CN111115610B - Dry mixing preparation method of lithium iron phosphate - Google Patents
Dry mixing preparation method of lithium iron phosphate Download PDFInfo
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- CN111115610B CN111115610B CN201911367687.1A CN201911367687A CN111115610B CN 111115610 B CN111115610 B CN 111115610B CN 201911367687 A CN201911367687 A CN 201911367687A CN 111115610 B CN111115610 B CN 111115610B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
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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
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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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- 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 discloses a dry mixing preparation method of lithium iron phosphate, which comprises the following steps: 1) Dispersing ferric phosphate, sanding with zirconium balls until the particle size of the material particles is less than or equal to 1um, filtering, drying, and dehydrating at high temperature to obtain nano-scale ferric phosphate with crystal water removed; 2) Preliminarily mixing the nanoscale ferric phosphate obtained in the step 1) with a lithium source, a carbon source and a dopant by using a mixer to obtain a mixture A; 3) Crushing the mixture A by using air flow, mixing for the second time, pressing and shaping, introducing organic compound gas under the protection of atmosphere, and firing at high temperature to obtain large-particle lithium iron phosphate; 4) And (3) carrying out jet milling on the large-particle lithium iron phosphate until the particle size of the material particles is less than or equal to 4um, so as to obtain the lithium iron phosphate suitable for the water system lithium ion battery process. The lithium iron phosphate prepared by the method disclosed by the invention is subjected to nano sanding treatment, the materials can be uniformly mixed in submicron level after being mixed, lithium ions can be embedded into the ferric phosphate more quickly, and the subsequent carbon coating of the lithium iron phosphate is more complete.
Description
Technical Field
The invention belongs to the field of functional energy materials, and particularly relates to a dry mixing preparation method of lithium iron phosphate.
Background
The lithium iron phosphate is a novel lithium ion battery anode material and is characterized by large discharge capacity, low price, no toxicity and no environmental pollution. The existing olivine type LiFePO4 used as the anode material of the lithium ion battery has the advantages of higher theoretical capacity (170 mAh/g), high theoretical cycle performance, stable structure, environmental protection, rich resources and the like.
The internal material of the lithium ion battery consists of a negative electrode material, an electrolyte, a diaphragm and a positive electrode material, and the structure and the performance of the internal material of the battery determine the electrochemical performance of the lithium ion battery. The cathode material of the lithium ion battery is mostly made of graphite materials in commerce, so that the cost of selecting the cathode material has a great influence on the cost of the battery, and the performance of the cathode material also has a great influence on the electrochemical performance of the lithium ion battery, such as rate capability, charge-discharge specific capacitance, cycle performance and the like.
The lithium iron phosphate market is mainly a transfer case market and an energy storage market; the lithium iron phosphate battery is mainly used in the fields of base station energy storage, data center energy storage, household energy storage, wind power generation energy storage, light power generation energy storage and the like in the energy storage market. Is a main direction of the development of energy storage batteries, and has huge market demand scale.
In the production of lithium iron phosphate cathode materials, organic solvents are required to be used for dispersing materials, and ball milling or sand milling is carried out to achieve the aim of refining the material particles. In the process of manufacturing lithium ion batteries, a large amount of organic solvent is also required to dissolve the binder and disperse the positive electrode material, and after the positive electrode material is prepared into slurry, the positive electrode material can be coated on the aluminum foil. The application of a large amount of organic solvents has great influence on the environment and conceals great potential safety hazards. Enterprises are required to bear huge cost pressure for protecting the environment and recycling the organic solvent.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a dry mixing preparation method of lithium iron phosphate, which is applicable to a water system lithium battery process, does not need to use an organic solvent and has low production cost.
