CN112614979A - Secondary carbon-coated lithium iron phosphate and preparation method thereof - Google Patents

Secondary carbon-coated lithium iron phosphate and preparation method thereof Download PDF

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Publication number
CN112614979A
CN112614979A CN202011500071.XA CN202011500071A CN112614979A CN 112614979 A CN112614979 A CN 112614979A CN 202011500071 A CN202011500071 A CN 202011500071A CN 112614979 A CN112614979 A CN 112614979A
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iron phosphate
lithium iron
secondary carbon
coated lithium
coated
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韩建涛
卢宇
方淳
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Huazhong University of Science and Technology
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Huazhong University of Science and Technology
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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
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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

Abstract

The invention relates to a preparation method of secondary carbon-coated lithium iron phosphate, which comprises the following steps: grinding and uniformly mixing a polymer and lithium iron phosphate with carbon content less than 1% in absolute ethyl alcohol, wherein the polymer is polypyrrole, polyaniline or polyvinylpyrrolidone; pressing the obtained mixed powder into a sheet shape; and calcining the obtained sheet in protective gas, and carbonizing to obtain the secondary carbon-coated lithium iron phosphate sheet. A secondary carbon-coated lithium iron phosphate is prepared by the preparation method. The surface of the lithium iron phosphate is coated with a nitrogen-doped carbon coating, so that a good continuous electronic conducting layer is formed, and the rate capability and the cycle capability of the material are improved; in addition, compared with the traditional lithium iron phosphate, the modified lithium iron phosphate serving as the cathode material has high conductivity and compact arrangement of micro-morphology, so that the lithium ion battery has excellent charge and discharge performance under large current.

