition equipment, the vacuum of the chemical vapour deposition reaction is 1~1000Pa.
10. application of the graphene combination electrode material described in claim 1 or 2 in electrochemical energy storing device.
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| CN108658037A (en) * | 2018-04-27 | 2018-10-16 | 国家纳米科学中心 | A kind of graphene functionalized nanometer pinpoint and preparation method thereof |
| CN108682859A (en) * | 2018-04-25 | 2018-10-19 | 福建翔丰华新能源材料有限公司 | A kind of preparation method of graphene modification lithium-ion battery negative material |
| CN109285993A (en) * | 2017-07-19 | 2019-01-29 | 中国科学院过程工程研究所 | A kind of sulphur carbon flexible electrode material and its preparation method and application |
| CN109399620A (en) * | 2018-12-05 | 2019-03-01 | 中国电子科技集团公司第十三研究所 | A method of preparing the silicon carbide-based grapheme material of high mobility |
| CN109616630A (en) * | 2018-11-27 | 2019-04-12 | 哈尔滨工业大学（深圳） | The silico-carbo composite material and preparation method and lithium ion battery applications of a kind of uniform carbon film and vertical graphene dual cladding |
| CN109850908A (en) * | 2019-04-12 | 2019-06-07 | 中国科学院重庆绿色智能技术研究院 | A kind of preparation method and product of silica/graphene complex |
| CN109941990A (en) * | 2017-12-21 | 2019-06-28 | 中国科学院上海硅酸盐研究所 | A kind of preparation method of LiFePO 4 material surface coated graphite alkene |
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| CN111072019A (en) * | 2018-10-22 | 2020-04-28 | 中国科学院上海硅酸盐研究所 | Graphene hollow microsphere conductive powder for lithium battery and preparation method thereof |
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| CN108658037A (en) * | 2018-04-27 | 2018-10-16 | 国家纳米科学中心 | A kind of graphene functionalized nanometer pinpoint and preparation method thereof |
| CN111072019A (en) * | 2018-10-22 | 2020-04-28 | 中国科学院上海硅酸盐研究所 | Graphene hollow microsphere conductive powder for lithium battery and preparation method thereof |
| CN109616630B (en) * | 2018-11-27 | 2021-12-21 | 哈尔滨工业大学（深圳） | Silicon-carbon composite material with uniform carbon film and vertical graphene double coating, preparation method thereof and application of silicon-carbon composite material in lithium ion battery |
| CN109616630A (en) * | 2018-11-27 | 2019-04-12 | 哈尔滨工业大学（深圳） | The silico-carbo composite material and preparation method and lithium ion battery applications of a kind of uniform carbon film and vertical graphene dual cladding |
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| CN111403708B (en) * | 2020-03-25 | 2021-11-30 | 广东凯金新能源科技股份有限公司 | Lithium ion battery silicon monoxide composite negative electrode material and preparation method thereof, and lithium ion battery |
| CN111547710A (en) * | 2020-04-03 | 2020-08-18 | 新奥（内蒙古）石墨烯材料有限公司 | Graphene-based composite material and preparation method and application thereof |
| CN111547710B (en) * | 2020-04-03 | 2022-06-07 | 新奥（内蒙古）石墨烯材料有限公司 | Graphene-based composite material and preparation method and application thereof |
| CN111807376A (en) * | 2020-07-21 | 2020-10-23 | 北京石墨烯研究院 | Graphene modified silicon monoxide/carbon composite material and preparation method thereof |
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