The technical scheme adopted for solving the technical problems is as follows: a dry mixing preparation method of lithium iron phosphate comprises the following steps:
1) Adding ferric phosphate into deionized water for dispersion, then transferring into a nano sand mill, sanding with zirconium balls with the diameter of 0.1-0.8mm for 1-8 hours until the particle size of material particles is less than or equal to 1um, filtering, drying at 60-160 ℃, and carrying out high-temperature dehydration treatment at 400-740 ℃ for 6-14 hours in an atmosphere environment to obtain nano-grade ferric phosphate with crystal water removed;
2) The nano-grade ferric phosphate with the crystal water removed, the lithium source, the carbon source and the dopant obtained in the step 1) are primarily mixed for 4 to 16 hours by a mixer according to the proportion of FeP to Li to C to X=1 to 0.9-1.2 to 0.6-1 to 0.001-0.008, so as to obtain a uniform mixture A of the ferric phosphate, the lithium source, the carbon source and the dopant;
3) Crushing the mixture A obtained in the step 2) by using air flow, mixing the crushed mixture A for the second time until the particle size is less than or equal to 3um, namely, uniformly mixing submicron-sized materials, pressing and shaping the mixture A, putting the mixture A into a high-temperature furnace, introducing organic compound gas under the protection of atmosphere, and firing the mixture A for 4 to 10 hours at 600 to 900 ℃ to obtain large-particle lithium iron phosphate;
4) And 3) carrying out jet milling on the large-particle lithium iron phosphate obtained in the step 3) until the particle size of the material particles is less than or equal to 4um, so as to obtain the lithium iron phosphate suitable for the water system lithium ion battery process.
Preferably, the nano sand mill in the step 1) is used for sand milling for 1-8 hours by using zirconium balls with the diameter of 0.1-0.7 mm.
Preferably, the drying temperature in the step 1) is 60-140 ℃, and the dehydration temperature is 450-740 ℃.
Preferably, the atmosphere in the step 1) is one or two or more of dry air, nitrogen and argon.
Preferably, the lithium source in the step 2) is one or two or more of lithium oxide, lithium hydroxide, lithium carbonate and lithium acetate; the carbon source is one or two or more of glucose, sucrose, chitosan and cyclodextrin; the dopant is one or two or more of Mg, mn, ti, nb, Y, ni, rb; the ratio of the ferric phosphate to the lithium source, the carbon source and the dopant is FeP to Li to C to X=1 to 0.9-1.15 to 0.65-1 to 0.001-0.007.
Preferably, the protective atmosphere in the step 3) is one or two or more of nitrogen, argon and carbon dioxide.
Preferably, the organic compound gas in the step 3) is one or two or more of methane, ethane, ethylene and acetylene.
Preferably, the firing temperature in the step 3) is 640-850 ℃.
Preferably, the large-particle lithium iron phosphate in the step 4) is crushed after being dried at the dew point of-5 ℃.
In the lithium iron phosphate production, the materials are mixed and refined by a dry method to prepare the product, an organic solvent is not needed in the sanding process, the influence of the organic solvent on the environment and the corresponding potential safety hazard are avoided, and meanwhile, the production cost is effectively reduced due to the fact that the organic solvent is not used; the lithium iron phosphate anode material overcomes the problems that the active material is low in proportion and difficult to disperse in the pulping process of the same product in the water system process in the process of using the water system process lithium ion battery; in the coating and tabletting process, the adhesive is poor, powder falls off, the pole piece is brittle, easy to crack and fall off and the like; after the battery is manufactured, the problems of poor capacity exertion, poor power performance, low cycle life and the like are solved, and the problems of environmental protection, safety and cost caused by using an organic solvent in the production of a positive electrode material and the manufacturing process of a lithium ion battery are well solved.
