CN108417773B - Lithium iron phosphate composite electrode and preparation method and application thereof - Google Patents
Lithium iron phosphate composite electrode and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the field of preparation of lithium ion battery materials, and particularly relates to a lithium iron phosphate composite electrode, a preparation method and application thereof, wherein the preparation process of the lithium iron phosphate composite electrode comprises the following steps: firstly, depositing aluminum ions on the surface of a lithium iron phosphate electrode in an oily solvent system by an electrochemical deposition method, drying to obtain a lithium iron phosphate composite electrode A, then depositing lithium salt on the surface of the composite electrode A in the oily solvent system by the electrochemical deposition method, cleaning, and drying to obtain a lithium iron phosphate composite electrode B. The lithium salt deposited by the electrodeposition method has the advantages of high ionic conductivity, high density, strong structural stability and the like, the gram capacity and the rate capability of the material are improved, the electron transmission rate of the material is improved by depending on the characteristic of high conductivity of the foamed aluminum deposited in the middle layer, and the energy density, the rate capability and the cycle performance of the lithium ion battery can be improved by applying the prepared composite electrode to the lithium iron phosphate battery.
Description
Technical Field
The invention belongs to the field of preparation of lithium ion battery materials, and particularly relates to a lithium iron phosphate composite electrode and a preparation method and application thereof.
Background
Lithium iron phosphate is a novel cathode material developed in recent years, and is applied to the fields of passenger cars and the like due to the advantages of high safety performance, environmental friendliness, low price, long cycle life and the like, but along with the publication of ' notice on the supporting policy of popularization and application of new energy automobiles in 2020 ', the ministry of finance and government of China's ministry of finance, the lithium iron phosphate battery is required to have higher energy density so as to reach the highest subsidy standard. The lithium iron phosphate anode material is a main component of lithium iron phosphate, and the quality of the performance of the lithium iron phosphate anode material plays a key role in the multiplying power, the cycle and the energy density of the lithium iron phosphate battery. The gram capacity of the current lithium iron phosphate anode material is generally 150-160mAh/g, and the compaction density of a pole piece is 2.3-2.4g/cm2In between, the energy density of the lithium iron phosphate is low, and the endurance mileage of the electric automobile is affected. The method for improving the energy density of the lithium iron phosphate anode material at present mainly comprises the following steps: the gram capacity and the compaction density of the material are improved by doping metal elements, nano-crystallizing the material and coating the material for densificationHigh in degree and good in compatibility with electrolyte. For example, patent (CN 201310570094.1) discloses a method for producing a high-capacity high-compaction lithium iron phosphate positive electrode material, which is a method for preparing a high-capacity high-compaction lithium iron phosphate positive electrode material by multiple compaction and sintering, so as to effectively achieve the purpose of improving the compaction density, electrochemical gram capacity and cycle performance of lithium iron phosphate, but the solid phase method has low density of a coating layer and low lithium ion transmission rate, which affects the gram capacity and compaction density of the material to be further improved.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a preparation method of a lithium iron phosphate composite electrode, which has high efficiency and can improve the compaction density, gram capacity and rate capability of the lithium iron phosphate electrode.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a lithium iron phosphate composite electrode comprises the following steps:
(1) adding 1 g-5 g of organic aluminum salt into a mixed organic solvent of 10-30 ml of benzene and 70-90 ml of tetrahydrofuran, uniformly stirring, then depositing on a working electrode for 1 min-30 min by adopting an electrochemical deposition method by taking press-formed lithium iron phosphate as the working electrode, a platinum wire as a counter electrode and saturated calomel as a reference electrode, and then cleaning and drying to obtain a lithium iron phosphate composite electrode A;
(2) adding 1 g-5 g of lithium salt into 100ml of ethylene carbonate, uniformly stirring to obtain an organic solvent system, then taking a lithium iron phosphate composite electrode A as a working electrode, a platinum electrode as a counter electrode and saturated calomel as a reference electrode, electrodepositing the lithium salt on the surface of the working electrode by adopting an electrochemical method for 1 min-30 min, and after the deposition is finished, cleaning and drying by adopting the ethylene carbonate to obtain a lithium iron phosphate electrode B, namely the lithium iron phosphate composite electrode.
Further, the preparation method of the molded lithium iron phosphate in the step (1) comprises the following steps: firstly, 80g to 95g of lithium iron phosphate powder, 5g to 20g of polyvinylidene fluoride and 50ml to 100ml of N-methyl pyrrolidone are uniformly mixed to obtain a sticky colloid, and then the sticky colloid is pressed and formed by a tablet machine to obtain a blocky lithium iron phosphate electrode after drying.
Preferably, the aluminum salt in step (1) is one of ethyl aluminum, butyl aluminum, aluminum acetate, aluminum formate, aluminum oxalate and aluminum propionate.
