CN103811757A - Graphene composite positive electrode material - Google Patents
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- CN103811757A CN103811757A CN201410087433.5A CN201410087433A CN103811757A CN 103811757 A CN103811757 A CN 103811757A CN 201410087433 A CN201410087433 A CN 201410087433A CN 103811757 A CN103811757 A CN 103811757A
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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
- H01M4/364—Composites as mixtures
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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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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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
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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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 relates to a graphene composite positive electrode material. The graphene composite positive electrode material is characterized in that graphene with a porous structure is selected, and is at a uniform dispersive phase in positive electrode material particles, and the mass ratio of graphene to the positive electrode material is (1:2) to (1:10); when the mass ratio of graphene to the positive electrode material is less than 1:6, a third component being 2-10% of the total mass of graphene and the positive electrode material is added. The graphene has a porous structure, can provide more ion transfer and diffusion channels and storage spaces; due to active substances which are distributed on holes, the influence on performances caused by structural variation can be alleviated. The composite material adopts a simple preparation technology, and can be in large scale easily.
Description
Technical field
The present invention relates to grapheme material, particularly grapheme composite positive electrode material, belongs to new energy materials technical field.
Background technology
China has become sale of automobile market the biggest in the world, and the continuous growth of consumption of petroleum and the continuous increase of pollutant emission have become the bottleneck of auto industry sustainable development.Energy-conservation and the new-energy automobile such as development hybrid electric vehicle, pure electric automobile, fuel-cell vehicle has become the task of top priority.At present, energy-conservation and new-energy automobile is also failed large-scale promotion, main or electrokinetic cell exists a series of problem, and for example, energy density is lower, and bulking value is large, and useful life is short, and cost is higher, and operating temperature range is narrow, and the charging interval is long etc.In order to improve these adverse effects, people start with from material technology, have carried out the further investigation of electrokinetic cell.
Graphene is a kind of novel Two-dimensional Carbon based nano-material, and its unique performance has attracted a lot of people's research interest, is a kind of very promising material that is applied to field of batteries.The Chinese patent of application publication number CN 103007927 A discloses the preparation method of a kind of lithium-air battery platinum/graphen catalyst, the Chinese patent of application publication number CN 103035409 A discloses graphene combination electrode and its preparation method and application, and the Chinese patent of application publication number CN 102891311 A discloses a kind of silicon/carbon/graphite in lithium ion batteries alkene-Li (Ni
xco
ymn
z) O
2combination electrode material and preparation method thereof, the Chinese patent of application publication number CN 103050692 A discloses a kind of preparation method of Graphene-manganese silicate of lithium positive electrode, and the Chinese patent of application publication number CN 102903907 A discloses the graphene-supported LiNi of high cycle performance
0.5mn
0.5o
2the preparation method of positive electrode, the Chinese patent of application publication number CN 103035417 A discloses low cost and has prepared ultracapacitor MnO
2the method of/graphene combination electrode material, the Chinese patent of application publication number CN 103013056 A discloses a kind of Graphene/MnO
2/ Conjugated Polymer Composites and its preparation method and application.
Graphene and positive active material composition composite material can improve the performance of battery device, but very easily reunite together because the two-dimensional nano lamellar structure of Graphene makes it, and the performance advantage of Graphene can not be brought into play greatly.Recently, people begin one's study and have the preparing high-specific surface area graphene material of pore structure, for example, the Chinese patent of application publication number CN 102115069 A discloses has Graphene of loose structure and preparation method thereof, the Chinese patent of application publication number CN 102107868 A discloses a kind of preparation method of porous graphene material, the Chinese patent of application publication number CN 102757036 A discloses the preparation method of porous graphene, the Chinese patent of application publication number CN 102992313 A discloses high-ratio surface Graphene of a kind of mesopore prosperity and preparation method thereof, the Chinese patent of application publication number CN 102849734 A discloses a kind of preparation method of porous graphene, the Chinese patent of application publication number CN 102826542 A discloses a kind of high-ratio surface Activated Graphite alkene with mesopore, Its Preparation Method And Use, the Chinese patent of application publication number CN 103011152 A discloses a kind of grapheme material with loose structure and preparation method thereof, the Chinese patent of application publication number CN 102874800 A discloses a kind of activation Graphene of mesopore, its preparation method.