The beneficial effects of the invention are as follows: (1)the sintering process in the production of the lithium iron phosphate material has the required time which is 20-30% less than that in the production of the same material; (2) the invention adopts the aqueous nanometer sand milling process mode to carry out the pre-processing to the ferric phosphate so as to change the particle volume of the ferric phosphate, does not need to use organic solvents, and in addition, in the step 3), the mixture A is mixed by adopting a dry mixing process that compressed air flow drives mixture particles to carry out opposite-impact mixing, and also does not adopt a wet mixing process of organic solvents, namely, the lithium iron phosphate material of the invention does not need to be dispersed by organic solvents in production, has no corresponding environmental influence and potential safety hazard, and the cost is reduced by 20-30 percent compared with the cost of preparing the material by using the organic solvents in a dispersing way; (3) in the process of using a water-based process and a lithium ion battery, the lithium iron phosphate anode material disclosed by the invention has the following advantages that the adding amount of the lithium iron phosphate in the slurry of the same material is 91%; compaction density of 1.9-2.1g/cm 3 The pole piece is fragile and is suitable for blanking; the addition amount of the lithium iron phosphate in the material slurry is 94.5 percent, and the compaction density is 2.2 to 2.4g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The pole piece is soft, and does not break or drop after being bent at 90 degrees; (4) the drying time is 1/3 less than that of the same-row products, and the problems of environmental protection, safety and cost caused by using an organic solvent in the production of the anode material and the manufacturing process of the lithium ion battery are well solved.
Drawings
Fig. 1 is a discharge capacity after a lithium battery was fabricated using the lithium iron phosphate of the present invention.
Fig. 2 is a 1C charge-discharge cycle capacity retention after a lithium battery was prepared using the lithium iron phosphate of the present invention.
Fig. 3 is an electron microscope image of the lithium iron phosphate of the present invention.
Detailed Description
In order to make the present invention better understood by those skilled in the art, the following description will make clear and complete descriptions of the technical solutions of the embodiments of the present invention with reference to the accompanying drawings in which it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, shall fall within the scope of the present invention.
Example 1
A dry mixing preparation method of lithium iron phosphate comprises the following steps:
1) Weighing 800g of ferric phosphate material, adding into 1485g of deionized water according to 35% of solid content, stirring and dispersing at a speed of 120r/min, transferring into a nano sand mill, sanding with a zirconium ball of 0.7mm for 7h to enable the particle size of the material to be less than 1um, filtering, drying at 140 ℃ for 18h, and dehydrating at high temperature of 740 ℃ for 6h in a nitrogen environment to obtain the nano ferric phosphate without crystal water;
2) Mixing the ferric phosphate obtained in the step 1) with lithium oxide, glucose and magnesium oxide according to a molar ratio FeP to Li to C and Mg=1:0.9:1:0.007, and then placing the mixture into a mixer for 12 hours for preliminary mixing to obtain a mixture A of the ferric phosphate, the lithium oxide, glucose and magnesium oxide;
3) Crushing the mixture A of the ferric phosphate, the lithium oxide, the glucose and the magnesium oxide obtained in the step 2) by using air flow, mixing the mixture A for the second time until the particle size is less than 3um, namely, uniformly mixing submicron-sized materials, pressing and shaping the mixture A, then adding the mixture A into a high-temperature furnace, heating the mixture A to 640 ℃ at a speed of 5 ℃/min, and continuously introducing methane gas at a flow speed of 0.2L/min under the protection of nitrogen atmosphere to fire the mixture A for 10 hours to obtain large-particle lithium iron phosphate;
4) And 3) carrying out jet milling on the large-particle lithium iron phosphate obtained in the step 3) under a dry environment with a dew point of minus 5 ℃ until the particle size of the material is less than 4um, thereby obtaining the lithium iron phosphate suitable for the water system lithium ion battery process.
Example 2
A dry mixing preparation method of lithium iron phosphate comprises the following steps:
1) Weighing 800g of ferric phosphate material, adding into 1485g of deionized water according to 35% of solid content, stirring and dispersing at a speed of 120r/min, transferring into a nano sand mill, sanding with a zirconium ball of 0.5mm for 5h to enable the particle size of the material to be less than 1um, drying at 120 ℃ for 18h after filtering, and dehydrating at high temperature of 680 ℃ for 8h in an argon environment to obtain the nano ferric phosphate without crystal water;
2) Mixing the ferric phosphate obtained in the step 1) with strong lithium oxide, sucrose and manganese carbonate according to a molar ratio FeP: li: C: mn=1:1:0.9:0.005, and then placing the mixture into a mixer for 8 hours for preliminary mixing to obtain a mixture A of the ferric phosphate, the strong lithium oxide, the sucrose and the manganese carbonate;
3) Crushing the mixture A of the ferric phosphate, the strong lithium oxide, the sucrose and the manganese carbonate obtained in the step 2) by using air flow, mixing the mixture A for the second time until the particle size is less than 3um, namely, uniformly mixing submicron-sized materials, pressing and shaping the mixture A, then adding the mixture A into a high-temperature furnace, heating the mixture A to 720 ℃ at a speed of 5 ℃/min, and continuously introducing ethane gas at a flow speed of 0.2L/min under the protection of argon atmosphere for firing for 8 hours to obtain large-particle lithium iron phosphate;
4) And 3) carrying out jet milling on the large-particle lithium iron phosphate obtained in the step 3) under a dry environment with a dew point of minus 5 ℃ until the particle size of the material is less than 4um, thereby obtaining the lithium iron phosphate suitable for the water system lithium ion battery process.
