CN106981639B - Preparation method of organic salt coated lithium iron phosphate cathode material - Google Patents
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Abstract
The invention relates to a preparation method of an organic salt coated lithium iron phosphate anode material, which comprises the following steps: (a) dissolving an organic salt in a solvent to prepare an organic salt solution; (b) adding lithium iron phosphate into the organic salt solution for mixing, and then heating the solution under the condition of continuous stirring until the solvent is completely volatilized; the chemical general formula of the organic salt is
Wherein R is hydrogen, alkyl, hydrocarbyl or alkyl chain containing alkenyl or/and carboxylate. Thus, the coating layer can be ensured not to be dissolved and not to fall off in the electrode slice preparation and the battery electrochemical circulation process; when the molecular formula of the lithium iron phosphate composite material contains conjugated carbon-carbon double bonds, a lithium ion transmission channel can be formed, the migration rate of lithium ions on the surface of the electrode is improved, the effective contact of electrolyte and a carbon coating layer on the surface of the electrode is prevented, the erosion of the electrolyte to an electrode material in the electrode circulation process is inhibited, and the stability of a lithium iron phosphate structure is ensured.
Description
Technical Field
The invention belongs to the field of lithium ion battery anode materials, relates to a coating modification method of a lithium iron phosphate anode material, and particularly relates to a preparation method of an organic salt coated lithium iron phosphate anode material.
Background
The surface coating is an important way for modifying the performance of the lithium ion battery electrode material and improving the cycling stability of the material. The lithium iron phosphate is an important lithium ion battery anode material, has the outstanding advantages of high specific capacity, good structural stability, stable charging and discharging voltage platform, rich resources, low cost, environmental friendliness and the like, and is widely applied to the fields of power batteries, large-scale energy storage and the like in recent years. However, the lithium iron phosphate material has two outstanding problems of poor electronic conductivity and low lithium ion migration rate, and in order to solve these problems, people mostly use a carbon coating technology, that is, a layer of conductive carbon layer is coated on the surface of the lithium iron phosphate material, so that on one hand, the electronic conductivity of the material is improved, on the other hand, the agglomeration phenomenon in the heat treatment process of the material is limited, and the ion migration property of the material is improved.
Nevertheless, the carbon-coated lithium iron phosphate positive electrode material still has some outstanding problems in the battery charging and discharging process, firstly, the mobility of lithium ions passing through the surface of the lithium iron phosphate is low, and the interface impedance of the material is high, so that the rate discharge performance of the material is not high enough. Moreover, in the long-term electrochemical cycle process of the carbon-coated lithium iron phosphate cathode material, a series of side reactions occur between the surface of the material and the electrolyte, so that an electrode/electrolyte interface film continuously grows, the impedance of the electrode is further increased, and the cycle performance and the storage performance of the battery are reduced. Therefore, by proper coating and modification technology, the lithium ion migration resistance on the surface of the electrode is reduced, and the stability of the electrode/electrolyte phase interface is the key for developing a high-performance lithium iron phosphate positive electrode material.
The surface coating is an effective means for further improving the lithium iron phosphate cathode material, so far, the research on the surface coating of the lithium iron phosphate material is very many, including atomic layer metal coating, metal oxide coating, conductive polymer coating and the like, and the coating methods are also many, such as atomic layer deposition technology, electrolysis technology, spraying technology and the like, and the methods also have some effects, but it must be pointed out that the methods and the coating technologies of the material have high production cost, low yield of the product, and are difficult to solve the problem of industrial mass production.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of organic salt coated lithium iron phosphate for improving the high-temperature stability and the cycling stability of a cathode material.
In order to achieve the purpose, the invention adopts the technical scheme that: a preparation method of an organic salt coated lithium iron phosphate anode material comprises the following steps:
(a) dissolving an organic salt in a solvent to prepare an organic salt solution;
(b) adding lithium iron phosphate into the organic salt solution for mixing, and then heating the solution under the condition of continuous stirring until the solvent is completely volatilized;
the chemical general formula of the organic salt is
Wherein R is hydrogen, alkyl, hydrocarbyl or alkyl chain containing alkenyl or/and carboxylate.
Preferably, the organic salt is an alkyl chain containing alkenyl or an alkyl chain containing alkenyl and carboxylate; the organic salt comprises conjugated carbon-carbon double bonds in a chemical general formula.
Preferably, the organic salt is one or more selected from acrylate, maleate, fumarate and itaconate.
