CN110518297A - Lithium ion cell positive mends lithium material Li5FeO4Preparation method and application - Google Patents
Lithium ion cell positive mends lithium material Li5FeO4Preparation method and application Download PDFInfo
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- CN110518297A CN110518297A CN201810491882.4A CN201810491882A CN110518297A CN 110518297 A CN110518297 A CN 110518297A CN 201810491882 A CN201810491882 A CN 201810491882A CN 110518297 A CN110518297 A CN 110518297A
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- lithium
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- lithium ion
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/0018—Mixed oxides or hydroxides
- C01G49/0027—Mixed oxides or hydroxides containing one alkali metal
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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
-
- 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
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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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
A kind of lithium ion cell positive benefit lithium material Li5FeO4Preparation method and application belongs to field of lithium ion battery.Lithium source material of the present invention and ferrous source material are uniformly mixed according to the ratio that lithium atom and iron atom molar ratio are 4-10:1, after being ground uniformly after Cold pretreatment 0.5-20h at a temperature of 150-500 DEG C, 500-1000 DEG C of high temperature is risen to 0.5-20 DEG C/min heating rate again, it is sintered 10-40h at these elevated temperatures, cooled to room temperature obtains Li5FeO4Anode mends lithium material;In positive pulping process, anode is mended into lithium material Li5FeO4Be uniformly mixed with positive main material, conductive agent, binder and solvent, it is coated, roll, assemble, lithium ion battery is made in fluid injection, chemical conversion, partial volume process.After lithium ion battery is by mending lithium, its first charge discharge efficiency and battery capacity can be improved, improve cycle performance, increase battery energy density, this method simple process and low cost is no dangerous, easy to industrialized production.
Description
Technical field
The present invention relates to technical field of lithium ion, specifically a kind of lithium ion cell positive mends lithium material Li5FeO4
Preparation method and application.
Background technique
Lithium ion battery is due to becoming application range most with advantages such as high voltage, high-energy density and long circulation lifes
One of wide secondary cell.But with portable electronic device micromation, standby for a long time continuous development and electrical salf-walking
Vehicle, electric car etc. be high-power, high-energy device enabling, all mentions to the energy density of the lithium ion battery as accumulation power supply
Increasingly higher demands are gone out.
During the initial charge of battery, due to solid electrolyte interface film (SEI film) meeting of negative electrode tab surface formation
Consumption part migrates the Li to come from positive plate+, thereby result in Li in positive electrode+Loss, lead to the drop of battery first charge discharge efficiency
It is low, to reduce the capacity of battery.Especially when the active material in negative electrode tab is alloy material (such as silicon alloy and tin alloy
Deng) when show particularly evident, so, in order to improve the first charge discharge efficiency of battery, the application for mending lithium technology seems especially urgent.
Presently the most common benefit lithium technology is divided into cathode and mends lithium and anode benefit lithium, and wherein cathode is mended lithium technology and mainly used
The techniques such as lithium powder and lithium foil supplement cathode irreversible capacity loss during initial charge, and this method process conditions are harsh, throw
Money is big, and the use of lithium metal causes biggish security risk.Such as Publication No. CN1290209C patent application mention by
Lithium metal, negative electrode material and on-aqueous liquid are mixed to form slurry, and slurry is coated on collector, then dry slurries, roll-in
After electrolyte is perfused, diffuse into lithium powder inside active material.Although this method can be improved first charge discharge efficiency, but due to metal
Lithium reactivity is higher, and whole operation needs carry out in anhydrous dry environment, and want strict temperature control, and process is multiple
It is miscellaneous.Further, since lithium powder is lighter, it is easy to float in the slurry, causes addition difficult.Publication No. CN102916164A's is special
Benefit can achieve the purpose that mend lithium and improve first effect, but the solvent of organolithium is hexane solution, the n-hexane of tert-butyl lithium is molten
Liquid and phenyl lithium, solution is toxic, and needs to operate in inert protective gas, increases cost and operation difficulty.Publication number
The patent of invention of CN105206779A discloses a kind of ceramic diaphragm, on the basis of existing basement membrane, coat one layer of Li2MnO3,
Li2MnO3-LiNiCoMnO2, Li5FeO4, Li5Fe5O8 etc. can deintercalate lithium ions compound, although this method is in charge and discharge
It can play the role of mending lithium in the process, but will definitely increase during diaphragm coating compound equipment, technique, material
Cost can also change the performances such as the tensile strength, gas permeability and porosity of diaphragm after diaphragm coating.