Example 3
A dry mixing preparation method of lithium iron phosphate comprises the following steps:
1) Weighing 800g of ferric phosphate material, adding into 1485g of deionized water according to 35% of solid content, stirring and dispersing at a speed of 120r/min, transferring into a nano sand mill, and sanding with a zirconium ball of 0.3mm for 5h to enable the particle size of the material to be less than 1um, drying at 100 ℃ for 18h after filtering, and carrying out dehydration treatment at high temperature of 600 ℃ for 10h in an argon environment to obtain the nano ferric phosphate without crystal water;
2) Mixing the ferric phosphate obtained in the step 1) with lithium carbonate, chitosan and titanium oxide according to a molar ratio FeP: li: C: ti=1:1.05:0.65:0.004, and then placing the mixture into a mixer for 14h for preliminary mixing to obtain a mixture A of the ferric phosphate, the lithium carbonate, the chitosan and the titanium oxide;
3) Crushing the mixture A of the ferric phosphate, the lithium carbonate, the chitosan and the titanium oxide obtained in the step 2) by using air flow, mixing the mixture A for the second time until the particle size is less than 3um, namely, uniformly mixing submicron-sized materials, pressing and shaping the mixture A, then adding the mixture A into a high-temperature furnace, heating the mixture A to 760 ℃ at a speed of 5 ℃/min, and continuously introducing ethylene gas at a flow speed of 0.2L/min under the protection of carbon dioxide atmosphere, and firing the mixture A for 8 hours to obtain large-particle lithium iron phosphate;
4) And 3) carrying out jet milling on the large-particle lithium iron phosphate obtained in the step 3) under a dry environment with a dew point of minus 5 ℃ until the particle size of the material is less than 4um, thereby obtaining the lithium iron phosphate suitable for the water system lithium ion battery process.
Example 4
A dry mixing preparation method of lithium iron phosphate comprises the following steps:
1) Weighing 800g of ferric phosphate material, adding into 1485g of deionized water according to 35% of solid content, stirring and dispersing at a speed of 120r/min, transferring into a nano sand mill, sanding with a zirconium ball of 0.2mm for 2h to enable the particle size of the material to be less than 1um, drying at 80 ℃ for 18h after filtering, and dehydrating at high temperature 520 ℃ for 12h in an argon environment to obtain the nano ferric phosphate without crystal water;
2) Mixing the ferric phosphate obtained in the step 1) with lithium acetate, cyclodextrin and yttrium oxide according to a molar ratio FeP: li: C: Y=1:1.1:0.75:0.001, and then placing the mixture into a mixer for 16h to perform preliminary mixing to obtain a mixture A of the ferric phosphate, the lithium acetate, the cyclodextrin and the yttrium oxide;
3) Crushing the mixture A of the ferric phosphate, the lithium acetate, the cyclodextrin and the yttrium oxide obtained in the step 2) by using air flow, mixing the mixture A for the second time until the particle size is less than 3um, namely, uniformly mixing submicron-sized materials, pressing and shaping the mixture A, then adding the mixture A into a high-temperature furnace, heating the mixture A to 800 ℃ at a speed of 5 ℃/min, and continuously introducing acetylene gas at a flow speed of 0.2L/min under the protection of nitrogen atmosphere to fire the mixture A for 6 hours to obtain large-particle lithium iron phosphate;
4) And 3) carrying out jet milling on the large-particle lithium iron phosphate obtained in the step 3) under a dry environment with a dew point of minus 5 ℃ until the particle size of the material is less than 4um, thereby obtaining the lithium iron phosphate suitable for the water system lithium ion battery process.
