CN112599730A - Preparation method of carbon-coated lithium iron phosphate cathode material - Google Patents
Preparation method of carbon-coated lithium iron phosphate cathode material Download PDFInfo
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- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 title claims abstract description 57
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 36
- 239000010406 cathode material Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 30
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 30
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000001354 calcination Methods 0.000 claims abstract description 28
- 238000000498 ball milling Methods 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 21
- 239000006185 dispersion Substances 0.000 claims abstract description 19
- 239000002243 precursor Substances 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 229910052786 argon Inorganic materials 0.000 claims abstract description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 15
- 239000002002 slurry Substances 0.000 claims abstract description 14
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 13
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052742 iron Inorganic materials 0.000 claims abstract description 12
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 12
- 239000011574 phosphorus Substances 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 10
- 239000003960 organic solvent Substances 0.000 claims abstract description 10
- 239000007774 positive electrode material Substances 0.000 claims abstract description 8
- 239000011265 semifinished product Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 6
- 229930006000 Sucrose Natural products 0.000 claims description 6
- 239000008103 glucose Substances 0.000 claims description 6
- SNKMVYBWZDHJHE-UHFFFAOYSA-M lithium;dihydrogen phosphate Chemical compound [Li+].OP(O)([O-])=O SNKMVYBWZDHJHE-UHFFFAOYSA-M 0.000 claims description 6
- 239000005720 sucrose Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 4
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 4
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 4
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 4
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- YNQRWVCLAIUHHI-UHFFFAOYSA-L dilithium;oxalate Chemical compound [Li+].[Li+].[O-]C(=O)C([O-])=O YNQRWVCLAIUHHI-UHFFFAOYSA-L 0.000 claims description 3
- PQVSTLUFSYVLTO-UHFFFAOYSA-N ethyl n-ethoxycarbonylcarbamate Chemical compound CCOC(=O)NC(=O)OCC PQVSTLUFSYVLTO-UHFFFAOYSA-N 0.000 claims description 3
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 3
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 3
- GLXDVVHUTZTUQK-UHFFFAOYSA-M lithium hydroxide monohydrate Substances [Li+].O.[OH-] GLXDVVHUTZTUQK-UHFFFAOYSA-M 0.000 claims description 3
- 229940040692 lithium hydroxide monohydrate Drugs 0.000 claims description 3
- 238000003837 high-temperature calcination Methods 0.000 claims description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 9
- 229910001416 lithium ion Inorganic materials 0.000 description 9
- 239000010405 anode material Substances 0.000 description 6
- 229910010710 LiFePO Inorganic materials 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 229910052493 LiFePO4 Inorganic materials 0.000 description 1
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- DVATZODUVBMYHN-UHFFFAOYSA-K lithium;iron(2+);manganese(2+);phosphate Chemical compound [Li+].[Mn+2].[Fe+2].[O-]P([O-])([O-])=O DVATZODUVBMYHN-UHFFFAOYSA-K 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000010450 olivine Substances 0.000 description 1
- 229910052609 olivine Inorganic materials 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
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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
-
- 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
- H01M4/36—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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
-
- 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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- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
-
- 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)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention provides a preparation method of a carbon-coated lithium iron phosphate positive electrode material, which comprises the following steps: s1, adding the mixture of the lithium source, the iron source and the phosphorus source into ball milling equipment, carrying out wet ball milling for the first time to obtain slurry, and drying and calcining the obtained slurry to obtain a lithium iron phosphate semi-finished product; s2, placing the precursor in a mixed solution of a carbon source and an organic solvent, and rapidly stirring; s3, performing ball milling treatment on the dispersion liquid formed in the step S2 to uniformly mix the raw materials; s4, calcining the material obtained in the step S3 at high temperature in a mixed atmosphere of nitrogen and argon; and S5, cooling the calcined substance obtained in the step S4 in a mixed atmosphere of nitrogen and argon to obtain the carbon-coated lithium iron phosphate cathode material. The carbon-coated lithium iron phosphate cathode material prepared by the invention has excellent tap density performance, and the rate capability of the battery is improved. And the cost is low, and the cost performance is high.
