CN115602833A - Method for synthesizing lithium iron phosphate hollow spheres by solid phase method and high-performance lithium battery - Google Patents

Method for synthesizing lithium iron phosphate hollow spheres by solid phase method and high-performance lithium battery Download PDF

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CN115602833A
CN115602833A CN202110775829.9A CN202110775829A CN115602833A CN 115602833 A CN115602833 A CN 115602833A CN 202110775829 A CN202110775829 A CN 202110775829A CN 115602833 A CN115602833 A CN 115602833A
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lithium
iron phosphate
lithium iron
solid phase
synthesizing
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肖丹
陈露
孟岩
王玉珏
王鹏飞
刘林
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Sichuan University
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Sichuan University
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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
    • 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
    • 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
    • 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 method for synthesizing lithium iron phosphate hollow spheres by a solid phase method and a high-performance lithium battery assembled by materials synthesized by the method. The prepared spherical lithium iron phosphate material has a hollow structure, the hollow structure can be fully contacted with an electrolyte, a rapid lithium ion migration channel is provided, the spherical lithium iron phosphate material has high discharge capacity and smaller impedance, and the macroscopic expression shows excellent electrochemical reversibility and dynamic behavior.

Description

Method for synthesizing lithium iron phosphate hollow spheres by solid phase method and high-performance lithium battery
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a method for synthesizing lithium iron phosphate hollow spheres by a solid phase method and a high-performance lithium battery.
Background
The lithium ion battery has started the revolution of energy storage technology and is playing a role in the development process of chemical power supplyA very important role. The electrochemical performance of the lithium ion battery anode material can fully influence the performance of the whole lithium ion battery. Among the positive electrode materials, lithium cobaltate (LiCoO) 2 ) Occupies the main market of portable electronic products, but the cobalt resource is scarce, the price is high, and the application field is limited; ternary materials (NCM and NCA) are currently applied to the field of new energy electric automobiles on a large scale, but the safety is not high enough; lithium iron phosphate (LiFePO) with a slightly lower discharge plateau 4 ) Has the characteristics of extraction safety, environmental friendliness and low cost, and is a development object with great potential.
Spherical lithium iron phosphate materials generally have excellent electrochemical performance. Traditional spherical lithium iron phosphate particles are synthesized by a hydrothermal method, a solvothermal method, a sol-gel method and a spray drying method, but the lithium iron phosphate is synthesized by a low-cost solid phase method in most industries. The method adopts a low-cost path to synthesize high-performance materials, and is more easily accepted and popularized. Therefore, the method is expected to realize the preparation of the spherical lithium iron phosphate material by the solid-phase method without the template additive through screening the material.
Disclosure of Invention
The invention aims to provide a solid-phase synthesis method of a lithium iron phosphate hollow sphere and a lithium battery with high rate performance by using a hollow sphere lithium iron phosphate material prepared by the method.
The purpose of the invention is realized by the following technical scheme:
the solid-phase synthesis method of the lithium iron phosphate hollow sphere comprises the steps of uniformly mixing a lithium source, an iron source, a phosphorus source and a carbon source to obtain a precursor; and calcining the precursor at high temperature to obtain the lithium iron phosphate material with the hollow sphere structure.
Optionally, the lithium source for synthesizing the lithium iron phosphate hollow sphere by the solid phase method is one or more of lithium carbonate, lithium hydroxide, lithium acetate, lithium nitrate and lithium phosphate.
Optionally, the iron source for synthesizing the lithium iron phosphate hollow spheres by the solid phase method is one or more of ferrous oxalate, ferrous carbonate, ferrous gluconate, ferric nitrate and ferric phosphate.
Optionally, the phosphorus source for synthesizing the lithium iron phosphate hollow spheres by the solid phase method is one or more of ammonium dihydrogen phosphate, ammonium polyphosphate, diammonium hydrogen phosphate, lithium dihydrogen phosphate and lithium dihydrogen phosphate.
Optionally, the carbon source for synthesizing the lithium iron phosphate hollow sphere by the solid phase method is one or more of glucose, sucrose, citric acid, polyethylene glycol, polyvinyl alcohol, starch, polyvinylidene fluoride, acetylene black and carbon black.
Optionally, the method for synthesizing the uniformly mixed material of the lithium iron phosphate hollow sphere by the solid phase method is one or more of wet high-energy ball milling, dry high-energy ball milling, wet planetary ball milling, dry planetary ball milling and grinding.
A high performance lithium battery comprising: positive pole, negative pole, its characterized in that: the cathode is a hollow spherical lithium iron phosphate material prepared by the method of any one of claims 1 to 6.
