CN112563472A - Polymer composite lithium iron phosphate anode material and preparation method thereof - Google Patents
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Abstract
The invention relates to a polymer composite lithium iron phosphate anode material and a preparation method thereof, belongs to the field of lithium ion battery anode materials, and aims to solve the technical problems of large impedance, low capacity, poor circulation and the like caused by poor wettability of the surface of lithium iron phosphate particles and an electrolyte. The polymer composite lithium iron phosphate material comprises a lithium iron phosphate-carbon composite material and a polymer coated on the surface of the lithium iron phosphate-carbon composite material, wherein the lithium iron phosphate-carbon composite material comprises a carbon-coated lithium iron phosphate composite material LixFeyMzPO4Wherein x is more than or equal to 0.7 and less than or equal to 1.3, y is more than or equal to 0.7 and less than or equal to 1.3, z is more than or equal to 0 and less than or equal to 0.3, and M is selected from at least one of Mg, Ti, Zr, Cr, Al, Si, B and Mn. Polymers of the inventionThe composite lithium iron phosphate material has the characteristics of good electrolyte wettability, high specific capacity, excellent cycle and the like, and has a wide application prospect.
Description
Technical Field
The invention relates to the field of lithium ion battery anode materials, in particular to a polymer composite lithium iron phosphate anode material and a preparation method thereof.
Background
Lithium iron phosphate is one of the main anode materials, and has been widely researched in the field of new energy devices. At present, lithium iron phosphate is already applied in the field of electric automobiles on a large scale. The lithium iron phosphate lithium ion battery is taken as an important energy storage device in the field of new energy transportation, and is widely popularized on new energy automobiles by virtue of higher energy density and power density and excellent safety performance, so that the lithium iron phosphate lithium ion battery becomes one of core components of the new energy electric automobiles.
In recent years, research has been conducted to improve the performance of a pole piece mainly by adding a polymer in the process of preparing lithium iron phosphate slurry so as to improve the conductivity and the electronic conductivity of lithium ion, for example, in a patent "preparation method of a lithium ion battery with a conductive polymer coated positive electrode" (application number 201110185785.0), it is shown that the specific capacity of the battery is improved by 10-20% by adding a conductive polymer or a conductive polymer monomer in the positive electrode slurry for coating. Although the process improves the conductivity and specific capacity of the lithium iron phosphate, the polymer is added in the process of preparing the electrode slurry, so that the lithium iron phosphate particles are not sufficiently coated, the lithium iron phosphate particles are not sufficiently soaked in the electrolyte, more polymers are used, and the cost is very high.
Therefore, it is necessary to develop a method capable of sufficiently coating lithium iron phosphate particles to improve wettability to an electrolyte and reduce the cost.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a polymer composite lithium iron phosphate anode material and a preparation method thereof.
The invention aims to provide a polymer composite lithium iron phosphate material, which comprises a lithium iron phosphate-carbon composite material and a polymer coated on the surface of the lithium iron phosphate-carbon composite material, wherein the lithium iron phosphate-carbon composite material comprises a carbon-coated lithium iron phosphate composite material LixFeyMzPO4Wherein x is more than or equal to 0.7 and less than or equal to 1.3, y is more than or equal to 0.7 and less than or equal to 1.3, z is more than or equal to 0 and less than or equal to 0.3, and M is selected from at least one of Mg, Ti, Zr, Cr, Al, Si, B and Mn.
Further, in the lithium iron phosphate-carbon composite material, carbon accounts for 0.5-10% of the mass fraction of the lithium iron phosphate-carbon composite material.
Further, the polymer is selected from at least one of polyacetylene, polypyrrole and polyaniline.
Further, the polymer accounts for 0.1-5% of the mass fraction of the lithium iron phosphate-carbon composite material.
Further, the preparation method of the polymer composite lithium iron phosphate material comprises the following steps:
(1) when z is 0, uniformly mixing an iron source, a phosphorus source, a lithium source and a carbon source, when z is more than 0 and less than or equal to 0.3, uniformly mixing the iron source, the phosphorus source, the lithium source, the carbon source and a substance containing an M element, drying the obtained mixed substance, and then sintering at high temperature in an inert or reducing atmosphere to obtain the lithium iron phosphate-carbon composite material; the high-temperature sintering temperature is 600-800 ℃;
(2) and uniformly mixing the lithium iron phosphate-carbon composite material and the polymer in a solvent, and drying to obtain the polymer composite lithium iron phosphate material.
The M element is used as a doping element and can be added according to requirements when the lithium iron phosphate-carbon composite material is prepared.
Further, in the steps (1) and (2), the materials are uniformly mixed by adopting a mechanical grinding method.
Further, in the step (1), the mechanical grinding time is 1-24 h.
Further, in the step (1), after the high-temperature sintering, the step of grinding the product is also included, and the grinding time is 1-24 h.
Further, in the step (1), among the lithium source, the iron source, and the phosphorus source, Li: fe: atomic ratio of P ═ (0.7 to 1.3): (0.7-1.3):1.
Further, in the step (1), the carbon source is at least one of sucrose, glucose, fructose and starch.
Further, in the step (1), the iron source is at least one of iron, ferric sulfate, ferrous sulfate, ferric chloride, ferrous chloride and ferric phosphate; the phosphorus source is at least one of phosphoric acid, ammonium phosphate and ammonium hydrogen phosphate, and the lithium source is at least one of lithium hydroxide, lithium sulfate and lithium carbonate.
Further, in step (1), the inert or reducing atmosphere is N2、Ar、CO、CO2、H2At least one of (1).
Further, in the step (1), the sintering time is 1-72 h.
Further, in the step (2), the polymer accounts for 0.1-5% of the mass fraction of the lithium iron phosphate-carbon composite material.