Description
Technical Field
The invention relates to the field of new energy materials, in particular to a preparation method of a carbon-coated lithium iron phosphate anode material.
Background
The currently widely used lithium ion battery anode materials mainly include lithium iron phosphate, nickel cobalt manganese ternary materials, lithium iron manganese phosphate, and other lithium-rich materials. With the continuous upgrading and upgrading of electric automobiles and electronic products and the rapid expansion of the application field, higher requirements are also put forward on the safety and energy density of the lithium ion battery. Therefore, the development of the lithium ion battery anode material with high energy density, good cycle performance, rate discharge performance and safety performance has important significance for equipment manufacture and kinetic energy conversion in China.
Compared with other lithium ion anode materials, the battery formed by using the lithium iron phosphate as the anode material has the outstanding advantages of long service life, low cost and high safety, and has larger market share in the lithium ion battery market. LiFePO with olivine structure4The lithium ion battery has the advantages of high capacity (the theoretical specific capacity is 170mAh/g), no toxicity, low price, good thermal stability in a charge-discharge state, small hygroscopicity, excellent charge-discharge cycle performance and the like, and is particularly suitable for being used as a lithium ion high-power supply. Therefore, from the environmental and development perspectives, LiFePO was developed4The positive electrode material makes the lithium ion battery break through the current storage capacity and electric energy limit, further promotes the development of the large-scale (electric vehicles, electric tools and distributed power grid peak shaving), the small-scale (portable electronic products such as multifunctional mobile phones and notebooks in 3G era) and the miniaturization (semiconductor devices, micro devices and thin film batteries) of the lithium ion battery, and finally becomes the watershed of the battery industry. For this purpose, LiFePO4The research on the cathode material becomes a current research hotspot.
However, at the present stage, the problem is that most of the currently marketed lithium iron phosphate is lower than 1.2g cm-3, and lower than other cathode materials, so that the volume energy density is lower, and therefore, the low tap density is a technical problem to be solved urgently.
Disclosure of Invention
The invention aims to provide a preparation method of a carbon-coated lithium iron phosphate positive electrode material, which has excellent tap density performance and improves the rate capability of a battery. And the cost is low, and the cost performance is high.
The invention aims to realize the technical scheme that the preparation method of the carbon-coated lithium iron phosphate anode material comprises the following steps:
s1, mixing a lithium source, an iron source and a phosphorus source according to the weight ratio of lithium: iron: phosphorus: the molar ratio is 1: 1: 1, mixing to obtain a mixture, adding the mixture into ball milling equipment, carrying out wet ball milling for the first time to obtain slurry, and drying and calcining the obtained slurry to obtain a lithium iron phosphate semi-finished product;
s2, placing the lithium iron phosphate precursor obtained in the step S1 in a mixed solution of a carbon source and an organic solvent, and quickly stirring;
s3, performing ball milling treatment on the dispersion liquid formed in the step S2 to uniformly mix the raw materials;
s4, calcining the material obtained in the step S3 at high temperature in a mixed atmosphere of nitrogen and argon;
and S5, cooling the calcined substance obtained in the step S4 in a mixed atmosphere of nitrogen and argon to obtain the carbon-coated lithium iron phosphate cathode material.
Further, in step S1, the lithium source is one or more of lithium carbonate, lithium dihydrogen phosphate, lithium oxalate, and lithium hydroxide monohydrate;
further, in the step S1, the phosphorus source is one or more of ammonium dihydrogen phosphate, phosphoric acid, and lithium dihydrogen phosphate;
further, in step S1, the iron source is one of iron powder and ferroferric oxide.
Further, the temperature in the step S1 is 300-400 ℃ for 2-3 h.
Further, in the step S2, the carbon source is one or a combination of two of glucose and sucrose, and the organic solvent is ethanol or acetone.