Optionally, the negative electrode material is one of graphite, a carbon-silicon composite material, metallic lithium, graphene oxide, and lithium titanate.
According to the technical scheme, the low-cost solid-phase synthesis steps are optimized, the polymer raw material is introduced into the synthesis of the traditional lithium iron phosphate material based on the cohesive behavior of the polymer under the temperature field, and the lithium iron phosphate with the hollow sphere structure is prepared, can provide a rapid lithium ion migration channel, and shows excellent electrochemical behavior.
Drawings
Fig. 1 is a scanning electron microscope morphology comparison diagram of the lithium iron phosphate materials prepared in example 1 and comparative examples 1 to 3.
Fig. 2 is a scanning electron microscope topography of the cross section of the lithium iron phosphate material prepared in example 1.
Fig. 3 is a comparative scanning electron microscope image of the lithium iron phosphate materials prepared in example 1 and comparative examples 4 and 5.
Fig. 4 is a graph comparing constant current charge and discharge cycle performance at 0.1C rate of the lithium battery assembled in example 6 with the lithium batteries assembled in comparative examples 8 to 10.
Fig. 5 is a graph comparing the constant current charge-discharge cycle performance at 0.1C rate of the lithium battery assembled in example 6 with the lithium batteries assembled in comparative examples 11 and 12.
Fig. 6 is a graph comparing electrochemical impedance of the lithium battery assembled in example 6 with that of the lithium battery assembled in comparative example 8.
Fig. 7 is a graph comparing cyclic voltammetry of the lithium battery assembled in example 6 with that of the lithium battery assembled in comparative example 8.
Fig. 8 is a graph comparing the constant current charge and discharge cycle performance at 10C rate of the lithium battery assembled in example 6 with the lithium batteries assembled in comparative example 8, comparative example 11, and comparative example 12.
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
Detailed Description
In order to make the aforementioned and other objects, features and advantages of the present invention more apparent, the following detailed description of the embodiments of the present invention is given without any limitation thereto.
The idea of the invention is to uniformly mix a lithium source, an iron source, a phosphorus source and a carbon source to obtain a precursor; and calcining the precursor at high temperature to obtain the lithium iron phosphate material with the hollow sphere structure.
The lithium source used for synthesizing the lithium iron phosphate hollow sphere by the solid phase method is one or more of lithium carbonate, lithium hydroxide, lithium acetate, lithium nitrate and lithium phosphate.
The iron source for synthesizing the lithium iron phosphate hollow spheres by the solid phase method is one or more of ferrous oxalate, ferrous carbonate, ferrous gluconate, ferric nitrate and ferric phosphate.
The phosphorus source for synthesizing the lithium iron phosphate hollow spheres by the solid phase method is one or more of ammonium dihydrogen phosphate, ammonium polyphosphate, diammonium hydrogen phosphate, lithium dihydrogen phosphate and lithium dihydrogen phosphate.
The carbon source used for synthesizing the lithium iron phosphate hollow spheres by the solid phase method is one or more of glucose, sucrose, citric acid, polyethylene glycol, polyvinyl alcohol, starch, polyvinylidene fluoride, acetylene black and carbon black.
The invention is used for
The method for synthesizing the uniformly mixed material of the lithium iron phosphate hollow sphere by the solid phase method comprises one or more of wet high-energy ball milling, dry high-energy ball milling, wet planetary ball milling, dry planetary ball milling and grinding.
When the lithium iron phosphate hollow sphere material is adopted to assemble a battery, the negative electrode material can be graphite, a carbon-silicon composite material, metallic lithium, graphene oxide and lithium titanate.
The present invention is further illustrated by the following specific examples and comparative examples. The reagents, materials and instruments used in the following description are all conventional reagents, conventional materials and conventional instruments which can be purchased and obtained from normal channels unless otherwise specified.
Example 1:
the lithium source of this example is lithium carbonate, the iron source is ferrous oxalate, the phosphorus source is ammonium polyphosphate, and the carbon source is glucose and polyethylene glycol:
lithium carbonate, ferrous oxalate, ammonium polyphosphate, glucose and polyethylene glycol are used according to a molar ratio of 0.5:1:1.2:0.1:0.1, mixing, grinding and mixing in a mortar;
carrying out wet high-energy ball milling treatment on the mixture for 2 hours;
transferring the material uniformly mixed by high-energy ball milling to an oven at 80 ℃ for drying;
and transferring the dried material to a tubular furnace, and calcining for 4 hours at 650 ℃ in an argon atmosphere to obtain the product lithium iron phosphate hollow sphere material.