The above-mentioned grapheme material with loose structure focuses mostly in the preparation of material, and existing people starts high-specific surface area and porous graphene material to apply and energy storage field as active material at present.For example, the Chinese patent of application publication number CN 103011143 A discloses Graphene and preparation method thereof, ultracapacitor, the Chinese patent of application publication number CN 102923698 A discloses the preparation method of the three-dimensional porous Graphene of a kind of ultracapacitor, the Chinese patent of application publication number CN 102891014 A discloses Graphene electrodes active material and method for making and electrode material and electrode slice and application, the Chinese patent of application publication number CN 102992308 A discloses a kind of Graphene with high specific capacitance and preparation method thereof, the Chinese patent of application publication number CN 101982408 A discloses graphene three-dimensional structure body material and its preparation method and application.
Comprehensively above analysis can be found out, in order to expand the application of Graphene on battery, people start by original lamellar structure to the loose structure transition with high-specific surface area.But at present mainly using the Graphene with loose structure as but be applied to field of batteries with active material.
Summary of the invention
The object of the invention is to provide a kind of grapheme composite positive electrode material, Graphene used has loose structure, and the feature that specific area is high, not only can reduce or limit side effect in positive active material charge and discharge process, and can provide more diffusion admittance for the transmission of ion.
Technical scheme of the present invention is achieved in that grapheme composite positive electrode material, it is characterized in that: select and have loose structure Graphene, Graphene is dispersed phase in positive electrode particle, and the mass ratio of Graphene and positive electrode is 1:2~1:10; When wherein Graphene quality and positive electrode mass ratio are less than 1:6, add 2~10% the 3rd component of Graphene and positive electrode gross mass.
Described Graphene specific area is 1200~2300 m
2/ g.
Described positive electrode is LiMn
2o
4, LiFePO
4, Li
3v
2(PO4)
3, LiM
xmn
2-xo
4(M=Ni, Co, Fe, Cr, Cu), LiNi
xco
ymn
1-x-yo
2, (0 < x < 0.5,0 < y < 0.5), LiNi
1-xal
xo
2(0≤x≤0.6), LiCoO
2, Li
2mnSiO
4, Li
2feSiO
4, MnO
2, V
2o
5, NaVPO
4f, Na
2fePO
4f, NaNi
0.5mn
0.5o
2, Na
0.7mnO
2.05, ZnMn
xo
yone in (0 < x < 3, x:y=1.5~4.5).
The 3rd described component is a kind of in carbon nano-tube, expanded graphite, acetylene black, carbon nano-fiber or their combination.
Described composite positive pole preparation method is physical mixed, a kind of during chemical original position is compound or their combination.
Described physical mixed method be stir, a kind of in ultrasonic, ball milling or their combination, in mixed process, can be dry mixed, add solvent wet mixing or be dry mixed-wet mixing combination.
The concrete steps of described physical mixed method are as follows: take Graphene according to mass ratio and put in mixer, add solvent that Graphene is infiltrated completely, according to mass ratio, positive electrode or positive electrode and the 3rd component are added in mixer, after high-speed stirred is uniformly dispersed, dry, obtain combination electrode material.Described solvent is deionized water or ethanol.
Described chemical in-situ compounding process is that Graphene mixes with the raw material of synthetic positive electrode, forms combination electrode material in building-up process.
Described composite material can be used as the positive electrode of lithium ion battery, sodium-ion battery, Zinc ion battery, ultracapacitor.
Good effect of the present invention is that adopted Graphene has loose structure, not only can reduce or limit side effect in positive active material charge and discharge process, can provide more diffusion admittance and memory space for the transmission of ion.This composite material preparation process is simple, is easy to scale.Grapheme composite positive electrode material can be used as the electrode material of lithium ion battery, sodium-ion battery, Zinc ion battery and ultracapacitor etc.