Example 5
A dry mixing preparation method of lithium iron phosphate comprises the following steps:
1) Weighing 800g of ferric phosphate material, adding into 1485g of deionized water according to 35% of solid content, stirring and dispersing at a speed of 120r/min, transferring into a nano sand mill, sanding with a zirconium ball of 0.1mm for 1h to enable the particle size of the material to be less than 1um, drying at 60 ℃ for 18h after filtering, and dehydrating at high temperature of 450 ℃ for 14h in an argon environment to obtain the nano ferric phosphate without crystal water;
2) Mixing the ferric phosphate obtained in the step 1) with lithium oxide, sucrose and nickel oxide according to a molar ratio FeP: li: C: ni=1:1.15:0.85:0.006, and then placing the mixture into a mixer for 6 hours for preliminary mixing to obtain a mixture A of the ferric phosphate, lithium oxide, sucrose and nickel oxide;
3) Crushing and secondarily mixing the mixture A of the ferric phosphate, lithium oxide, sucrose and nickel oxide obtained in the step 2) by using air flow until the particle size is below 3 mu m, namely uniformly mixing submicron-sized materials, pressing and shaping, then adding into a high-temperature furnace, heating to 850 ℃ at 5 ℃/min, continuously introducing methane gas at the flow rate of 0.2L/min under the protection of argon atmosphere, and firing for 4 hours to obtain large-particle lithium iron phosphate;
4) And 3) carrying out jet milling on the large-particle lithium iron phosphate obtained in the step 3) under a dry environment with a dew point of minus 5 ℃ until the particle size of the material is less than 4um, thereby obtaining the lithium iron phosphate suitable for the water system lithium ion battery process.
As shown in fig. 1, the discharge capacity of the soft package 4ah lithium battery prepared by using the lithium iron phosphate as the positive electrode material through the aqueous battery process is 0.2C current, 0.5C current and 1C current. Fig. 2 shows the capacity retention efficiency of the following 1C charge-discharge cycle of the pouch cell.
The foregoing detailed description is provided to illustrate the present invention and not to limit the invention, and any modifications and changes made to the present invention within the spirit of the present invention and the scope of the appended claims fall within the scope of the present invention.
Claims (8)
1. The dry mixing preparation method of the lithium iron phosphate is characterized by comprising the following steps of:
1) Adding ferric phosphate into deionized water for dispersion, then transferring into a nano sand mill, sanding with zirconium balls with the diameter of 0.1-0.8mm for 1-8 hours until the particle size of material particles is less than or equal to 1um, filtering, drying at 60-160 ℃, and carrying out high-temperature dehydration treatment at 400-740 ℃ for 6-14 hours in an atmosphere environment to obtain nano-grade ferric phosphate with crystal water removed;
2) The nano-grade ferric phosphate with the crystal water removed, the lithium source, the carbon source and the dopant obtained in the step 1) are primarily mixed for 4 to 16 hours by a mixer according to the proportion of FeP to Li to C to X=1 to 0.9-1.2 to 0.6-1 to 0.001-0.008, so as to obtain a uniform mixture A of the ferric phosphate, the lithium source, the carbon source and the dopant; the lithium source is one or two or more of lithium oxide, lithium hydroxide, lithium carbonate and lithium acetate; the carbon source is one or two or more of glucose, sucrose, chitosan and cyclodextrin; the dopant is one or two or more of Mg, mn, ti, nb, Y, ni, rb; the ratio of the ferric phosphate to the lithium source, the carbon source and the dopant is FeP to Li to C to X=1 to 0.9-1.15 to 0.65-1 to 0.001-0.007;
3) Crushing the mixture A obtained in the step 2) by using air flow, mixing the crushed mixture A for the second time until the particle size is less than or equal to 3um, pressing and shaping the mixture A, putting the mixture A into a high-temperature furnace, introducing organic compound gas under the protection of atmosphere, and firing the mixture A for 4 to 10 hours at 600 to 900 ℃ to obtain large-particle lithium iron phosphate;
4) And 3) carrying out jet milling on the large-particle lithium iron phosphate obtained in the step 3) until the particle size of the material particles is less than or equal to 4um, so as to obtain the lithium iron phosphate suitable for the water system lithium ion battery process.