Example 2:
the lithium source in this example is lithium carbonate, the iron source is ferrous oxalate, the phosphorus source is ammonium polyphosphate, and the carbon source is glucose and polyethylene glycol:
lithium carbonate, ferrous oxalate, ammonium polyphosphate, glucose and polyethylene glycol are used according to a molar ratio of 0.5:1:1.2:0.1:0.1, mixing, grinding and mixing in a mortar;
carrying out dry high-energy ball milling treatment on the mixture for 2 hours;
transferring the material uniformly mixed by high-energy ball milling to an oven at 80 ℃ for drying;
and transferring the dried material to a tubular furnace, and calcining for 4 hours at 650 ℃ in an argon atmosphere to obtain the product lithium iron phosphate material.
Example 3:
the lithium source of this example is lithium carbonate, the iron source is ferrous oxalate, the phosphorus source is ammonium polyphosphate, and the carbon source is glucose and polyethylene glycol:
lithium carbonate, ferrous oxalate, ammonium polyphosphate, glucose and polyethylene glycol are used according to a molar ratio of 0.5:1:1.2:0.1:0.1, mixing, grinding and mixing in a mortar;
carrying out wet planetary ball milling treatment on the mixture for 2 hours;
transferring the planetary ball-milled and uniformly mixed material to an oven at 80 ℃ for drying;
and transferring the dried material to a tubular furnace, and calcining for 4 hours at 650 ℃ in an argon atmosphere to obtain the product lithium iron phosphate material.
Example 4:
the lithium source in this example is lithium carbonate, the iron source is ferrous oxalate, the phosphorus source is ammonium polyphosphate, and the carbon source is glucose and polyethylene glycol:
lithium carbonate, ferrous oxalate, ammonium polyphosphate, glucose and polyethylene glycol are used according to a molar ratio of 0.5:1:1.2:0.1:0.1, mixing, grinding and mixing in a mortar;
carrying out dry planetary ball milling treatment on the mixture for 2 hours;
transferring the planetary ball-milled and uniformly mixed material to an oven at 80 ℃ for drying;
and transferring the dried material to a tubular furnace, and calcining for 4 hours at 650 ℃ in an argon atmosphere to obtain the product lithium iron phosphate material.
Example 5:
the lithium source in this example is lithium carbonate, the iron source is ferrous oxalate, the phosphorus source is ammonium polyphosphate, and the carbon source is glucose and polyethylene glycol:
lithium carbonate, ferrous oxalate, ammonium polyphosphate, glucose and polyethylene glycol are used according to a molar ratio of 0.5:1:1.2:0.1:0.1, grinding and mixing for 0.5h in a mortar;
transferring the uniformly ground material to an oven at 80 ℃ for drying;
and transferring the dried material to a tubular furnace, and calcining for 4 hours at 650 ℃ in an argon atmosphere to obtain the product lithium iron phosphate material.
Example 6:
the hollow spherical lithium iron phosphate material prepared in the example 1 is used for assembling the lithium ion battery by adopting a conventional assembly process, wherein the loading capacity of the lithium iron phosphate anode material is 2mg cm -2 The separator was a 20 μm thick polypropylene separator, and metallic lithium was used for the negative electrode.
Example 7:
the lithium iron phosphate material prepared in the example 3 is used for assembling the lithium ion battery by adopting a conventional assembly process, wherein the loading capacity of the lithium iron phosphate anode material is 2mg cm -2 The separator was a 20 μm thick polypropylene separator, and metallic lithium was used for the negative electrode.
Example 8:
the lithium iron phosphate material prepared in the example 5 is used for assembling the lithium ion battery by adopting a conventional assembly process, wherein the loading capacity of the lithium iron phosphate anode material is 2mg cm -2 The separator was a 20 μm-thick polypropylene separator, and metallic lithium was used for the negative electrode.
Comparative example 1:
the comparative example 1 is different from example 1 in that a phosphorus source is replaced with ammonium dihydrogen phosphate when preparing a lithium iron phosphate material.
Comparative example 2:
the comparative example 2 is different from the example 1 in that a carbon source is changed to a single glucose carbon source when preparing the lithium iron phosphate material.
Comparative example 3:
the difference between the comparative example 3 and the example 1 is that the carbon source is changed to a single polyethylene glycol carbon source when the lithium iron phosphate material is prepared.
Comparative example 4:
the comparative example 4 is different from example 1 in that the time of high energy of the wet process in preparing the lithium iron phosphate material is extended to 4 hours.