Description

Secondary carbon-coated lithium iron phosphate and preparation method thereof
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to secondary carbon-coated lithium iron phosphate and a preparation method thereof.
Background
As an advanced electrochemical energy storage and conversion system, the lithium ion battery has been widely applied to a power source for portable electronic devices, and is extended to the fields of Hybrid Electric Vehicles (HEVs), pure Electric Vehicles (EVs), renewable energy storage (solar energy, wind energy, etc.), smart grids, etc., but the preparation of the lithium ion battery with low price, high performance and high safety still has a challenge.
The positive electrode material of the lithium ion battery has important influence on the capacity, the cycle life, the safety and the price of the battery, and becomes a bottleneck for restricting the large-scale popularization and application of the lithium ion battery. Currently, inorganic cathode materials for commercial applications mainly include LiCoO2、LiMn2O4、LiFePO4LiNi, a ternary materialxCoyMnzO2(NCM) and LiNixCoyAl2O2(NCA) and the like.
LiFePO4As a next-generation lithium ion battery anode material with great development prospect, the lithium ion battery anode material has the excellent performances of good cycle stability, good safety, light weight, environmental protection and the like, but the lithium ion diffusion coefficient is low, the electronic conductivity is low, and the capacity attenuation is serious under high multiplying power in the charging and discharging processes of the battery. At present, the conductivity of the material is improved by adopting a proper nano technology in the industry, which inevitably reduces the compactibility of the material, and reduces the energy density of the battery because the particles are loosely combined.
Disclosure of Invention
The invention aims to solve the technical problem of providing secondary carbon-coated lithium iron phosphate and a preparation method thereof, so as to overcome the defects in the prior art.
The technical scheme for solving the technical problems is as follows: a preparation method of secondary carbon-coated lithium iron phosphate comprises the following steps:
s100, grinding and uniformly mixing a polymer and lithium iron phosphate with carbon content less than 1% in absolute ethyl alcohol, wherein the polymer is polypyrrole, polyaniline or polyvinylpyrrolidone;
s200, pressing the mixed powder obtained in the step S100 into a sheet shape;
s300, placing the sheet obtained in the step S200 in protective gas for calcining, and carbonizing to obtain a secondary carbon-coated lithium iron phosphate sheet;
and S400, grinding the secondary carbon-coated lithium iron phosphate sheets into powder to obtain the secondary carbon-coated lithium iron phosphate which is tightly arranged.
Further: the lithium iron phosphate with the carbon content less than 1% is No. 1 commercial lithium iron phosphate.
Further: the mass ratio of the lithium iron phosphate to the polymer is (8-10): 1.
Further: the mass ratio of the lithium iron phosphate to the polymer is 10: 1.
Further: the pressure for pressing the mixed powder is 10MPa to 20 MPa.
Further: the protective gas is Ar or N2。
Further: the calcining temperature is 600-700 ℃, and the calcining time is 5-7 h.
Further: the calcination time was 6 h.
A secondary carbon-coated lithium iron phosphate is prepared by the preparation method.
The invention has the beneficial effects that: the surface of the lithium iron phosphate is coated with a nitrogen-doped carbon coating, so that a good continuous electronic conducting layer is formed, and the rate capability and the cycle capability of the material are improved; in addition, compared with the traditional lithium iron phosphate, the modified lithium iron phosphate serving as the cathode material has high conductivity and compact arrangement of micro-morphology, so that the lithium ion battery has excellent charge and discharge performance under large current.
Drawings
Fig. 1 is a microscopic morphology of secondary carbon-coated lithium iron phosphate in example 1.
Fig. 2 is an xrd diffraction pattern of the secondary carbon-coated lithium iron phosphate in example 1.
Fig. 3 is a button cell charge-discharge performance diagram comparing the secondary carbon-coated lithium iron phosphate with the lithium iron phosphate in example 1.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth by way of illustration only and are not intended to limit the scope of the invention.
Example 1
A preparation method of secondary carbon-coated lithium iron phosphate comprises the following steps:
s100, taking No. 1 commercial lithium iron phosphate as a starting material, and mixing the starting material with polypyrrole according to a mass ratio of 10:1 grinding and uniformly mixing in absolute ethyl alcohol;
s200, taking 1g of the mixed powder obtained in the S100, putting the mixed powder into a die with the diameter of 20mm of a hydraulic press, and pressing the mixed powder into a sheet under the pressure of 10 MPa-20 MPa;
s300, placing the sheet obtained in the S200 in Ar or N2Calcining the mixture for 6 hours at the temperature of 600-700 ℃ in protective gas, and carbonizing the mixture to obtain a secondary carbon-coated lithium iron phosphate sheet;
and S400, grinding the secondary carbon-coated lithium iron phosphate sheets into powder to obtain the secondary carbon-coated lithium iron phosphate which is tightly arranged.
Example 2
A preparation method of secondary carbon-coated lithium iron phosphate comprises the following steps:
s100, taking No. 1 commercial lithium iron phosphate as a starting material, and mixing the starting material with polyaniline according to the mass ratio of 10:1 grinding and uniformly mixing in absolute ethyl alcohol;
s200, taking 1g of the mixed powder obtained in the S100, putting the mixed powder into a die with the diameter of 20mm of a hydraulic press, and pressing the mixed powder into a sheet under the pressure of 10 MPa-20 MPa;
s300, placing the sheet obtained in the S200 in Ar or N2Calcining the mixture for 6 hours at the temperature of 600-700 ℃ in protective gas, and carbonizing the mixture to obtain a secondary carbon-coated lithium iron phosphate sheet;
and S400, grinding the secondary carbon-coated lithium iron phosphate sheets into powder to obtain the secondary carbon-coated lithium iron phosphate which is tightly arranged.
Example 3
A preparation method of secondary carbon-coated lithium iron phosphate comprises the following steps:
s100, taking No. 1 commercial lithium iron phosphate as a starting material, and mixing the starting material with polyvinylpyrrolidone according to a mass ratio of 10:1 grinding and uniformly mixing in absolute ethyl alcohol;
s200, taking 1g of the mixed powder obtained in the S100, putting the mixed powder into a die with the diameter of 20mm of a hydraulic press, and pressing the mixed powder into a sheet under the pressure of 10 MPa-20 MPa;
s300, placing the sheet obtained in the S200 in Ar or N2Calcining the mixture for 6 hours at the temperature of 600-700 ℃ in protective gas, and carbonizing the mixture to obtain a secondary carbon-coated lithium iron phosphate sheet;
and S400, grinding the secondary carbon-coated lithium iron phosphate sheets into powder to obtain the secondary carbon-coated lithium iron phosphate which is tightly arranged.
Fig. 1 shows the microscopic morphology of lithium iron phosphate prepared by secondary carbon coating in example 1, which is in the form of uniformly distributed and closely arranged nanospheres of about 200 nm.
Fig. 2 is an xrd diffraction pattern of lithium iron phosphate prepared by secondary carbon coating in example 1, the characteristic peak intensity of which is consistent with that of lithium iron phosphate pdf card, no impurity peak, and good crystallinity, and which shows pnma type olivine structure.
Fig. 3 is a comparison graph of charge and discharge performances of a button battery in which commercial lithium iron phosphate (LFP) No. 1 and secondary carbon-coated lithium iron phosphate (C-LFP) are respectively used as positive electrode materials, lithium metal is used as a negative electrode, and a commercial lithium iron phosphate electrolyte is used as an electrolyte, at a rate of 0.2C to 20C, the modified positive electrode material at 20C has a specific discharge capacity of 60mAh/g to 70mAh/g, a capacity retention rate of 43%, a high-rate charge and discharge performance is good, and the capacity of an unmodified material is 0.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.

