CN113745503A - Preparation method of high-compaction lithium iron phosphate cathode material - Google Patents
Preparation method of high-compaction lithium iron phosphate cathode material Download PDFInfo
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Abstract
The invention discloses a preparation method of a high-compaction lithium iron phosphate cathode material, which belongs to the technical field of lithium ion batteries and comprises the steps of firstly adding a lithium source, an iron source, a phosphorus source and a carbon source into a solvent, grinding and drying to obtain a precursor; and sintering the obtained precursor under the protection of nitrogen atmosphere, and crushing to obtain the high-compaction lithium iron phosphate anode material. According to the invention, multiple reaction stages are constructed by utilizing the uniqueness of the lithium source and the difference of different reaction temperatures of different iron sources and the lithium source, and high-compaction lithium iron phosphate composed of different particle sizes is obtained by one-time mixed material sintering.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and relates to a preparation method of a high-compaction lithium iron phosphate positive electrode material.
Background
In recent years, lithium ion batteries have been greatly developed as effective energy storage devices for sustainable energy. The commonly used lithium ion battery anode materials mainly comprise lithium cobaltate, lithium manganate, ternary materials and lithium iron phosphate, wherein the lithium iron phosphate material has stable structure, good safety and ultra-long cycle life, and is widely applied to electric vehicles. With the development of electric vehicles, people have made higher requirements on endurance mileage, and therefore, the energy density of lithium ion batteries needs to be improved. For lithium iron phosphate materials, the actual specific capacity is close to the theoretical value, the improvement range is small, and the difficulty is high, so that the improvement of the compaction density of the lithium iron phosphate material and the energy density of a lithium ion battery becomes a hot point of research in recent years.
In the patent application with publication number CN102916179B, lithium salt, iron source, and phosphorus salt are added twice and mixed, and wet ball milling is performed twice to obtain two groups of slurries with different particle sizes, and then the two groups of slurries are mixed according to different proportions, dried, pre-sintered, wet ball milled for the third time, and then sintered to obtain the high-compaction lithium iron phosphate material. Although the method improves the compaction density by means of grading raw materials with different particle sizes, different equipment is needed for grinding to obtain slurry with different particle sizes, and the final product can be obtained by ball milling and sintering for multiple times, so that the process is complex and the productivity is influenced. The patent application with the publication number of CN103618083B discloses high-compaction lithium iron phosphate obtained by a three-time tabletting method, but the method needs to carry out tabletting, crushing and sintering for many times, the process is complex, and the industrial production cost is high. Patent application publication No. CN106744780A discloses the preparation of high compaction lithium iron phosphate by using an iron source with high compaction density, but the overall yield of the method is low, the productivity is affected and the cost is high. Although the above patent application improves the compaction density of the lithium iron phosphate material to a certain extent, the problems of complex preparation method and high cost still exist.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a method for simply and conveniently preparing high-compaction-density lithium iron phosphate with low cost, multiple reaction stages are constructed by utilizing the uniqueness of a lithium source and the difference of different reaction temperatures of different iron sources and the lithium source, and high-compaction lithium iron phosphate composed of different particle sizes is obtained by one-time material mixing and sintering.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a high-compaction lithium iron phosphate positive electrode material comprises the following steps:
firstly, adding a lithium source, an iron source, a phosphorus source and a carbon source into a solvent, grinding and drying to obtain a precursor;
and sintering the obtained precursor under the protection of nitrogen atmosphere, and crushing to obtain the high-compaction lithium iron phosphate anode material.
Preferably, the lithium source is one or more of lithium phosphate, dilithium hydrogen phosphate and lithium dihydrogen phosphate.
Preferably, the iron source is one or more of iron phosphate, ferric oxide, iron powder, ferroferric oxide and ferrous oxalate.
Preferably, the phosphorus source is one or more of lithium phosphate, dilithium hydrogen phosphate, lithium dihydrogen phosphate and iron phosphate.
Preferably, the molar ratio of the elements of the lithium source, the phosphorus source and the iron source is Li: P: Fe ═ (1-1.1):1 (0.9-1).
Preferably, the carbon source is one or more of sucrose, glucose, cellulose, phenolic resin, polyethylene glycol, polyvinylpyrrolidone and starch; the adding amount of the carbon source is 5-15% of the total mass of the lithium source, the phosphorus source and the iron source.
Preferably, the solvent comprises water, an organic solvent or a mixed solution of the water and the organic solvent; the organic solvent includes: alcohols: such as methanol, ethanol, etc.; aromatic hydrocarbons: benzene, toluene, xylene, etc.; aliphatic hydrocarbons: pentane, hexane, octane, and the like; alicyclic hydrocarbons: cyclohexane, etc.; ethers: ethyl ether, propylene oxide, and the like; lipid: methyl acetate, ethyl acetate, and the like; ketones: acetone, methyl butanone, and the like; and (3) the other: one or more of acetonitrile, pyridine, phenol, and the like.