Accompanying drawing explanation
Fig. 1 is that the composite positive pole of the embodiment of the present invention 1 is at 1M lithium sulfate electrolyte charge-discharge test curve.
Fig. 2 is that the composite positive pole of the embodiment of the present invention 1 is at 1M hexafluoro phosphorus lithium electrolyte charge-discharge test curve.
Embodiment
Below in conjunction with drawings and Examples, the present invention will be further described: described embodiment is the specific descriptions to claim of the present invention just, and claim includes but not limited to described embodiment content.
Embodiment 1
Taking specific area according to mass ratio 1:4 is 2200m
2/ g, the Graphene that aperture is 3~8nm and LiMn
2o
4.Graphene is put in the ball grinder of ball mill, added a small amount of ethanol to stir 2min, make Graphene complete wetting, add LiMn
2o
4continue ball milling 1h, take out the material having mixed, dry, obtain LiMn
2o
4/ graphene combination electrode material, makes pole piece with binding agent according to mass ratio 95:5, can be used as ultracapacitor positive pole.As shown in Figure 1, 2.
Embodiment 2
Taking specific area according to mass ratio 1:10 is 2200m
2/ g, the Graphene that aperture is 3~8nm and LiNi
1/3co
1/3mn
1/3o
2.Graphene is put in the ball grinder of ball mill, added a small amount of ethanol ball milling 3min, make Graphene complete wetting, add carbon nano-tube to stir 30min, then add a small amount of ethanol ball milling 2min, add LiNi
1/3co
1/3mn
1/3o
2continue to stir 1h, take out the material having mixed, dry, obtain combination electrode material, make pole piece with Kynoar according to mass ratio 90:10, can be used as lithium ion cell positive.
Embodiment 3
Taking specific area according to carbon and manganese mass ratio 1:3 is 2200m
2/ g, the Graphene that aperture is 3~8nm, adds the ultrasonic 1h of deionized water, obtains Graphene aqueous dispersions.Take potassium permanganate, join in Graphene aqueous dispersions, stir, obtain mixed solution.Take manganese sulfate and be dissolved in deionized water, then drop in mixed liquor.The solution obtaining is transferred to (filling rate 80%) in hydrothermal reaction kettle, be placed in incubation water heating reaction 3h at 120 ℃, baking oven, cool to room temperature, by gained sedimentation and filtration, washing, dry, can obtain MnO
2/ graphene composite material, makes pole piece with polytetrafluoroethylene according to mass ratio 90:10, can be used as ultracapacitor positive pole.
Embodiment 4
Taking specific area according to carbon and fluorine mass ratio 1:4 is 2200m
2/ g, aperture is that the Graphene of 3~8nm joins in the aqueous solution of sodium acetate, ferric nitrate, ammonium dihydrogen phosphate, sodium fluoride and stirs 30min, adds citric acid, pH is adjusted to 7 left and right with ammoniacal liquor, 80 ℃ of reaction 1h, the mixture obtaining is dry, is placed in reacting furnace, atmosphere of inert gases, 300 ℃ of reaction 2h, take out compressing tablet, then 700 ℃ of reaction 5h, obtain Na
2fePO
4f/ graphene composite material, makes pole piece with polytetrafluoroethylene according to mass ratio 90:10, can be used as sodium-ion battery electrode.
Embodiment 5
Taking specific area according to carbon and zinc mass ratio 1:4 is 2200m
2/ g, Graphene, manganese carbonate, citric acid, zinc carbonate that aperture is 3~8nm.Manganese carbonate and citric acid mix by magnetic agitation in deionized water, add the active carbon aqueous dispersions through ultrasonic dispersion, be warming up to 60 ℃, isothermal reaction 30min, adds zinc carbonate, continues to stir 2h, be cooled to room temperature, by the product sedimentation and filtration of gained, deionized water is cleaned, and 60 ℃ of vacuumizes are to constant weight; Atmosphere of inert gases, by 700 ℃ of calcining 2h of the product obtaining, obtains ZnMn
2o
4/ graphene composite material, makes pole piece with polytetrafluoroethylene according to mass ratio 90:10, can be used as the positive pole of Zinc ion battery.