Summary of the invention
In order to overcome the deficiencies of the prior art, goal of the invention of the invention is to provide a kind of lithium ion cell positive benefit lithium material
Expect Li5FeO4Preparation method and application, to solve the problems, such as that battery first charge discharge efficiency is low in charge and discharge process.
For achieving the above object, the present invention is using lithium-containing materials as lithium source, and iron-bearing materials are source of iron, according to lithium-containing materials
It is 4-10:1 with the lithium atom of iron-bearing materials and the molar ratio of iron atom, after mixing by two kinds of materials, at 150-500 DEG C
At a temperature of Cold pretreatment 0.5-20h, then after grinding uniformly, then high temperature, In risen to the heating rate of 0.5-20 DEG C/min
10-40h is sintered at a high temperature of 500-1000 DEG C, last cooled to room temperature obtains Li5FeO4Anode mends lithium material.
The lithium source material is one or more of lithium hydroxide, lithium carbonate, lithium acetate mixture.
The ferrous source material is the mixture of one or more of ferric nitrate, ferric sulfate, iron chloride, di-iron trioxide.
Preferably, the above-mentioned heating rate for rising to high temperature is 1-10 DEG C/min, and high temperature sintering temperature is 600-800 DEG C, is burnt
The knot time is 12-30h.
Lithium ion cell positive of the invention mends lithium material Li5FeO4Application, it is characterised in that: in positive pulping process
In, anode is mended into lithium material Li5FeO4It is uniformly mixed with positive main material, conductive agent, binder and solvent, then by coating, stone roller
Lithium ion battery is made in pressure, assembly, fluid injection, chemical conversion, partial volume process;The anode mends lithium material Li5FeO4During the charging process,
Li+ element is deviate from from high capacity positive electrode, is embedded into the irreversible capacity that first charge-discharge is supplemented in cathode.
Anode is added and mends lithium material Li5FeO4Amount account for positive main material ratio be 0.1-20%;Preferably, anode mends lithium material
Expect Li5FeO4Amount account for positive main material ratio be 0.5-3%.
The anode main material is cobalt acid lithium, LiMn2O4, LiFePO 4, nickle cobalt lithium manganate, one kind of nickel cobalt aluminic acid or two
Kind mixture.
The conductive agent is one of SUPER-P, KS-6, KS-15, VGCF, SFG6, ECP, carbon nanotube, graphene
Or several mixtures.
The binder is one or more of PVDF, PTFE, LA132, LA133, CMC and SBR mixture.
The solvent is one or both of NMP or water mixture.
Compared with prior art, the present invention the first charge discharge efficiency of battery can be effectively improved, simple process and low cost is easy to work
Industry metaplasia produces, and prepared material granule is uniform, easy to operate without changing prior art;Without inert atmosphere protection, to ring
Border is transformed without particular/special requirement without to existing production technology and equipment, only need to be in existing production environment, equipment and technique
Under the conditions of, lithium material will be mended in positive pulping process and will be uniformly mixed with materials such as main material, binder and conductive agents, be not required to
Increase additional equipment cost;The invention belongs to " wet process benefit lithiums ", avoid dust pollution and safety problem that dry method mends lithium.
After lithium ion battery is by mending lithium, its first charge discharge efficiency and battery capacity can be improved, to increase the energy density of battery.
Detailed description of the invention
Fig. 1 is that present invention anode mends lithium material Li5FeO4X-ray diffractometer (XRD) structure chart.
