CN108565428A - Improve lithium ion battery LiFePO4The method of composite positive pole performance - Google Patents

Improve lithium ion battery LiFePO4The method of composite positive pole performance Download PDF

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Publication number
CN108565428A
CN108565428A CN201810352549.5A CN201810352549A CN108565428A CN 108565428 A CN108565428 A CN 108565428A CN 201810352549 A CN201810352549 A CN 201810352549A CN 108565428 A CN108565428 A CN 108565428A
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lifepo
lithium ion
positive pole
ion battery
composite positive
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刘伟
李丽
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1002 Information Technology (cangzhou) Co Ltd
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1002 Information Technology (cangzhou) Co Ltd
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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
    • 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
    • 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
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • 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
    • 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
    • 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

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Composite Materials (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The present invention provides a kind of raising lithium ion battery LiFePO4The method of composite positive pole performance, includes the following steps：(1) in LiFePO4Middle dispersion or coated with conductive carbon；(2) in dispersion or the LiFePO of coated with conductive carbon4It is middle that a small amount of conductive metal ion is added；(3) hereafter, in LiFePO4A small amount of high valent cationic is adulterated in lattice, to increase the intrinsic conductivity of material；(4) by the LiFePO4It is modified as the LiFePO of Nano grade4Particle.Using this method, the electric conductivity of material grains is effectively increased, and increases the intrinsic conductivity of material, and chemical property is also improved.