Preferably, the electrochemical deposition method described in step (1) and step (2) is one of cyclic voltammetry, constant pressure method, constant current method, and pulse method.
Preferably, the lithium salt in the step (2) is one of lithium carbonate, lithium hydroxide, lithium metaaluminate, lithium perchlorate and lithium zirconate.
The lithium iron phosphate composite electrode prepared by the preparation method is characterized by comprising lithium iron phosphate and aluminum salt and lithium salt thereof deposited on the surface of the lithium iron phosphate, and the mass ratio of the lithium iron phosphate composite electrode to the aluminum salt is as follows: lithium iron phosphate: aluminum salt: the lithium salt is 100: 1-5: 1 to 5.
The application of the lithium iron phosphate composite electrode is characterized in that the lithium iron phosphate battery mainly comprises the lithium iron phosphate composite electrode, a graphite negative electrode material, a ceramic diaphragm and functional electrolyte thereof.
The electrochemical method has the characteristics of fast preparation process, high density, high consistency, easy control of the process and the like, and the prepared material has the advantages of thin deposited layer, high density, strong structural stability and the like, and can greatly improve the tap density of the material and improve the gram capacity and the rate capability of the material when being applied to the preparation of lithium iron phosphate.
Advantageous effects
(1) According to the invention, the aluminum salt is deposited on the surface of the lithium iron phosphate electrode A, is foamed aluminum and is coated on the surface of the lithium iron phosphate, so that the electronic conductivity of the lithium iron phosphate is improved, the specific surface area of the lithium iron phosphate is reduced, the active points of the lithium iron phosphate are reduced, and the primary efficiency of the lithium iron phosphate is improved; meanwhile, the organic aluminum salt and the lithium iron phosphate have good compatibility and can be uniformly and firmly deposited on the surface of the lithium iron phosphate.
(2) Lithium salt is deposited on the outermost layer through electrochemistry, the transmission rate of lithium ions in the material in the charging and discharging process is improved by the high conductivity characteristic of lithium salt lithium ions, and meanwhile, the foamed aluminum in the middle layer has a nano-pore structure and does not influence the transmission rate of the lithium ions in the charging and discharging process.
(3) The invention adopts an electrochemical method to deposit aluminum salt and lithium salt, has the characteristics of fast preparation process, high density, high consistency, easy control of the process and the like, and the prepared material has the advantages of thin deposition layer, high density, strong structural stability and the like, and can greatly improve the tap density of the material and improve the gram capacity and the rate capability of the material when being applied to the preparation of lithium iron phosphate.
Drawings
Fig. 1 is a graph showing cycle curves of lithium iron phosphate batteries prepared in examples and comparative examples.
Detailed Description
The present invention will be further described with reference to examples and comparative examples, but it should be noted that the following description is only for the purpose of explaining the present invention and does not limit the contents thereof.
Example 1
The preparation method of the block-shaped lithium iron phosphate electrode comprises the following steps:
firstly, uniformly mixing 90g of lithium iron phosphate powder, 10g of polyvinylidene fluoride and 80ml of N-methyl pyrrolidone to obtain a sticky colloid, coating the sticky colloid on foamed aluminum, drying, performing compression molding under the pressure of 10Mpa by using a tablet press, and drying at the temperature of 80 ℃ to obtain the block-shaped lithium iron phosphate electrode.
1) Adding 3g of ethyl aluminum into a mixed organic solvent of 20ml of benzene and 80ml of tetrahydrofuran, uniformly stirring to obtain a deposition solution, then using press-formed blocky lithium iron phosphate as a working electrode, a platinum wire as a counter electrode, saturated calomel as a reference electrode, and then adopting a cyclic voltammetry (voltage range-2V-2V, sweeping rate: 5 mV/s) is deposited on the working electrode for 20min, and then the lithium iron phosphate composite electrode A is obtained by adopting 0.1mol/L ethylene carbonate for cleaning and drying;
2) adding 3g of lithium hydroxide into 100ml of ethylene carbonate, uniformly stirring to obtain an organic solvent system, then taking a lithium iron phosphate composite electrode A as a working electrode, a platinum electrode as a counter electrode and saturated calomel as a reference electrode, and adopting a cyclic voltammetry (voltage range-2V-2V, scanning rate: 5 mV/s) is adopted to carry out electrodeposition of lithium salt on the surface of the working electrode, the deposition time is 20min, and after the completion, the lithium iron phosphate composite electrode B is obtained by adopting ethylene carbonate to wash and dry.
Example 2
The preparation method of the block-shaped lithium iron phosphate electrode comprises the following steps:
firstly, uniformly mixing 80g of lithium iron phosphate powder, 20g of polyvinylidene fluoride and 50ml of N-methyl pyrrolidone to obtain a sticky colloid, coating the sticky colloid on foamed aluminum, drying, performing compression molding under the pressure of 10Mpa by using a tablet press, and drying at the temperature of 80 ℃ to obtain the block-shaped lithium iron phosphate electrode.