Further, the mass ratio of the carbon source to the lithium iron phosphate precursor in the step S2 is 3-10: 100, respectively; the mass ratio of the organic solvent to the lithium iron phosphate precursor is 80-150: 100.
further, the stirring time in the step S2 is 3-5h, and the stirring speed is 600-.
Further, the rotation speed of the ball milling dispersion in the step S3 is 2000-3000 r/min, and the dispersion time is 2-5 h.
Further, the temperature of the high-temperature calcination in the step S4 is 500-800 ℃, and the calcination time is 2-5 hours.
According to the invention, firstly, a semi-finished product is obtained through conventional mixing, calcining and other operations of phosphorus, iron and lithium, a carbon source is further mixed, and then the mixture is stirred, dispersed and calcined at a high temperature and cooled in nitrogen and argon to obtain the carbon-coated lithium iron phosphate cathode material, so that the tap density of the lithium iron phosphate is greatly improved. The method obtains the carbon-coated lithium iron phosphate cathode material, and has the advantages of low cost, simple equipment requirement and short preparation flow.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
A preparation method of a carbon-coated lithium iron phosphate positive electrode material comprises the following steps:
s1, mixing lithium carbonate, iron powder and ammonium dihydrogen phosphate according to the weight ratio of lithium: iron: phosphorus: the molar ratio is 1: 1: 1, mixing to obtain a mixture, adding the mixture into water, carrying out primary wet ball milling to obtain slurry, drying and calcining the obtained slurry at the calcining temperature of 300 ℃ for 3 hours to obtain a lithium iron phosphate semi-finished product;
s2, placing the lithium iron phosphate precursor obtained in the step S1 in a mixed solution of glucose and ethanol, and quickly stirring; stirring for 3 hours at a stirring speed of 1000 revolutions per minute; the mass ratio of the glucose to the lithium iron phosphate precursor is 3: 100, respectively; the mass ratio of the organic solvent to the lithium iron phosphate precursor is 8: 10;
s3, performing ball milling treatment on the dispersion liquid formed in the step S2 to uniformly mix the raw materials; the rotating speed of ball milling dispersion is 2000 r/min, and the dispersion time is 5 h;
s4, calcining the material obtained in the step S3 at high temperature in a mixed atmosphere of nitrogen and argon; the calcining temperature is 500 ℃, and the calcining time is 5 hours;
and S5, cooling the calcined substance obtained in the step S4 in a mixed atmosphere of nitrogen and argon to obtain the carbon-coated lithium iron phosphate cathode material.
Example 2
A preparation method of a carbon-coated lithium iron phosphate positive electrode material comprises the following steps:
s1, mixing lithium dihydrogen phosphate, ferroferric oxide and phosphoric acid according to the weight ratio of lithium: iron: phosphorus: the molar ratio is 1: 1: 1, mixing to obtain a mixture, adding the mixture into water, carrying out primary wet ball milling to obtain slurry, drying and calcining the obtained slurry at 400 ℃ for 2 hours to obtain a lithium iron phosphate semi-finished product;
s2, placing the lithium iron phosphate precursor obtained in the step S1 in a mixed solution of sucrose and propanol, and quickly stirring; stirring for 5 hours at a stirring speed of 600 revolutions per minute; the mass ratio of the sucrose to the lithium iron phosphate precursor is 10: 100, respectively; the mass ratio of the organic solvent to the lithium iron phosphate precursor is 15: 10;
s3, performing ball milling treatment on the dispersion liquid formed in the step S2 to uniformly mix the raw materials; the rotating speed of ball milling dispersion is 3000 r/min, and the dispersion time is 2 h;
s4, calcining the material obtained in the step S3 at high temperature in a mixed atmosphere of nitrogen and argon; the calcining temperature is 800 ℃, and the calcining time is 2 hours;
and S5, cooling the calcined substance obtained in the step S4 in a mixed atmosphere of nitrogen and argon to obtain the carbon-coated lithium iron phosphate cathode material.