Fig. 2 is that present invention anode mends lithium material Li5FeO4Scanning electron microscope (SEM) figure.
Fig. 3 is that present invention anode mends lithium material Li5FeO4Charging and discharging curve figure.
Specific embodiment
Lithium ion cell positive of the present invention mends lithium material Li5FeO4Preparation method:
Embodiment one: after mixing with Li/Fe atomic molar ratio 5:1 by lithium carbonate and ferric nitrate, locate in advance at a temperature of 450 DEG C
8h is managed, then grinding is uniform, then is warming up to 750 DEG C with the speed of 5 DEG C/min, is sintered 18h, last natural cooling at this temperature
To room temperature, Li is obtained5FeO4Anode mends lithium material.
Embodiment two: after mixing with Li/Fe atomic molar ratio 6:1 by lithium hydroxide and ferric nitrate, in 470 DEG C of temperature
Lower pretreatment 10h, then grinding is uniform, then is warming up to 750 DEG C with the speed of 5 DEG C/min, is sintered 16h at this temperature, finally
Cooled to room temperature obtains Li5FeO4Anode mends lithium material.
Embodiment three: after mixing with Li/Fe atomic molar ratio 5.5:1 by lithium hydroxide and ferric sulfate, in 450 DEG C of temperature
Degree is lower to pre-process 8h, and then grinding is uniform, then is warming up to 800 DEG C with the speed of 8 DEG C/min, is sintered 20h at this temperature, finally
Cooled to room temperature obtains Li5FeO4Anode mends lithium material.
Example IV: after mixing with Li/Fe atomic molar ratio 6:1 by lithium acetate and di-iron trioxide, in 500 DEG C of temperature
Degree is lower to pre-process 7h, and then grinding is uniform, then is warming up to 780 DEG C with the speed of 5 DEG C/min, is sintered at this temperature for 24 hours, finally
Cooled to room temperature obtains Li5FeO4Anode mends lithium material.
Embodiment five: after mixing with Li/Fe atomic molar ratio 8:1 by lithium acetate and di-iron trioxide, in 400 DEG C of temperature
Degree is lower to pre-process 7h, and then grinding is uniform, then is warming up to 850 DEG C with the speed of 10 DEG C/min, is sintered 22h at this temperature, most
Cooled to room temperature afterwards obtains Li5FeO4Anode mends lithium material.
Lithium ion cell positive of the present invention mends lithium material Li5FeO4Application:
Embodiment one: in positive pulping process, by Li5FeO4Mend lithium material and cobalt acid lithium main material, SUPER-P conductive agent,
The materials such as PVDF binder and nmp solvent are uniformly mixed, wherein Li5FeO4Amount be cobalt acid lithium weight 2%, then through painting
Cloth, roll, assemble, lithium ion battery is made in fluid injection, chemical conversion, the processes such as partial volume.
Embodiment two: in positive pulping process, by Li5FeO4Mend lithium material and LiMn2O4, SUPER-P conductive agent, PVDF
Binder and nmp solvent are uniformly mixed, wherein Li5FeO4Amount be the 1% of LiMn2O4 weight, then by being coated with, roll, filling
Match, lithium ion battery is made in fluid injection, chemical conversion, the processes such as partial volume.
Embodiment three: in positive pulping process, by Li5FeO4Mend lithium material and nickle cobalt lithium manganate, SUPER-P and KS-6
Conductive agent, PVDF binder and nmp solvent are uniformly mixed, wherein Li5FeO4Amount be nickle cobalt lithium manganate weight 3%, then pass through
Cross be coated with, roll, assembling, lithium ion battery is made in fluid injection, chemical conversion, the processes such as partial volume.
Example IV: in positive pulping process, by Li5FeO4Mend lithium material and LiFePO4, SUPER-P, KS-6 and stone
Black alkene conductive agent, PVDF binder and nmp solvent are uniformly mixed, wherein Li5FeO4Amount be LiFePO 4 pressure, assembly, note
Lithium ion battery is made in the processes such as liquid, chemical conversion, partial volume.