Preferably, in the grinding process, the granularity of the slurry is controlled to be 300-5000 nm.
Preferably, the sintering condition is that the temperature is raised from room temperature to 200-350 ℃ at the temperature raising rate of 1-10 ℃/min, and the temperature is kept for 1-5 h; then heating to 700-800 ℃ at the same heating rate, and preserving the heat for 3-15 h.
According to the invention, multiple reaction stages are constructed by utilizing the uniqueness of the lithium source and the difference of the reaction temperatures of different iron sources and the lithium source, so that different iron source matrixes can obtain proper growth time, and high-compaction lithium iron phosphate composed of different particle sizes can be obtained only by one-time material mixing and sintering without an additional grading process; on the other hand, the raw materials used in the invention have low cost, no toxicity and no pollution, the overall yield is higher, the preparation process is simple, and the method is suitable for large-scale production.
Drawings
Fig. 1 is an SEM image of lithium iron phosphate prepared in example 1 of the present invention.
Fig. 2 is an XRD pattern of lithium iron phosphate prepared in example 1 of the present invention.
Fig. 3 is a capacity test curve of lithium iron phosphate prepared in example 1 of the present invention.
FIG. 4 is a graph of diffraction peak intensities of different materials as a function of temperature in an in-situ sintering XRD test in example 1 of the present invention.
Fig. 5 is an SEM image of lithium iron phosphate prepared in comparative example 1 of the present invention.
Detailed Description
The invention is further illustrated by the following examples. These examples are only illustrative and are not intended to limit the scope of the invention.
Example 1
Adding lithium phosphate, iron phosphate, ferrous oxalate, ferric oxide, starch and glucose which are 12% of the total mass of the four materials into water according to the mol ratio of Li to P to Fe of 1:1:0.96, carrying out high-energy ball milling until the particle size reaches 700-800 nm, and carrying out spray drying on the slurry. And (3) placing the dried powder in a reaction furnace under the protection of nitrogen, heating to 320 ℃ at the heating rate of 5 ℃/min, preserving heat for 5h, heating to 760 ℃ at the heating rate of 5 ℃/min, preserving heat for 10h, cooling to room temperature, and crushing by airflow to obtain the lithium iron phosphate.
The lithium iron phosphate prepared in example 1 is used as a representative, and the particle and performance of the lithium iron phosphate are characterized as follows:
fig. 1 is an SEM image of lithium iron phosphate prepared in example 1. The obtained sample can be clearly observed to have part of large particles with the particle size of 1-2 mu m and small particles with the particle size of about 400nm, the large particles and the small particles are uniformly distributed and reach effective gradation, so that the compaction density is improved and reaches 2.6g/cm3。
Fig. 2 is an XRD pattern of lithium iron phosphate prepared in example 1. The diffraction peak in the graph corresponds to the standard lithium iron phosphate peak (JCPDS 19-0721) in the PDF card well.
Fig. 3 is a graph illustrating a capacity test of lithium iron phosphate prepared in example 1 of the present invention. According to the capacity test result, the following results are obtained: the 0.1C discharge of the sample can reach 157 mAh/g.
FIG. 4 is a graph of diffraction peak intensities of different materials as a function of temperature in an in-situ sintering XRD test in example 1 of the present invention. The result of the test analysis shows that FePO4The diffraction peak intensity of the compound begins to decrease at 320 ℃, remarkably decreases after 350 ℃, and disappears at 410 ℃; and Fe2O3The diffraction peak intensity of the compound does not start to slowly decrease at 400 ℃ until the compound disappears at 600 ℃; further, LiFePO4The diffraction peak of (1) appears from 340 ℃ and corresponds to FePO4Is reduced and reacts with a lithium source to generate LiFePO4. These analytical results show that FePO4With Fe2O3The reduction and the reaction temperature with the lithium source are greatly different, so that multiple reaction stages can be constructed by controlling the sintering system in FePO4And reacting with a lithium source by maintaining the temperature to form LiFePO4Crystal nucleus growth and formation of large-particle LiFePO4(ii) a And Fe during subsequent elevated temperature2O3LiFePO generated by reduction and reaction with lithium source and phosphorus source4Small particles of LiFePO can be formed4(ii) a Therefore, the characteristics of lithium phosphate, dilithium hydrogen phosphate, lithium dihydrogen phosphate and the like that the decomposition temperature is low and the lithium source and the phosphorus source are provided simultaneously are utilized, and different iron sources react with the lithium source to generate LiFePO4Due to the temperature difference, multiple reaction stages can be constructed, so that different iron source matrixes can obtain proper growth time, and high-compaction lithium iron phosphate composed of different particle sizes can be obtained only by one-time material mixing and sintering without an additional grading process.