Optimally, the mass ratio of the lithium iron phosphate to the organic salt is 100: 1 to 10.
Optimally, the heating temperature is 50-100 ℃.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages: according to the preparation method of the organic salt coated lithium iron phosphate cathode material, the organic salt with a specific chemical structure is dissolved in the solvent to form a liquid phase and is coated on the surface of the lithium iron phosphate to form a uniform coating layer, so that the quality and the thickness of the coating layer can be easily controlled, and the coating uniformity is ensured; the organic salt is very insoluble in organic solvents commonly used by lithium ion batteries, such as N-methyl pyrrolidone and carbonate solvents, and can ensure that the coating layer is not dissolved and does not fall off in the electrode slice preparation and the battery electrochemical circulation process; when the molecular formula of the lithium iron phosphate material contains conjugated carbon-carbon double bonds, a lithium ion transmission channel can be formed, the migration rate of lithium ions on the surface of the electrode is improved, the effective contact of electrolyte and a carbon coating layer on the surface of the electrode is prevented, the erosion of the electrolyte to the electrode material in the electrode circulation process is inhibited, and the stability of a lithium iron phosphate structure is ensured, so that the rate property and the long-term circulation stability of the material are improved, and particularly the circulation stability of the material under a high-temperature condition is improved.
Drawings
Fig. 1 is a TEM image of the lithium iron phosphate positive electrode material used in different examples: (a) comparative example 1; (b) example 1; (c) example 2; (d) example 3;
fig. 2 is a magnification image of the modified lithium iron phosphate positive electrode material of the lithium ion battery in comparative example 1 and examples 1 to 3;
fig. 3 is a diagram of the post-formation ac impedance of the modified lithium iron phosphate positive electrode material of the lithium ion battery in comparative example 1 and examples 1 to 3;
fig. 4 is an alternating current impedance diagram of the modified lithium iron phosphate positive electrode material of the lithium ion battery in comparative example 1 and examples 1 to 3 after 200 cycles;
fig. 5 is a graph comparing long-term cycling performance of lithium iron phosphate cathode materials of lithium ion batteries modified in comparative example 1 and example 2 at 1C rate under the condition of 60 ℃.
Detailed Description
The preparation method of the organic salt coated lithium iron phosphate anode material comprises the following steps: (a) dissolving an organic salt in a solvent to prepare an organic salt solution; (b) adding lithium iron phosphate into the organic salt solution for mixing, and then heating the solution under the condition of continuous stirring until the solvent is completely volatilized; the chemical general formula of the organic salt is
Wherein R is hydrogen, alkyl, hydrocarbyl or alkyl chain containing alkenyl or/and carboxylate. The organic salt with a specific chemical structure is dissolved in the solvent to form a liquid phase, and the liquid phase is coated on the surface of the lithium iron phosphate to form an even coating layer, so that the quality and the thickness of the coating layer can be easily controlled, and the coating is ensuredUniformity of (a); the organic salt is very insoluble in organic solvents commonly used by lithium ion batteries, such as N-methyl pyrrolidone and carbonate solvents, can ensure that a coating layer is not dissolved and does not fall off in the electrode slice preparation and the battery electrochemical circulation process, inhibit the erosion of electrolyte to an electrode material in the electrode circulation process, and ensure the stability of a lithium iron phosphate structure, thereby improving the rate property and long-term circulation stability of the material, and particularly improving the circulation stability of the material under a high-temperature condition.
The organic salt is an alkyl chain containing alkenyl or an alkyl chain containing alkenyl and carboxylate radical, so that conjugated carbon-carbon double bonds are formed by the alkenyl (namely alkenyl) and double bonds in the structural general formula of the organic salt, a lithium ion transmission channel can be formed, the migration rate of lithium ions on the surface of the electrode is improved, the electrolyte is prevented from being effectively contacted with a carbon coating on the surface of the electrode, and the circulation stability of the material is further improved. The organic salt is preferably one or more selected from the group consisting of acrylate, maleate, fumarate and itaconate salts (the organic salt here is typically the corresponding lithium, sodium or potassium salt). The mass ratio of the lithium iron phosphate to the organic salt is preferably 100: 1-10, and the heating temperature is preferably 50-100 ℃. The solvent is usually water, conventional alcohol or their mixture, and the organic salt solution can also be prepared by preparing the corresponding organic acid into a solution and then adding lye. The drying is carried out by adopting conventional modes such as heating drying, forced air drying or vacuum drying. The organic salt solution may be divided into a plurality of portions in step (b) to perform coating a plurality of times in a batch, which may further improve the coating effect. In step (b), the resulting material may be further dried to remove traces of moisture from the material.