Example 3
A preparation method of a carbon-coated lithium iron phosphate positive electrode material comprises the following steps:
s1, mixing lithium oxalate, iron powder and lithium dihydrogen phosphate according to the weight ratio of lithium: iron: phosphorus: the molar ratio is 1: 1: 1, mixing to obtain a mixture, adding the mixture into water, carrying out primary wet ball milling to obtain slurry, drying and calcining the obtained slurry at the calcining temperature of 350 ℃ for 2.5 hours to obtain a lithium iron phosphate semi-finished product;
s2, placing the lithium iron phosphate precursor obtained in the step S1 in a mixed solution of glucose and propanol, and quickly stirring; stirring time is 4h, and stirring speed is 800 revolutions per minute; the mass ratio of the glucose to the lithium iron phosphate precursor is 5: 100, respectively; the mass ratio of the organic solvent to the lithium iron phosphate precursor is 10: 10;
s3, performing ball milling treatment on the dispersion liquid formed in the step S2 to uniformly mix the raw materials; the rotating speed of ball milling dispersion is 2500 rpm, and the dispersion time is 3 h;
s4, calcining the material obtained in the step S3 at high temperature in a mixed atmosphere of nitrogen and argon; the calcining temperature is 600 ℃, and the calcining time is 4 hours;
and S5, cooling the calcined substance obtained in the step S4 in a mixed atmosphere of nitrogen and argon to obtain the carbon-coated lithium iron phosphate cathode material.
Example 4
A preparation method of a carbon-coated lithium iron phosphate positive electrode material comprises the following steps:
s1, mixing lithium hydroxide monohydrate, ferroferric oxide and ammonium dihydrogen phosphate according to the weight ratio of lithium: iron: phosphorus: the molar ratio is 1: 1: 1, mixing to obtain a mixture, adding the mixture into water, carrying out primary wet ball milling to obtain slurry, drying and calcining the obtained slurry at the calcining temperature of 280 ℃ for 2.5 hours to obtain a lithium iron phosphate semi-finished product;
s2, placing the lithium iron phosphate precursor obtained in the step S1 in a mixed solution of sucrose and ethanol, and quickly stirring; the stirring time is 3.5h, and the stirring speed is 900 revolutions per minute; the mass ratio of the sucrose to the lithium iron phosphate precursor is 8: 100, respectively; the mass ratio of ethanol to the lithium iron phosphate precursor is 12: 10;
s3, performing ball milling treatment on the dispersion liquid formed in the step S2 to uniformly mix the raw materials; the rotating speed of ball milling dispersion is 2200 revolutions per minute, and the dispersion time is 4 hours;
s4, calcining the material obtained in the step S3 at high temperature in a mixed atmosphere of nitrogen and argon; the calcining temperature is 700 ℃, and the calcining time is 3 hours;
and S5, cooling the calcined substance obtained in the step S4 in a mixed atmosphere of nitrogen and argon to obtain the carbon-coated lithium iron phosphate cathode material.
The carbon-coated lithium iron phosphate cathode material prepared by the invention has excellent tap density performance, and the rate capability of the battery is improved. And the cost is low, and the cost performance is high.
It should be understood that the examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that any changes and modifications to the present invention may occur to those skilled in the art after reading the present teachings, and such equivalents are also intended to be limited by the appended claims.
Claims (10)
1. A preparation method of a carbon-coated lithium iron phosphate positive electrode material comprises the following steps:
s1, mixing a lithium source, an iron source and a phosphorus source according to the weight ratio of lithium: iron: phosphorus: the molar ratio is 1: 1: 1, mixing to obtain a mixture, adding the mixture into water, carrying out wet ball milling for the first time to obtain slurry, and drying and calcining the obtained slurry to obtain a lithium iron phosphate semi-finished product;
s2, placing the lithium iron phosphate precursor obtained in the step S1 in a mixed solution of a carbon source and an organic solvent, and quickly stirring;
s3, performing ball milling treatment on the dispersion liquid formed in the step S2 to uniformly mix the raw materials;
s4, calcining the material obtained in the step S3 at high temperature in a mixed atmosphere of nitrogen and argon;
and S5, cooling the calcined substance obtained in the step S4 in a mixed atmosphere of nitrogen and argon to obtain the carbon-coated lithium iron phosphate cathode material.