Description

Improve lithium ion battery LiFePO4The method of composite positive pole performance
Technical field
The present invention relates to lithium ion battery technologies, especially improve lithium ion battery LiFePO4Composite positive pole performance Technology.
Background technology
LiFePO4With higher energy density and theoretical capacity, discharge voltage is stablized, and good cycle is before applying The good anode material for lithium-ion batteries of scape, but on the other hand, due to LiFePO4Specific structure determined some lack Point seriously restricts its application and development.
Pure LiFePO4Electronic conductivity and ionic diffusion coefficient are relatively low, are only suitable for carrying out under low current density Charge and discharge, in LiFePO4Structure in, due to not continuous FePO6Side octahedral volume grid altogether, therefore cause the low electricity of material Electron conductivity；The oxygen atom in crystal is arranged by close to the closelypacked mode of six sides simultaneously, is only lithium ion and is provided with The channel of limit so that the apology rate very little of lithium ion wherein at room temperature, at room temperature LiCoO2And LiMn2O4Conductivity point It Wei 10-3With 10-4S/cm, and pure LiFePO4Conductivity be only 10-10S/cm, lithium ion is in LiCoO2In diffusion coefficient be 10-8cm2/ s, and in LiFePO4And FePO4Middle diffusion coefficient is respectively 10-14cm2/ s and 10-16cm2/s。
LiFePO4Tap density it is relatively low, this point and LiCoO2And LiCoO2、LiNiO2And LiMn2O4Have larger Gap has seriously affected the volume and capacity ratio of material.
How LiFePO is improved4Electric conductivity and improve lithium ion between material body and solid liquid interface migration speed Degree be the key that such material can practical application, therefore, the emphasis and hot spot collection of current such materials synthesis and study on the modification In in the electron conduction and the aspect of ion diffusion rates two for improving material.
Invention content
The purpose of the present invention is to provide a kind of raising lithium ion battery LiFePO4The method of composite positive pole performance, Include the following steps：(1) in LiFePO4Middle dispersion or coated with conductive carbon；(2) in dispersion or the LiFePO of coated with conductive carbon4In plus Enter the metal ion of a small amount of conduction；(3) hereafter, in LiFePO4A small amount of high valent cationic is adulterated in lattice, to increase material The intrinsic conductivity of material.
Preferably, the carbon source of conductive carbon described in step (1) is carbon black, sucrose, organic additive and carbon gel.
Preferably, the feed postition of conductive carbon described in step (1) includes two kinds, is to prepare LiFePO respectively4In plus Enter, and the LiFePO that gained will be reacted4After powder is mixed with carbon source, high-temperature heat treatment introduces.
Preferably, dispersion or coated with conductive carbon use solid phase reaction method in step (1), after raw material predecomposition, 80 Degree Celsius, the carbon black of high-specific surface area is added in the case of 1C discharge capacities, so that particle size is less than 10 microns, electronics is led Electric rate is increased to 1.7*10-3S/cm。
Preferably, the carbon that dispersion or cladding mass fraction are 1% in step (1).
Preferably, step (2) synthesizes LiFePO using sol-gel method4, add Ag and Cu that mass fraction is 1%.
Preferably, the metal ion of the step (3) includes Nb5+、Al3+、Ti4+、W6+、Zr4+In one kind or one Kind or more.
Preferably, further include step：(4) by the LiFePO4It is modified as the LiFePO of Nano grade4Particle.
Preferably, the step (4) uses two methods：First method is to synthesize unformed FePO first4Preceding body Body, then using LiI be reducing agent to FePO4The embedding lithium of chemistry is carried out, finally roasting generation average grain diameter only has under 550 degrees Celsius The LiFePO of 100nm4Crystal grain, product have good chemical property, and discharge capacity reaches for the first time under the conditions of 1C 155mAh/g, capacity is gradually reduced after cycle-index increase, is stablized in 110mAh/g or more always after 200 cycles, 700 are followed Capacity is not decayed after ring；Second method is by FeSO4·7H2O and H3PO4Mixing is slowly added to the pH that LiOH adjusts solution After magnetic stirrer, 3h is heated under the reducing atmosphere of 500 ° of c close to neutrality for value.
Using this method, the electric conductivity of material grains is effectively increased, and increases the intrinsic conductivity of material, and And chemical property is also improved.
According to the following detailed description of specific embodiments of the present invention in conjunction with the accompanying drawings, those skilled in the art will be brighter The above and other objects, advantages and features of the present invention.
Description of the drawings
Some specific embodiments that the invention will be described in detail by way of example and not limitation with reference to the accompanying drawings hereinafter. Identical reference numeral denotes same or similar component or part in attached drawing.It should be appreciated by those skilled in the art that these What attached drawing was not necessarily drawn to scale.The target and feature of the present invention will be apparent from view of following description taken together with the accompanying drawings, In attached drawing：
Fig. 1 is the method stream according to the raising lithium ion battery LiFePO4 composite positive pole performances of the embodiment of the present invention Cheng Tu.
Specific implementation mode