The invention will be further explained with reference to the embodiments of the drawings.
Example 1
The embodiment provides an organic salt coated lithium iron phosphate positive electrode material and a preparation method thereof, and the preparation method comprises the following steps:
(a) dissolving 0.04g of sodium maleate in 10ml of deionized water, and fully stirring to form a homogeneous phase aqueous solution;
(b) adding 2g of lithium iron phosphate into the solution, and mechanically stirring at a high speed to enable the lithium iron phosphate to be completely soaked in the solution, wherein the mass of the maleate is 2% of that of the lithium iron phosphate; carrying out water bath on the obtained mixture at the temperature of 70 ℃, and continuously stirring until the solvent is completely volatilized; then the mixture is placed in a vacuum drying oven at 120 ℃ and dried for 24 hours to remove residual trace moisture.
Example 2
The embodiment provides an organic salt coated lithium iron phosphate positive electrode material and a preparation method thereof, the preparation process of which is basically the same as that in embodiment 1, except that 0.1g of sodium maleate is taken to prepare a solution, and 2g of the lithium iron phosphate positive electrode material is added, so that the mass of the maleate is 5% of that of the lithium iron phosphate.
Example 3
The embodiment provides an organic salt coated lithium iron phosphate positive electrode material and a preparation method thereof, the preparation process of which is basically the same as that in embodiment 1, except that 0.2g of sodium maleate is taken to prepare a solution, and 2g of the lithium iron phosphate positive electrode material is added, so that the mass of the sodium maleate is 10% of that of the lithium iron phosphate.
Example 4
The embodiment provides an organic salt coated lithium iron phosphate positive electrode material and a preparation method thereof, the preparation process of which is basically the same as that in embodiment 2, except that 0.12g of lithium maleate preparation solution is directly taken, and 2g of lithium iron phosphate positive electrode material is added, so that the mass of the maleate is 6% of that of the lithium iron phosphate.
Example 5
The embodiment provides an organic salt coated lithium iron phosphate positive electrode material and a preparation method, the preparation process of which is basically the same as that in embodiment 2, except that 0.076g of maleic acid is directly taken to prepare an aqueous solution, a proper amount of NaOH aqueous solution is added until the PH is 7, the mass of the obtained maleate (sodium maleate) is 0.1g, and 2g of the lithium iron phosphate positive electrode material is added, so that the mass of the maleate is 5% of that of the lithium iron phosphate.
Example 6
The embodiment provides an organic salt coated lithium iron phosphate positive electrode material and a preparation method, the preparation process of which is basically the same as that in embodiment 2, except that 0.1g of lithium maleate is directly taken to prepare an alcohol-water solution, and 2g of lithium iron phosphate positive electrode material is added to obtain 0.1g of lithium maleate, so that the mass of the maleate is 5% of that of the lithium iron phosphate.
Example 7
The embodiment provides an organic salt coated lithium iron phosphate cathode material and a preparation method thereof, the preparation process of which is basically the same as that in embodiment 2, except that 0.1g of sodium acrylate is directly taken to prepare an alcohol aqueous solution, and 2g of the lithium iron phosphate cathode material is added, so that the mass of the sodium acrylate is 5% of that of the lithium iron phosphate.
Example 8
The embodiment provides an organic salt coated lithium iron phosphate cathode material and a preparation method thereof, the preparation process of which is basically the same as that in embodiment 2, except that 0.1g of sodium fumarate is directly taken to prepare an aqueous solution, and 2g of the lithium iron phosphate cathode material is added, so that the mass of the fumarate is 5% of that of the lithium iron phosphate.
Example 9
The embodiment provides an organic salt coated lithium iron phosphate cathode material and a preparation method thereof, the preparation process of which is basically the same as that in embodiment 2, except that 0.1g of sodium itaconate is directly taken to prepare an aqueous solution, and 2g of the lithium iron phosphate cathode material is added, so that the mass of the sodium itaconate is 5% of that of the lithium iron phosphate.
Comparative example 1
The embodiment provides an organic salt coated lithium iron phosphate cathode material and a preparation method thereof, the preparation process of which is basically the same as that in embodiment 1, except that no organic acid salt is added, and a TEM (transmission electron microscope) of the finally obtained lithium iron phosphate material is shown in fig. 1.