Embodiment 6
Taking specific area according to mass ratio 1:10 is 2200m
2/ g, the Graphene that aperture is 3~8nm and LiMn
2o
4.Graphene is put in the ball grinder of ball mill, added a small amount of ethanol to stir 2min, make Graphene complete wetting, add LiMn
2o
4continue ball milling 1h, add Graphene LiMn
2o
4the carbon nano-tube ball milling 2h of gross mass 5%, takes out the material having mixed, dry, obtains LiMn
2o
4/ graphene combination electrode material, makes pole piece with Kynoar according to mass ratio 90:10, can be used as lithium ion cell positive.
Claims (10)
1. grapheme composite positive electrode material, is characterized in that: select and have loose structure Graphene, Graphene is dispersed phase in positive electrode particle, and the mass ratio of Graphene and positive electrode is 1:2~1:10; When wherein Graphene quality and positive electrode mass ratio are less than 1:6, add 2~10% the 3rd component of Graphene and positive electrode gross mass.
2. grapheme composite positive electrode material according to claim 1, is characterized in that described Graphene specific area is 1200~2300 m
2/ g.
3. grapheme composite positive electrode material according to claim 1, is characterized in that described positive electrode is LiMn
2o
4, LiFePO
4, Li
3v
2(PO4)
3, LiM
xmn
2-xo
4(M=Ni, Co, Fe, Cr, Cu), LiNi
xco
ymn
1-x-yo
2, (0 < x < 0.5,0 < y < 0.5), LiNi
1-xal
xo
2(0≤x≤0.6), LiCoO
2, Li
2mnSiO
4, Li
2feSiO
4, MnO
2, V
2o
5, NaVPO
4f, Na
2fePO
4f, NaNi
0.5mn
0.5o
2, Na
0.7mnO
2.05, ZnMn
xo
yone in (0 < x < 3, x:y=1.5~4.5).
4. grapheme composite positive electrode material according to claim 1, is characterized in that the 3rd described component is a kind of in carbon nano-tube, expanded graphite, acetylene black, carbon nano-fiber or their combination.
5. grapheme composite positive electrode material according to claim 1, is characterized in that described composite positive pole preparation method is physical mixed, a kind of during chemical original position is compound or their combination.
6. grapheme composite positive electrode material according to claim 5, it is characterized in that described physical mixed method be stir, a kind of in ultrasonic, ball milling or their combination, in mixed process, can be dry mixed, add solvent wet mixing or be dry mixed-wet mixing combination.
7. grapheme composite positive electrode material according to claim 6, the concrete steps that it is characterized in that described physical mixed method are as follows: take Graphene according to mass ratio and put in mixer, add solvent that Graphene is infiltrated completely, according to mass ratio, positive electrode or positive electrode and the 3rd component are added in mixer, after high-speed stirred is uniformly dispersed, dry, obtain combination electrode material.
8. the solvent described in is deionized water or ethanol.
9. grapheme composite positive electrode material according to claim 5, is characterized in that described chemical in-situ compounding process is that Graphene mixes with the raw material of synthetic positive electrode, forms combination electrode material in building-up process.
10. grapheme composite positive electrode material according to claim 1, is characterized in that described composite material can be used as the positive electrode of lithium ion battery, sodium-ion battery, Zinc ion battery, ultracapacitor.
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CN105449213A (en) * | 2015-12-29 | 2016-03-30 | 哈尔滨工业大学 | Porous graphene-coated modified lithium ion battery cathode material and preparation method thereof |
CN105575678A (en) * | 2015-12-17 | 2016-05-11 | 中国电子科技集团公司第十八研究所 | Preparation method of electrode membrane used for Li-ion capacitor |
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