1) Adding 1g of butyl aluminum into a mixed organic solvent of 10ml of benzene and 90ml of tetrahydrofuran, uniformly stirring to obtain a deposition solution, then depositing the deposition solution on a working electrode for 1min by using a constant pressure method (voltage is 2V) by using press-formed lithium iron phosphate as the working electrode, a platinum wire as a counter electrode and saturated calomel as a reference electrode, and then cleaning and drying by using 0.1mol/L of ethylene carbonate to obtain a lithium iron phosphate composite electrode A;
2) adding 1g of lithium carbonate into 100ml of ethylene carbonate, uniformly stirring to obtain an organic solvent system, then taking a lithium iron phosphate composite electrode A as a working electrode, a platinum electrode as a counter electrode and saturated calomel as a reference electrode, electrodepositing lithium salt on the surface of the working electrode by adopting a constant pressure method (voltage of 2V) for 1min, and after the deposition is finished, cleaning and drying by using ethylene carbonate to obtain a lithium iron phosphate composite electrode B.
Example 3
The preparation method of the block-shaped lithium iron phosphate electrode comprises the following steps:
firstly, uniformly mixing 95g of lithium iron phosphate powder, 5g of polyvinylidene fluoride and 100ml of N-methyl pyrrolidone to obtain a sticky colloid, coating the sticky colloid on foamed aluminum, drying, performing compression molding under the pressure of 10Mpa by using a tablet press, and drying at the temperature of 80 ℃ to obtain the block-shaped lithium iron phosphate electrode.
1) Adding 5g of aluminum acetate into a mixed organic solvent of 30ml of benzene and 70ml of tetrahydrofuran, uniformly stirring to obtain a deposition solution, then using press-formed lithium iron phosphate as a working electrode, a platinum wire as a counter electrode, saturated calomel as a reference electrode, and adopting a constant current method (1 mA/cm) on the deposition solution2) Depositing on the working electrode for 30min, and then cleaning and drying by adopting 0.1mol/L ethylene carbonate to obtain a lithium iron phosphate composite electrode A;
2) adding 5g of lithium metaaluminate into 100ml of ethylene carbonate, uniformly stirring to obtain an organic solvent system, then taking a lithium iron phosphate composite electrode A as a working electrode, a platinum electrode as a counter electrode and saturated calomel as a reference electrode, and adopting a constant current method (1 mA/cm)2) And (3) electrodepositing lithium salt on the surface of the working electrode for 30min, and then cleaning and drying by using ethylene carbonate to obtain the lithium iron phosphate composite electrode B.
Comparative example:
lithium iron phosphate purchased in the market was used as a comparative example (model: N1, manufacturer: Jiangsu Leneng batteries, Ltd.)
1) Manufacturing the button cell:
2.0000g of the positive electrode active material lithium iron phosphate electrode prepared in the examples 1-3 and the comparative example, 0.1111g of conductive carbon black and 0.1111g of PVDF are respectively weighed according to the mass ratio of 0.9: 0.05 and mixed, and then 2.5g of NMP (N-methyl pyrrolidone) as an organic solvent is added and fully and uniformly mixed. Coating a film with the thickness of 140 micrometers on an aluminum foil, drying the film for 2 hours at 120 ℃ in vacuum, beating the film into a wafer with the thickness of 5mm by using a puncher, tabletting the wafer by using a tabletting machine under the pressure of 10MPa, keeping the temperature for 12 hours at 120 ℃ in vacuum, and weighing the weight of the positive plate. The button cell is assembled in a glove box protected by argon, a metal lithium sheet is taken as a negative electrode, an electrolyte is EC (ethylene carbonate), DMC ((1, 2-dimethyl carbonate) solvent and electrolyte LiPF (lithium ion plasma) with the volume ratio of 1: 16And the diaphragm is a Celgard2400 microporous polyethylene film. The assembled cell was tested for electrical performance on a blue tester. The button cells A1, A2, A3 and B1 were prepared as shown in Table 1 by testing the specific capacity by charging/discharging at a constant current of 0.2C within a voltage range of 2.5V to 4.2V.
TABLE 1 comparison of test results of test for test of test and comparative test
As can be seen from table 1, the discharge capacity and the first efficiency of the lithium iron phosphate material prepared in the example are significantly higher than those of the comparative example, because the lithium salt is doped on the surface of the material in the example to provide the transmission rate of lithium ions in the charging and discharging processes, the first efficiency and gram capacity exertion of the material are improved; meanwhile, the material intermediate layer is coated with an aluminum material with high electronic conductivity, so that the conductivity of the material is improved.