As can be seen in fig. 1, as the amount of sodium maleate added increases, the thickness of the coating layer gradually increases. Regardless of the coating amount, the sodium maleate can be uniformly coated on the surface of the lithium iron phosphate anode material to form a uniform and continuous surface coating layer. Fig. 2 compares the rate discharge properties of the electrode material under different coating layer thicknesses, and it can be seen that the rate discharge properties of the material are significantly improved after the organic acid salt containing unsaturated double bonds is coated, and ac impedance studies (fig. 3) indicate that the improvement of the rate properties is mainly related to the reduction of the charge transfer resistance of lithium ions on the surface of the electrode, and after the electrode is formed, the charge transfer resistance of the lithium iron phosphate electrode coated with 5% sodium maleate is reduced by about 50% compared with the charge transfer resistance of the uncoated material, wherein the coating amount is 5% of the minimum material impedance. This is a good demonstration that organic salt coating can effectively reduce the lithium ion transport resistance of the electrode surface. Fig. 4 further compares the impedance behavior of the electrode after 200 cycles of the uncoated material and the organic salt coated material, and as can be seen from comparison with fig. 3, after the uncoated material undergoes long-term charge-discharge cycles, the surface charge transfer resistance of the electrode is significantly increased, which is related to the growth of the passivation film on the surface of the electrode and the oxidation of the electrolyte on the surface of the electrode. In contrast, after the 5% coated lithium iron phosphate material is cycled for 200 times, the charge transfer resistance on the surface of the electrode is hardly increased, which indicates that the surface film of the electrode is very stable, and the oxidative decomposition of the electrolyte on the surface of the electrode is effectively controlled. As can be seen from fig. 5, the cycle performance of the lithium iron phosphate coated with 5% maleate in the high-temperature 1C charge-discharge state is greatly improved compared with that of the raw material, the interface and structural stability of the coating material are improved, and the special high-temperature stability is of great significance for developing high-performance lithium iron phosphate cathode materials applied in special occasions.
TABLE 1 comparison of experimental data for example 2 and examples 4-9
The above embodiments are merely illustrative of the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the content of the present invention and implement the invention, and not to limit the scope of the invention, and all equivalent changes or modifications made according to the spirit of the present invention should be covered by the scope of the present invention.
Claims (3)
1. A preparation method of an organic salt coated lithium iron phosphate anode material is characterized by comprising the following steps:
(a) dissolving an organic salt in a solvent to prepare an organic salt solution;
(b) adding lithium iron phosphate into the organic salt solution for mixing, and then heating the solution under the condition of continuous stirring until the solvent is completely volatilized;
the organic salt is one or more selected from acrylate, maleate, fumarate, itaconate and mesoconate.
2. The method for preparing the organic salt coated lithium iron phosphate positive electrode material according to claim 1, wherein the method comprises the following steps: the mass ratio of the lithium iron phosphate to the organic salt is 100: 1 to 10.
3. The method for preparing the organic salt coated lithium iron phosphate positive electrode material according to claim 1, wherein the method comprises the following steps: the heating temperature is 50-100 ℃.
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| CN110444752B (en) * | 2019-08-12 | 2021-07-20 | 苏州大学 | Ternary cathode material of long-life lithium ion battery and preparation method and application thereof |
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| CN105244508A (en) * | 2015-11-06 | 2016-01-13 | 中国科学院青岛生物能源与过程研究所 | Lithium ion battery high-voltage positive electrode material surface coating method |
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| JP6811007B2 (en) * | 2015-09-09 | 2021-01-13 | 三洋化成工業株式会社 | Method for manufacturing resin for coating non-aqueous secondary battery active material, coating active material for non-aqueous secondary battery, and coating active material for non-aqueous secondary battery |
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| CN103887508A (en) * | 2014-03-24 | 2014-06-25 | 四川兴能新材料有限公司 | Preparation method of polyelectrolyte-coated LiNi0.5Mn1.5O4 positive electrode material |
| CN105244508A (en) * | 2015-11-06 | 2016-01-13 | 中国科学院青岛生物能源与过程研究所 | Lithium ion battery high-voltage positive electrode material surface coating method |
| CN105514394A (en) * | 2016-01-26 | 2016-04-20 | 苏州大学 | Modification method for lithium-ion battery graphite cathode material |
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