Example 2
Adding lithium phosphate, lithium dihydrogen phosphate, iron phosphate, ferroferric oxide, glucose and polyethylene glycol which are 15% of the total mass of the lithium phosphate, the lithium dihydrogen phosphate, the iron phosphate, the ferroferric oxide and the glucose and the polyethylene glycol into ethanol according to the molar ratio of Li to P to Fe of 1.1:1:0.9, carrying out high-energy ball milling, and carrying out spray drying on slurry after the particle size reaches 4500-5000 nm. And (3) placing the dried powder in a nitrogen-protected reaction furnace, heating to 350 ℃ at a heating rate of 1 ℃/min, preserving heat for 1h, heating to 800 ℃ at a heating rate of 1 ℃/min, preserving heat for 3h, cooling to room temperature, and crushing by airflow to obtain the lithium iron phosphate.
Example 3
Adding lithium phosphate, dilithium hydrogen phosphate, iron phosphate, ferrous oxalate, phenolic resin and polyethylene glycol which are 5% of the total mass of the lithium phosphate, the dilithium hydrogen phosphate, the iron phosphate, the ferrous oxalate and the polyethylene glycol into diethyl ether according to the molar ratio of Li to P to Fe of 1.05:1:0.9, carrying out high-energy ball milling, and carrying out spray drying on the slurry after the particle size reaches 1800-2000 nm. And (3) placing the dried powder in a reaction furnace under the protection of nitrogen, heating to 200 ℃ at the heating rate of 10 ℃/min, preserving heat for 5h, heating to 700 ℃ at the heating rate of 10 ℃/min, preserving heat for 15h, cooling to room temperature, and crushing by airflow to obtain the lithium iron phosphate.
Example 4
Adding lithium phosphate, iron phosphate, ferric oxide and glucose accounting for 10% of the total mass of the lithium phosphate, the iron phosphate, the ferric oxide and the glucose into water according to the molar ratio of Li to P to Fe of 1.03:1:1, carrying out high-energy ball milling until the particle size reaches 300-400 nm, and carrying out spray drying on the slurry. And (3) placing the dried powder in a nitrogen-protected reaction furnace, heating to 250 ℃ at a heating rate of 2 ℃/min, preserving heat for 5h, heating to 750 ℃ at a heating rate of 2 ℃/min, preserving heat for 8h, cooling to room temperature, and crushing by airflow to obtain the lithium iron phosphate.
Example 5
Adding lithium phosphate, iron powder and polyvinylpyrrolidone accounting for 5% of the total mass of the lithium phosphate, the iron phosphate and the iron powder into methanol according to the molar ratio of Li to P to Fe being 1:1:1, carrying out high-energy ball milling, and carrying out spray drying on slurry after the particle size reaches 2200-2500 nm. And (3) placing the dried powder in a nitrogen-protected reaction furnace, heating to 350 ℃ at the heating rate of 8 ℃/min, preserving heat for 1h, heating to 800 ℃ at the heating rate of 8 ℃/min, preserving heat for 6h, cooling to room temperature, and crushing by airflow to obtain the lithium iron phosphate.
Example 6
Adding lithium phosphate, iron phosphate, ferroferric oxide, ferric oxide and 15% of glucose and polyethylene glycol of the total mass of the four into water according to the molar ratio of Li to P to Fe of 1.03:1:1, carrying out high-energy ball milling until the particle size reaches 600-700 nm, and carrying out spray drying on the slurry. And (3) placing the dried powder in a reaction furnace under the protection of nitrogen, heating to 300 ℃ at the heating rate of 4 ℃/min, preserving heat for 3h, heating to 730 ℃ at the heating rate of 4 ℃/min, preserving heat for 12h, cooling to room temperature, and crushing by airflow to obtain the lithium iron phosphate.
Comparative example 1
Adding lithium carbonate, iron phosphate, starch and glucose which are 12% of the total mass of the lithium carbonate and the iron phosphate and are 12% of the total mass of the starch and the glucose into water according to the molar ratio of Li to P to Fe of 1:1:0.96, carrying out high-energy ball milling, and carrying out spray drying on the slurry after the particle size reaches 700-800 nm. And (3) placing the dried powder in a reaction furnace under the protection of nitrogen, heating to 320 ℃ at the heating rate of 5 ℃/min, preserving heat for 5h, heating to 760 ℃ at the heating rate of 5 ℃/min, preserving heat for 10h, cooling to room temperature, and crushing by airflow to obtain the lithium iron phosphate.