2. The method according to claim 1, wherein the lithium source in step S1 is one or more of lithium carbonate, lithium dihydrogen phosphate, lithium oxalate, and lithium hydroxide monohydrate.
3. The method for preparing the carbon-coated lithium iron phosphate cathode material according to claim 1, wherein the phosphorus source in step S1 is one or more of ammonium dihydrogen phosphate, phosphoric acid, and lithium dihydrogen phosphate.
4. The method for preparing the carbon-coated lithium iron phosphate cathode material according to claim 1, wherein the iron source in step S1 is one of iron powder and ferroferric oxide.
5. The method as claimed in claim 1, wherein the temperature in step S1 is 300-400 ℃ for 2-3 h.
6. The method for preparing the carbon-coated lithium iron phosphate cathode material according to claim 1, wherein the carbon source in step S2 is one or a combination of two of glucose and sucrose, and the organic solvent is ethanol or acetone.
7. The method for preparing the carbon-coated lithium iron phosphate cathode material according to claim 1, wherein the mass ratio of the carbon source to the lithium iron phosphate precursor in the step S2 is 3-10: 100, respectively; the mass ratio of the organic solvent to the lithium iron phosphate precursor is 80-150: 100.
8. the method as claimed in claim 1, wherein the stirring time in step S2 is 3-5h, and the stirring speed is 600-1000 rpm.
9. The method for preparing a carbon-coated lithium iron phosphate cathode material as claimed in any one of claims 1 to 8, wherein the ball milling dispersion in the step S3 is performed at a rotation speed of 2000-3000 rpm for a dispersion time of 2-5 h.
10. The method for preparing a carbon-coated lithium iron phosphate cathode material as claimed in any one of claims 1 to 8, wherein the temperature of the high-temperature calcination in step S4 is 500-800 ℃, and the calcination time is 2-5 hours.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113321197A (en) * | 2021-05-27 | 2021-08-31 | 合肥国轩电池材料有限公司 | Lithium iron phosphate material and preparation method thereof |
| CN113526484A (en) * | 2021-08-06 | 2021-10-22 | 唐山亨坤新能源材料有限公司 | Preparation method of lithium iron phosphate, product and application thereof |
| CN115367723A (en) * | 2022-08-16 | 2022-11-22 | 超威电源集团有限公司 | LiFe 2 Preparation method of F-coated lithium iron phosphate positive electrode material |
| CN116525827A (en) * | 2023-04-28 | 2023-08-01 | 湖北亿纬动力有限公司 | Composite electrode material and preparation method and application thereof |
-
2020
- 2020-11-30 CN CN202011376849.0A patent/CN112599730A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113321197A (en) * | 2021-05-27 | 2021-08-31 | 合肥国轩电池材料有限公司 | Lithium iron phosphate material and preparation method thereof |
| CN113321197B (en) * | 2021-05-27 | 2023-11-07 | 合肥国轩电池材料有限公司 | Lithium iron phosphate material and preparation method thereof |
| CN113526484A (en) * | 2021-08-06 | 2021-10-22 | 唐山亨坤新能源材料有限公司 | Preparation method of lithium iron phosphate, product and application thereof |
| CN115367723A (en) * | 2022-08-16 | 2022-11-22 | 超威电源集团有限公司 | LiFe 2 Preparation method of F-coated lithium iron phosphate positive electrode material |
| CN116525827A (en) * | 2023-04-28 | 2023-08-01 | 湖北亿纬动力有限公司 | Composite electrode material and preparation method and application thereof |
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