Embodiment five: in positive pulping process, by Li5FeO4Mend lithium material and nickle cobalt lithium manganate, SUPER-P, carbon nanometer
The materials such as pipe conductive agent, PVDF binder and nmp solvent are uniformly mixed, wherein Li5FeO4Amount be nickle cobalt lithium manganate weight
1.5%, then by being coated with, rolling, assembling, fluid injection, chemical conversion, the processes such as partial volume lithium ion battery is made.
The lithium ion battery of different systems performance comparison such as table 1 before and after mending lithium:
It should be noted that negative electrode material of the invention is the mixing of graphite, silicon-carbon, silicon oxygen and silicon-carbon and silicon oxygen and graphite
Object and other tin alloys etc..
Claims (10)
1. a kind of lithium ion cell positive mends lithium material Li5FeO4Preparation method, it is characterised in that: this method is with lithium-containing materials
Lithium source, iron-bearing materials are source of iron, the ratio for being 4-10:1 according to the molar ratio of lithium atom and iron atom, two kinds of materials are mixed equal
After even, in 150-500 DEG C of at a temperature of Cold pretreatment 0.5-20h, then grinding is uniform, then with the heating of 0.5-20 DEG C/min
Speed rises to 500-1000 DEG C of high temperature, is sintered 10-40h at these elevated temperatures, and last cooled to room temperature obtains Li5FeO4Just
Mend lithium material in pole.
2. lithium ion cell positive according to claim 1 mends lithium material Li5FeO4Preparation method, it is characterised in that: described
Lithium source material is one or more of lithium hydroxide, lithium carbonate, lithium acetate mixture.
3. lithium ion cell positive according to claim 1 mends lithium material Li5FeO4Preparation method, it is characterised in that: described
Ferrous source material is one or more of ferric nitrate, ferric sulfate, iron chloride, di-iron trioxide mixture.
4. lithium ion cell positive according to claim 1 mends lithium material Li5FeO4Preparation method, it is characterised in that: described
Heating rate is 1-10 DEG C/min, and high temperature sintering temperature is 600-800 DEG C, sintering time 12-30h.
5. a kind of lithium ion cell positive of claim 1 mends lithium material Li5FeO4Application, it is characterised in that: in positive slurrying
In the process, anode is mended into lithium material Li5FeO4It is uniformly mixed with positive main material, conductive agent, binder and solvent, then by applying
Cloth, roll, assemble, lithium ion battery is made in fluid injection, chemical conversion, partial volume process;The anode mends lithium material Li5FeO4It was charging
Cheng Zhong, Li+Element is deviate from from high capacity positive electrode, is embedded into the irreversible capacity that first charge-discharge is supplemented in cathode.
6. lithium ion cell positive according to claim 5 mends lithium material Li5FeO4Application, it is characterised in that: be added just
Mend lithium material Li in pole5FeO4Amount account for positive main material ratio be 0.1-20%;Preferably, anode mends lithium material Li5FeO4Amount
The ratio for accounting for positive main material is 0.5-5%.
7. the application that lithium ion cell positive according to claim 5 mends lithium material Li5FeO4, it is characterised in that: described
Positive main material is one or both of cobalt acid lithium, LiFePO 4, LiMn2O4, nickle cobalt lithium manganate, nickel cobalt aluminic acid mixture.
8. the application that lithium ion cell positive according to claim 5 mends lithium material Li5FeO4, it is characterised in that: described
Conductive agent is one or more of SUPER-P, KS-6, KS-15, VGCF, SFG6, ECP, carbon nanotube, graphene mixture.
9. the application that lithium ion cell positive according to claim 5 mends lithium material Li5FeO4, it is characterised in that: described
Binder is one or more of PVDF, PTFE, LA132, LA133, CMC and SBR mixture.
10. the application that lithium ion cell positive according to claim 5 mends lithium material Li5FeO4, it is characterised in that: described
Solvent is one or both of NMP or water mixture.
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