Fig. 5 is an SEM image of lithium iron phosphate prepared in comparative example 1. It can be clearly observed that the obtained sample has large particles of about 1 μm in size and small particles, and has a compacted density of 2.5g/cm3. Due to the traditional carbonThe unity of the iron source in the lithium and iron phosphate processes generally results in relatively uniform sample particles, resulting in gaps where large particles are packed without small particles filling, and thus, lower compacted density.
The above embodiments are only intended to illustrate the technical solution of the present invention, but not to limit it, and a person skilled in the art can modify the technical solution of the present invention or substitute it with an equivalent, and the protection scope of the present invention is subject to the claims.
Claims (10)
1. The preparation method of the high-compaction lithium iron phosphate anode material is characterized by comprising the following steps of:
firstly, adding a lithium source, an iron source, a phosphorus source and a carbon source into a solvent, grinding and drying to obtain a precursor;
and sintering the obtained precursor under the protection of nitrogen atmosphere, and crushing to obtain the high-compaction lithium iron phosphate anode material.
2. The method of claim 1, wherein the lithium source is one or more of lithium phosphate, dilithium hydrogen phosphate, and lithium dihydrogen phosphate.
3. The method of claim 1, wherein the iron source is one or more of iron phosphate, ferric oxide, iron powder, ferroferric oxide, and ferrous oxalate.
4. The method of claim 1, wherein the phosphorus source is one or more of lithium phosphate, dilithium hydrogen phosphate, lithium dihydrogen phosphate, and iron phosphate.
5. The method according to claim 1, wherein the molar ratio of the elements of the lithium source, the phosphorus source and the iron source is Li: P: Fe ═ (1-1.1):1 (0.9-1).
6. The method of claim 1, wherein the carbon source is one or more of sucrose, glucose, cellulose, phenolic resin, polyethylene glycol, polyvinylpyrrolidone, starch; the adding amount of the carbon source is 5-15% of the total mass of the lithium source, the phosphorus source and the iron source.
7. The method of claim 1, wherein the solvent is one or both of water and an organic solvent; the organic solvent includes: one or more of alcohols, aromatic hydrocarbons, aliphatic hydrocarbons, alicyclic hydrocarbons, ethers, lipids, ketones, acetonitrile, pyridine and phenol.
8. The method according to claim 7, wherein the alcohol is at least one of methanol and ethanol, the aromatic hydrocarbon is at least one of benzene, toluene and xylene, the aliphatic hydrocarbon is at least one of pentane, hexane and octane, the alicyclic hydrocarbon is cyclohexane, the ether is at least one of diethyl ether and propylene oxide, the lipid is at least one of methyl acetate and ethyl acetate, and the ketone is at least one of acetone and methyl butanone.
9. The method according to claim 1, wherein the grinding is performed while controlling a particle size of the slurry to 300 to 5000 nm.
10. The method of claim 1, wherein the sintering conditions are: heating from room temperature to 350 ℃ at the heating rate of 1-10 ℃/min, and keeping the temperature for 1-5 h; then heating to 700-800 ℃ at the same heating rate, and preserving the heat for 3-15 h.
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Cited By (4)
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| CN114335517A (en) * | 2021-12-31 | 2022-04-12 | 欣旺达电动汽车电池有限公司 | Carbon composite lithium iron phosphate cathode material, preparation method and application thereof |
| CN114368737A (en) * | 2022-02-23 | 2022-04-19 | 东莞市创明电池技术有限公司 | High-compaction and high-capacity lithium iron phosphate positive electrode material and preparation method and application thereof |
| CN114524424A (en) * | 2021-12-17 | 2022-05-24 | 青海泰丰先行锂能科技有限公司 | Preparation method of high-compaction high-capacity lithium iron phosphate positive electrode material |
| CN117088352A (en) * | 2023-10-20 | 2023-11-21 | 宁德时代新能源科技股份有限公司 | Preparation method of lithium iron phosphate, positive electrode active material, positive electrode plate, battery and electricity utilization device |
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| CN114335517A (en) * | 2021-12-31 | 2022-04-12 | 欣旺达电动汽车电池有限公司 | Carbon composite lithium iron phosphate cathode material, preparation method and application thereof |
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| CN114368737A (en) * | 2022-02-23 | 2022-04-19 | 东莞市创明电池技术有限公司 | High-compaction and high-capacity lithium iron phosphate positive electrode material and preparation method and application thereof |
| CN117088352A (en) * | 2023-10-20 | 2023-11-21 | 宁德时代新能源科技股份有限公司 | Preparation method of lithium iron phosphate, positive electrode active material, positive electrode plate, battery and electricity utilization device |
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Application publication date: 20211203 |