Referring to attached drawing 1, a kind of raising lithium ion battery LiFePO4The method of composite positive pole performance, including walk as follows Suddenly：(1) in LiFePO4On the one hand middle dispersion or coated with conductive carbon can enhance the electric conductivity between particle and particle, subtract in this way The polarization of few battery, on the other hand can also be LiFePO4Electron tunnel is provided, with compensate lithium ion it is embedding it is de- during charge it is flat Weighing apparatus, carbon source are carbon black, sucrose, organic additive and carbon gel etc., and the mode that carbon is added includes two kinds, and one is preparing LiFePO4Middle addition, another is the LiFePO that will react gained4After powder is mixed with carbon source, high-temperature heat treatment introduces. Dispersion or coated with conductive carbon use solid phase reaction method, after raw material predecomposition, add in the case of 80 degrees Celsius, 1C discharge capacities Enter the carbon black of high-specific surface area, so that particle size is less than 10 microns, electronic conductivity is increased to 1.7*10-3S/cm. In the carbon black to raw material for adding carbon gel or surface oxidation before reactant predecomposition, the LiFePO of preparation4Crystal grain diameter exists 100-200nm, point capacity also has 120mAh/g below 5C multiplying powers, this is because the material that little crystal grain high surface area carbon coating is good The intrinsic defect of material can be overcome, but surface area increases, cladding needs more with carbon, and the density of carbon is 2.2g/cm3, only There is LiFePO461%, the carbon of addition will significantly reduce the energy density and tap density of material, therefore also need to vacation wherein Such as a small amount of conductive metal ion；(2) in dispersion or the LiFePO of coated with conductive carbon4It is middle that a small amount of conductive metal ion is added, LiFePO is synthesized using sol-gel method4, Ag and Cu that mass fraction is 1% are added, specific capacity improves 25mAh/g, room temperature Discharge capacity is 140mAh/g to lower 0.2C multiplying powers for the first time, still has 130mAh/g after 30 cycles, is dispersed in LiFePO4In metal Ultra micro fission does not interfere with LiFePO4Microstructure, help so that crystallite size becomes smaller, and substantially reduce intercrystalline Impedance；(3) hereafter, in LiFePO4A small amount of high valent cationic is adulterated in lattice, is disperseed using conductive materials such as carbon and metals Or the method for cladding, the electrical contact between active material particle is mainly improved, the conductivity of composite material is increased, and for material The intrinsic conductivity of material does not influence substantially, therefore the intrinsic conductivity for improving the i.e. increase material of particle internal conductance rate is still The low critical issue of material electric conductivity is solved, includes Nb on a small quantity by adulterating5+、Al3+、Ti4+、W6+、Zr4+In one kind or one kind Conductivity can be increased to 10 by above high volence metal ion-2S/cm, about pure LiFePO4108Times, higher than traditional LiCoO2Conductivity, material capacity under the conditions of low range still have 85mAh/g's close to theoretical capacity under 10C multiplying powers Capacity simultaneously maintains good cycle performance, due to LiFePO4It is a kind of semiconductor, the band gap between conduction band and valence band is offside 300meV, in the charge and discharge process of material, Fe3+/Fe2+It changes than regular meeting, so that LiFePO4Crystal is in p-type and N It changes between type, individual Fe3+And Fe2+Electric conductivity is all poor, but since there are the defect of lithium position, shapes after doping At there are Fe3+And Fe2+The deficient compound of mixed valence reduces the band gap between conduction band and valence band, is effectively increased LiFePO4Conductivity.
By the LiFePO of doping vario-property4Although conductivity is more than LiCoO2, but its chemical property is but not as good as the latter, Main cause is that Li insertion extraction process, which is mainly spread by lithium particle, to be controlled, due to currently existing to lithium particle in the charge and discharge later stage LiFePO4In diffusion mechanism research it is not deep enough so that from internal structure improve lithium particle diffusion rate there are some Difficulty, therefore there is also a steps for this method, i.e., by the LiFePO4It is fabricated to the LiFePO of Nano grade4Particle, mainly By two methods, one is synthesize unformed FePO first4Precursor, then using LiI be reducing agent to FePO4Carry out chemistry Embedding lithium, finally roasting generates the LiFePO that average grain diameter only has 100nm under 550 degrees Celsius4Crystal grain, product have good Chemical property, discharge capacity reaches 155mAh/g for the first time under the conditions of 1C, and capacity is gradually reduced after cycle-index increase, 200 Stablize the capacity after 110mAh/g or more, 700 cycles after a cycle always not decay；Second method is by FeSO4· 7H2O and H3PO4Mixing is slowly added to the close neutrality of pH value that LiOH adjusts solution, after magnetic stirrer, in 500 ° of c Reducing atmosphere under heat 3h.
Using this method, the electric conductivity of material grains is effectively increased, and increases the intrinsic conductivity of material, and And chemical property is also improved.
It, will not be by these embodiments although the present invention is described by reference to specific illustrative embodiment Restriction and only limited by accessory claim.It should be understood by those skilled in the art that can be without departing from the present invention's The embodiment of the present invention can be modified and be changed in the case of protection domain and spirit.