2. The dry mixing preparation method of lithium iron phosphate according to claim 1, wherein: and (3) sanding the nano sand mill in the step 1) for 1-8 hours by using a zirconium ball with the diameter of 0.1-0.7 mm.
3. The dry mixing preparation method of lithium iron phosphate according to claim 1, wherein: the drying temperature in the step 1) is 60-140 ℃, and the dehydration temperature is 450-740 ℃.
4. The dry mixing preparation method of lithium iron phosphate according to claim 1, wherein: the atmosphere in the step 1) is one or two or more of dry air, nitrogen and argon.
5. The dry mixing preparation method of lithium iron phosphate according to claim 1, wherein: the protective atmosphere in the step 3) is one or two or more of nitrogen, argon and carbon dioxide.
6. The dry mixing preparation method of lithium iron phosphate according to claim 1, wherein: the organic compound gas in the step 3) is one or two or more of methane, ethane, ethylene and acetylene.
7. The dry mixing preparation method of lithium iron phosphate according to claim 1, wherein: the firing temperature in the step 3) is 640-850 ℃.
8. The dry mixing preparation method of lithium iron phosphate according to claim 1, wherein: and (3) drying the large-particle lithium iron phosphate in the step 4) at the dew point of-5 ℃ and then crushing.
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| CN112938926B (en) * | 2021-02-19 | 2022-04-29 | 贵州安达科技能源股份有限公司 | Lithium iron phosphate and preparation method thereof |
| CN113104829B (en) * | 2021-03-19 | 2024-02-09 | 合肥国轩电池材料有限公司 | Lithium iron phosphate material and preparation method and application thereof |
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| CN106654227A (en) * | 2017-01-18 | 2017-05-10 | 新乡天力锂能股份有限公司 | Preparation method of lithium nickel cobalt manganese oxide positive electrode material |
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| CN101693532B (en) * | 2009-10-16 | 2011-06-29 | 清华大学 | Method for preparing lithium ferrous phosphate |
| CN103268938A (en) * | 2013-01-22 | 2013-08-28 | 合肥国轩高科动力能源股份公司 | Method for preparing lithium manganese iron phosphate solid solution lithium-ion cathode material |
| CN104892070A (en) * | 2015-05-29 | 2015-09-09 | 宁夏农林科学院 | Method for preparing biological biochar based fertilizer applicable to improvement of low-quality light sierozem |
| CN106229505B (en) * | 2016-08-17 | 2019-10-25 | 深圳市贝特瑞纳米科技有限公司 | A kind of high-density spherical nano lithium iron phosphate material and preparation method thereof and lithium ion battery comprising it |
| CN107814372A (en) * | 2017-11-02 | 2018-03-20 | 沈阳国科金能新材料有限公司 | A kind of preparation method and application of lithium iron phosphate positive material |
| CN110600708A (en) * | 2019-09-25 | 2019-12-20 | 贝特瑞（天津）纳米材料制造有限公司 | Preparation method of step-by-step metal ion-doped and carbon-coated lithium iron phosphate positive electrode material |
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| CN104009223A (en) * | 2014-06-18 | 2014-08-27 | 中信国安盟固利电源技术有限公司 | Method for wrapping lithium cobalt oxide serving as anode material of lithium ion secondary battery through wet method |
| CN106654227A (en) * | 2017-01-18 | 2017-05-10 | 新乡天力锂能股份有限公司 | Preparation method of lithium nickel cobalt manganese oxide positive electrode material |
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