Claims (9)

1. A preparation method of secondary carbon-coated lithium iron phosphate is characterized by comprising the following steps:
s100, grinding and uniformly mixing a polymer and lithium iron phosphate with carbon content less than 1% in absolute ethyl alcohol, wherein the polymer is polypyrrole, polyaniline or polyvinylpyrrolidone;
s200, pressing the mixed powder obtained in the step S100 into a sheet shape;
and S300, calcining the sheet obtained in the step S200 in protective gas, and carbonizing to obtain the secondary carbon-coated lithium iron phosphate sheet.
2. The method for preparing secondary carbon-coated lithium iron phosphate according to claim 1, wherein the lithium iron phosphate containing less than 1% of carbon is commercial lithium iron phosphate No. 1.
3. The preparation method of the secondary carbon-coated lithium iron phosphate according to claim 1, wherein the mass ratio of the lithium iron phosphate to the polymer is (8-10): 1.
4. The preparation method of the secondary carbon-coated lithium iron phosphate according to claim 3, wherein the mass ratio of the lithium iron phosphate to the polymer is 10: 1.
5. The method for preparing secondary carbon-coated lithium iron phosphate according to claim 1, wherein the pressure for pressing the mixed powder is 10 to 20 MPa.
6. The method for preparing secondary carbon-coated lithium iron phosphate according to any one of claims 1 to 5, wherein the protective gas is Ar or N2。
7. The method for preparing secondary carbon-coated lithium iron phosphate according to any one of claims 1 to 6, wherein the calcination temperature is 600 ℃ to 700 ℃ and the calcination time is 5h to 7 h.
8. The method for preparing secondary carbon-coated lithium iron phosphate according to any one of claims 1 to 7, wherein the calcination time is 6 hours.
9. A secondary carbon-coated lithium iron phosphate prepared by the preparation method of any one of claims 1 to 8.
CN202011500071.XA 2020-12-17 2020-12-17 Secondary carbon-coated lithium iron phosphate and preparation method thereof Pending CN112614979A (en)

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Cited By (2)

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CN114132970A (en) * 2021-11-25 2022-03-04 蜂巢能源科技有限公司 Method for improving cycle stability of positive electrode material, positive electrode material and lithium ion battery
US11881582B2 (en) 2021-12-29 2024-01-23 Contemporary Amperex Technology Co., Limited Positive electrode active material and preparation method thereof, secondary battery, and electric apparatus

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114132970A (en) * 2021-11-25 2022-03-04 蜂巢能源科技有限公司 Method for improving cycle stability of positive electrode material, positive electrode material and lithium ion battery
CN114132970B (en) * 2021-11-25 2023-12-29 蜂巢能源科技有限公司 Method for improving circulation stability of positive electrode material, positive electrode material and lithium ion battery
US11881582B2 (en) 2021-12-29 2024-01-23 Contemporary Amperex Technology Co., Limited Positive electrode active material and preparation method thereof, secondary battery, and electric apparatus

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