Comparative example 5:
the comparative example 5 is different from example 1 in that the time for high energy by the wet process in preparing the lithium iron phosphate material is extended to 6 hours.
Comparative example 6:
the comparative example 6 is different from the example 1 in that the calcination temperature when preparing the lithium iron phosphate material is 600 ℃.
Comparative example 7:
the comparative example 7 is different from the example 1 in that the calcination temperature when preparing the lithium iron phosphate material is 700 ℃.
Comparative example 8
The lithium iron phosphate material prepared in the comparative example 1 was used to assemble a lithium ion battery by a conventional assembly process, wherein the loading of the lithium iron phosphate positive electrode material was 2mg cm -2 The separator was a 20 μm thick polypropylene separator, and metallic lithium was used for the negative electrode.
Comparative example 9
The lithium iron phosphate material prepared in the comparative example 2 is used for assembling the lithium ion battery by adopting a conventional assembly process, wherein the loading capacity of the lithium iron phosphate anode material is 2mg cm -2 The separator was a 20 μm thick polypropylene separator, and metallic lithium was used for the negative electrode.
Comparative example 10
The lithium iron phosphate material prepared in the comparative example 3 is used for assembling the lithium ion battery by adopting a conventional assembly process, wherein the loading capacity of the lithium iron phosphate anode material is 2mg cm -2 The separator was a 20 μm-thick polypropylene separator, and metallic lithium was used for the negative electrode.
Comparative example 11
The lithium iron phosphate material prepared in the comparative example 4 is used for assembling the lithium ion battery by adopting a conventional assembly process, wherein the loading capacity of the lithium iron phosphate anode material is 2mg cm -2 The separator was a 20 μm thick polypropylene separator, and metallic lithium was used for the negative electrode.
Comparative example 12
The lithium iron phosphate material prepared in the comparative example 5 is used for assembling the lithium ion battery by adopting a conventional assembly process, wherein the loading capacity of the lithium iron phosphate anode material is 2mg cm -2 The separator is a 20 μm thick polypropylene separator, and the cathode isWith metallic lithium.
The materials prepared in example 1 and comparative examples 1 to 5 were subjected to a scanning electron microscope test, the cross section of the material prepared in example 1 was subjected to a scanning electron microscope test, the batteries assembled in example 6 and comparative examples 8 to 12 were subjected to a constant current charge and discharge characterization, the batteries assembled in example 6 and comparative example 8 were subjected to an electrochemical impedance test, and the batteries assembled in example 6 and comparative example 8 were subjected to a cyclic voltammetry test.
Fig. 1 is a scanning electron microscope morphology comparison diagram of the lithium iron phosphate materials prepared in example 1 and comparative examples 1 to 3, and it can be seen from fig. 1 that the lithium iron phosphate materials prepared in example 1 and comparative example 2 are spherical particles, and the lithium iron phosphate materials prepared in comparative examples 1 and 3 are bulk particles, which indicates that a phosphorus source and a carbon source have an effect on the formation of spherical particles.
Fig. 2 is a scanning electron microscope topography of a cross section of the lithium iron phosphate material prepared in example 1, and it can be seen from fig. 2 that the spherical particles in example 1 are hollow structures.
Fig. 3 is a comparison graph of the shapes of the scanning electron microscopes of the lithium iron phosphate materials prepared in example 1 and comparative examples 4 and 5, and it can be seen from fig. 3 that the lithium iron phosphate materials prepared in comparative example 4 and 5 are bulk particles, which indicates that the time of wet high-energy ball milling has an influence on the formation of spherical particles.
FIG. 4 is a graph comparing the constant current charge and discharge cycle performance at 0.1C rate of the lithium battery assembled in example 6 with that of the lithium batteries assembled in comparative examples 8 to 10, and it can be seen from FIG. 4 that the specific capacity of the lithium battery assembled in example 6 reaches 163mAh g at 0.1C rate -1 The lithium battery assembled in the comparative example 8 has a specific capacity of 159mAh g at a rate of 0.1C -1 In comparative example 9, the lithium battery assembled in the comparative example 9 has a specific capacity of 158mAh g at a rate of 0.1C -1 In comparative example 10, the lithium battery assembled has a specific capacity of 160mAh g at 0.1C rate -1 It is shown that the hollow sphere structured lithium iron phosphate positive electrode material in example 6 has the best charge and discharge performance.