2) Manufacturing a soft package battery:
the materials obtained in example 1, example 2, example 3 and comparative example were used as positive electrode materials, artificial graphite was used as negative electrode material, and LiPF was used62.5Ah cylindrical batteries C1, C2, C3 and D1 are prepared by using/EC + DEC (volume ratio of 1: 1) as an electrolyte and a Celgard2400 membrane as a diaphragm, and the rate performance of the materials is tested, wherein the charge rate is 0.3C, and the discharge rate is 0.3C, 0.5C, 1.0C, 5.0C, 10.0C and 20.0C.
TABLE 2 comparison of the discharge rates of the examples and comparative examples
As can be seen from table 2, the rate performance of the battery prepared from the example material is significantly better than that of the comparative example, because the surface of the example material is coated with a lithium salt substance, sufficient lithium ions are provided for the charging and discharging process, and the rate discharge performance of the battery in the charging and discharging process is improved.
Table 3 shows the rate cycles of the examples and pouch cells, where the parameters are: multiplying power charging and discharging is not 2.0C/2.0C, the voltage range is 2.5-4.2V, the temperature is 25 +/-3 ℃, the cycle times are 500 times, and the energy density of the battery is calculated at the same time.
TABLE 3 energy Density comparison of examples and comparative examples
As can be seen from table 3, the energy density of the batteries prepared in examples is significantly superior to that of the comparative examples because the example materials have higher specific capacities and their tap densities increase the energy density of the materials. Meanwhile, the lithium iron phosphate material has high density, strong structural stability and sufficient lithium ions, thereby improving the cycle performance of the lithium iron phosphate material.
Claims (5)
1. A preparation method of a lithium iron phosphate composite electrode is characterized by comprising the following steps:
(1) adding 1g to 5g of organic aluminum salt into a mixed organic solvent of 10ml to 30ml of benzene and 70ml to 90ml of tetrahydrofuran, uniformly stirring, then depositing on a working electrode for 1min to 30min by adopting an electrochemical deposition method by taking press-formed lithium iron phosphate as the working electrode, a platinum wire as a counter electrode and saturated calomel as a reference electrode, and then cleaning and drying to obtain a lithium iron phosphate composite electrode A;
(2) adding 1 g-5 g of lithium salt into 100ml of ethylene carbonate, uniformly stirring to obtain an organic solvent system, then taking a lithium iron phosphate composite electrode A as a working electrode, a platinum electrode as a counter electrode and saturated calomel as a reference electrode, electrodepositing the lithium salt on the surface of the working electrode by adopting an electrochemical method for 1 min-30 min, and after the deposition is finished, cleaning and drying by adopting the ethylene carbonate to obtain a lithium iron phosphate electrode B, namely the lithium iron phosphate composite electrode;
the preparation method of the molded lithium iron phosphate in the step (1) comprises the following steps: firstly, uniformly mixing 80-95 g of lithium iron phosphate powder, 5-20 g of polyvinylidene fluoride and 50-100 ml of N-methyl pyrrolidone to obtain a sticky colloid, then performing compression molding by a tablet press, and drying to obtain a block-shaped lithium iron phosphate electrode;
the aluminum salt in the step (1) is one of ethyl aluminum, butyl aluminum, aluminum acetate, aluminum formate, aluminum oxalate and aluminum propionate.
2. The method of claim 1, wherein the electrochemical deposition method in the steps (1) and (2) is one of cyclic voltammetry, constant pressure method, constant current method, and pulse method.
3. The method according to claim 1, wherein the lithium salt in the step (2) is one of lithium carbonate, lithium hydroxide, lithium metaaluminate, lithium perchlorate and lithium zirconate.
4. The lithium iron phosphate composite electrode prepared by the preparation method of any one of claims 1 to 3, which is characterized by comprising lithium iron phosphate and aluminum salt and lithium salt thereof deposited on the surface thereof, and the mass ratio of the lithium iron phosphate composite electrode to the aluminum salt is as follows: lithium iron phosphate: aluminum salt: the lithium salt is 100: 1-5: 1 to 5.
5. The application of the lithium iron phosphate composite electrode in a lithium iron phosphate composite electrode according to claim 4, wherein the lithium iron phosphate battery mainly comprises the lithium iron phosphate composite electrode, a graphite negative electrode material, a ceramic diaphragm and a functional electrolyte thereof.
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| CN103579623A (en) * | 2013-11-12 | 2014-02-12 | 上海冠旗电子新材料股份有限公司 | Preparation method of nano-level lithium iron phosphate electrode material |
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| CN101478039B (en) * | 2009-02-05 | 2011-05-04 | 上海交通大学 | Preparation for polypyrole coated lithium iron phosphate |
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| CN103579623A (en) * | 2013-11-12 | 2014-02-12 | 上海冠旗电子新材料股份有限公司 | Preparation method of nano-level lithium iron phosphate electrode material |
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