Claims (9)

1. a kind of raising lithium ion battery LiFePO4The method of composite positive pole performance, it is characterised in that include the following steps： (1) in LiFePO4Middle dispersion or coated with conductive carbon；(2) in dispersion or the LiFePO of coated with conductive carbon4The middle a small amount of conduction of addition Metal ion；(3) hereafter, in LiFePO4A small amount of high valent cationic is adulterated in lattice, to increase the intrinsic conductance of material Rate.
2. a kind of raising lithium ion battery LiFePO according to claim 14The method of composite positive pole performance, it is special Sign is that the carbon source of conductive carbon described in step (1) is carbon black, sucrose, organic additive and carbon gel.
3. a kind of raising lithium ion battery LiFePO according to claim 14The method of composite positive pole performance, it is special Sign is that the feed postition of conductive carbon described in step (1) includes two kinds, is to prepare LiFePO respectively4Middle addition, and will React the LiFePO of gained4After powder is mixed with carbon source, high-temperature heat treatment introduces.
4. a kind of raising lithium ion battery LiFePO according to claim 14The method of composite positive pole performance, it is special Sign is in step (1) that dispersion or coated with conductive carbon use solid phase reaction method, after raw material predecomposition, at 80 degrees Celsius, and 1C The carbon black of high-specific surface area is added in the case of discharge capacity, so that particle size is less than 10 microns, electronic conductivity improves To 1.7*10-3S/cm。
5. a kind of raising lithium ion battery LiFePO according to claim 14The method of composite positive pole performance, it is special Sign is the carbon that dispersion or cladding mass fraction are 1% in step (1).
6. a kind of raising lithium ion battery LiFePO according to claim 14The method of composite positive pole performance, it is special Sign is that step (2) synthesizes LiFePO using sol-gel method4, add Ag and Cu that mass fraction is 1%.
7. a kind of raising lithium ion battery LiFePO according to claim 14The method of composite positive pole performance, it is special Sign is that the metal ion of the step (3) includes Nb5+、Al3+、Ti4+、W6+、Zr4+In one or more.
8. according to a kind of any raising lithium ion battery LiFePO of claim 1-74The side of composite positive pole performance Method, it is characterised in that further include step：
(4) by the LiFePO4It is modified as the LiFePO of Nano grade4Particle.
9. a kind of raising lithium ion battery LiFePO according to claim 84The method of composite positive pole performance, it is special Sign is that the step (4) uses two methods：First method is to synthesize unformed FePO first4Precursor, then with LiI It is reducing agent to FePO4The embedding lithium of chemistry is carried out, finally roasting generation average grain diameter only has 100nm's under 550 degrees Celsius LiFePO4Crystal grain, product have good chemical property, and discharge capacity reaches 155mAh/g for the first time under the conditions of 1C, follows Capacity is gradually reduced after ring number increase, stablizes the capacity after 110mAh/g or more, 700 cycles after 200 cycles always and does not have There is decaying；Second method is by FeSO4·7H2O and H3PO4Mixing is slowly added to LiOH and adjusts the pH value of solution in Property, after magnetic stirrer, 3h is heated under 500 DEG C of reducing atmosphere.
CN201810352549.5A 2018-04-19 2018-04-19 Improve lithium ion battery LiFePO4The method of composite positive pole performance Pending CN108565428A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101635349A (en) * 2009-08-21 2010-01-27 广州市云通磁电有限公司 Method for preparing metal-silver-doped carbon-covering lithium iron phosphate of lithium-ion battery cathode material
CN101888973A (en) * 2007-12-06 2010-11-17 南方化学股份公司 Nanoparticulate composition and method for the production thereof
CN102044667A (en) * 2010-11-26 2011-05-04 兰州金川新材料科技股份有限公司 Method for preparing spherical LFP (lithium iron phosphate)/carbon doped composite powder
CN102275890A (en) * 2011-07-19 2011-12-14 彩虹集团公司 Microwave-assisted synthesis method of nanometer lithium iron phosphate
CN102751493A (en) * 2012-06-27 2012-10-24 武陟县鑫凯科技材料有限公司 Preparation method of lithium iron phosphate
CN103762361A (en) * 2014-01-20 2014-04-30 中南大学 Low-energy preparation method of lithium iron phosphate

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101888973A (en) * 2007-12-06 2010-11-17 南方化学股份公司 Nanoparticulate composition and method for the production thereof
CN101635349A (en) * 2009-08-21 2010-01-27 广州市云通磁电有限公司 Method for preparing metal-silver-doped carbon-covering lithium iron phosphate of lithium-ion battery cathode material
CN102044667A (en) * 2010-11-26 2011-05-04 兰州金川新材料科技股份有限公司 Method for preparing spherical LFP (lithium iron phosphate)/carbon doped composite powder
CN102275890A (en) * 2011-07-19 2011-12-14 彩虹集团公司 Microwave-assisted synthesis method of nanometer lithium iron phosphate
CN102751493A (en) * 2012-06-27 2012-10-24 武陟县鑫凯科技材料有限公司 Preparation method of lithium iron phosphate
CN103762361A (en) * 2014-01-20 2014-04-30 中南大学 Low-energy preparation method of lithium iron phosphate

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