FIG. 5 shows the results obtained in example 6The comparison graph of the constant current charge-discharge cycle performance of the assembled lithium battery and the lithium batteries assembled in the comparative examples 11 and 12 under the rate of 0.1C shows that the specific capacity of the lithium battery assembled in the comparative example 11 under the rate of 0.1C reaches 153mAh g from the graph of FIG. 5 -1 In comparative example 12, the lithium battery assembled therein had a specific capacity of 158mAh g at a rate of 0.1C -1 The material with the hollow sphere structure is favorable for the charge and discharge performance of the material.
Fig. 6 is a comparison graph of electrochemical impedance of the lithium battery assembled in example 6 and the lithium battery assembled in comparative example 8, and it can be seen from fig. 6 that the impedance curve of the lithium battery assembled in example 6 has lower impedance than that of the lithium battery assembled in comparative example 8, indicating that the lithium iron phosphate material with a hollow sphere structure has better kinetics.
Fig. 7 is a comparison graph of cyclic voltammetry of the lithium battery assembled in example 6 and the lithium battery assembled in comparative example 8, and it can be seen from fig. 7 that the difference between the cyclic voltammetry of the lithium battery assembled in example 6 and the redox peak position of the cyclic voltammetry of the lithium battery assembled in comparative example 8 is smaller, which indicates that the lithium iron phosphate material with a hollow sphere structure has better reversibility.
FIG. 8 is a graph comparing the constant current charge and discharge cycle performance at 10C rate of the lithium battery assembled in example 6 with those of the lithium batteries assembled in comparative examples 8, 11 and 12, and it can be seen from FIG. 8 that the specific capacity of the lithium battery assembled in example 6 reaches 123mAh g at 10C rate -1 In comparative example 8, the lithium battery assembled in the comparative example 8 has a specific capacity of 107mAh g at a rate of 10C -1 In comparative example 11, the lithium battery assembled in the lithium battery has a specific capacity of 101mAh g at a rate of 10C -1 In comparative example 10, the lithium battery assembled in the comparative example 10 had a specific capacity of 100mAh g at a rate of 10C -1 It is shown that the lithium iron phosphate cathode material with a hollow sphere structure in example 6 has the best rate performance.
The present invention is not limited to the above-mentioned embodiments, and based on the technical solutions disclosed in the present invention, those skilled in the art can make some substitutions and modifications to some technical features without creative efforts according to the disclosed technical contents, and these substitutions and modifications are all within the protection scope of the present invention.

Claims (8)

1. A method for synthesizing lithium iron phosphate hollow spheres by a solid phase method is characterized by comprising the following steps: uniformly mixing a lithium source, an iron source, a phosphorus source and a carbon source to obtain a precursor; and calcining the precursor at high temperature to obtain the lithium iron phosphate material with the hollow sphere structure.
2. The method for synthesizing the lithium iron phosphate hollow spheres by the solid phase method according to claim 1, which is characterized by comprising the following steps of: the lithium source is one or more of lithium carbonate, lithium hydroxide, lithium acetate, lithium nitrate and lithium phosphate.
3. The method for synthesizing the lithium iron phosphate hollow spheres by the solid phase method according to claim 1, which is characterized by comprising the following steps of: the iron source is one or more of ferrous oxalate, ferrous carbonate, ferrous gluconate, ferric nitrate and ferric phosphate.
4. The method for synthesizing the lithium iron phosphate hollow spheres by the solid phase method according to claim 1, which is characterized by comprising the following steps of: the phosphorus source is one or more of ammonium dihydrogen phosphate, ammonium polyphosphate, diammonium hydrogen phosphate, lithium dihydrogen phosphate and lithium dihydrogen phosphate.
5. The method for synthesizing the lithium iron phosphate hollow spheres by the solid phase method according to claim 1, which comprises the following steps: the carbon source is one or more of glucose, sucrose, citric acid, polyethylene glycol, polyvinyl alcohol, starch, polyvinylidene fluoride, acetylene black and carbon black.
6. The method for synthesizing the lithium iron phosphate hollow spheres by the solid phase method according to claim 1, which is characterized by comprising the following steps of: the method for uniformly mixing the materials comprises one or more of wet high-energy ball milling, dry high-energy ball milling, wet planetary ball milling, dry planetary ball milling and grinding.
7. A high performance lithium battery comprising: positive pole, negative pole, its characterized in that: the cathode is a hollow spherical lithium iron phosphate material prepared by the method of any one of claims 1 to 6.
8. A high performance lithium battery as claimed in claim 7, wherein: the negative electrode material is one of graphite, a carbon-silicon composite material, metal lithium, graphene oxide and lithium titanate.
CN202110775829.9A 2021-07-08 2021-07-08 Method for synthesizing lithium iron phosphate hollow spheres by solid phase method and high-performance lithium battery Pending CN115602833A (en)

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