Further, in the step (2), the solvent is at least one of ethanol, acetone, methanol and water.
Further, in the step (2), the grinding time is 1-24 h.
The second purpose of the invention is to disclose the application of the polymer composite lithium iron phosphate material as the anode material of the lithium ion battery.
The invention also discloses a lithium ion battery anode which comprises the polymer composite lithium iron phosphate material.
The invention further discloses a lithium ion battery which comprises the lithium ion battery anode.
By the scheme, the invention at least has the following advantages:
the invention provides a polymer composite lithium iron phosphate material, which is characterized in that a polymer is used for coating a lithium iron phosphate-carbon composite material, so that the surface characteristics of lithium iron phosphate particles and the wettability to an electrolyte are improved, the conductivity is improved, and the lithium iron phosphate has good electrochemical performance.
The polymer composite lithium iron phosphate material has the characteristics of simple preparation process, good electrolyte wettability, high specific capacity, excellent cycle and the like, and has wide application prospect.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following description is made with reference to the preferred embodiments of the present invention and the accompanying detailed drawings.
Drawings
FIG. 1 is an SEM image of a polymer composite lithium iron phosphate powder prepared in example 1;
fig. 2 is the discharge capacity retention ratio and voltage plateau at 2C for a button cell assembled from the positive electrode material in comparative example 1 and examples 1 and 4;
fig. 3 shows the discharge capacity retention ratio and voltage plateau at 3C for the button cell assembled with the positive electrode material in comparative example 1 and examples 1 and 4.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Comparative example 1
(1) According to the atomic ratio of Li: fe: p is 1: 1: 1, taking 55.6g of FeSO4·7H2O, 23.1g of 83% by mass of H3PO4Solution, 7.4g of Li2CO30.8g of glucose was ground in deionized water for 2h until mixed well.
(2) And transferring the mixed solution to a drying oven for full drying, and then transferring to a high-temperature furnace under the nitrogen protection atmosphere, wherein the sintering time is 24h at 700 ℃.
(3) Grinding the sintered sample to obtain carbon-coated lithium iron phosphate LiFePO4Powder material (0.2mol, 31.6 g).
Example 1
(1) According to the atomic ratio of Li: fe: p is 1: 1: 1, taking 55.6g of FeSO4·7H2O, 23.1g substanceAn amount fraction of 83% of H3PO4Solution, 7.4g of Li2CO30.8g of glucose was ground in deionized water for 2h until mixed well.
(2) Transferring the mixed solution to a drying oven for full drying, then transferring to a high-temperature furnace in a nitrogen protective atmosphere, sintering at 700 ℃ for 24h, wherein the sintered sample is carbon-coated lithium iron phosphate LiFePO4(0.2mol，31.6g)。
(3) And grinding the sintered sample and 0.3g of polyaniline in ethanol for 1 hour, and drying to obtain the polymer composite lithium iron phosphate material.
Example 2
(1) According to the atomic ratio of Li: fe: p is 1: 1: 1, taking 55.6g of FeSO4·7H2O, 23.1g of 83% by mass of H3PO4Solution, 7.4g of Li2CO30.8g of glucose was ground in deionized water for 2h until mixed well.
(2) Transferring the mixed solution to a drying oven for full drying, then transferring to a high-temperature furnace in a nitrogen protective atmosphere, sintering at 700 ℃ for 24h, wherein the sintered sample is carbon-coated lithium iron phosphate LiFePO4(0.2mol，31.6g)。
(3) And grinding the sintered sample and 0.6g of polyaniline in ethanol for 1 hour, and drying to obtain the polymer composite lithium iron phosphate material.
Example 3
(1) According to the atomic ratio of Li: fe: p is 1: 1: 1, taking 55.6g of FeSO4·7H2O, 23.1g of 83% by mass of H3PO4Solution, 7.4g of Li2CO30.8g of glucose was ground in deionized water for 2h until mixed well.
(2) Transferring the mixed solution to a drying oven for full drying, then transferring to a high-temperature furnace in a nitrogen protective atmosphere, sintering at 700 ℃ for 24h, wherein the sintered sample is carbon-coated lithium iron phosphate LiFePO4(0.2mol，31.6g)。
(3) And grinding the sintered sample and 0.9g of polyaniline in ethanol for 1 hour, and drying to obtain the polymer composite lithium iron phosphate material.
Example 4
(1) According to the atomic ratio of Li: fe: p is 1: 1: 1, taking 55.6g of FeSO4·7H2O, 23.1g of 83% by mass of H3PO4Solution, 7.4g of Li2CO30.8g of glucose was ground in deionized water for 2h until mixed well.
(2) Transferring the mixed solution to a drying oven for full drying, then transferring to a high-temperature furnace in a nitrogen protective atmosphere, sintering at 700 ℃ for 24h, wherein the sintered sample is carbon-coated lithium iron phosphate LiFePO4(0.2mol，31.6g)。
(3) And grinding the sintered sample and 0.3g of polyacetylene in ethanol for 1 hour, and drying to obtain the polymer composite lithium iron phosphate material.
Example 5
(1) According to the atomic ratio of Li: fe: p is 1: 1: 1, taking 55.6g of FeSO4·7H2O, 23.1g of 83% by mass of H3PO4Solution, 7.4g of Li2CO30.8g of glucose was ground in deionized water for 2h until mixed well.
(2) Transferring the mixed solution to a drying oven for full drying, then transferring to a high-temperature furnace in a nitrogen protective atmosphere, sintering at 700 ℃ for 24h, wherein the sintered sample is carbon-coated lithium iron phosphate LiFePO4(0.2mol，31.6g)。
(3) And grinding the sintered sample and 0.3g of polypyrrole in ethanol for 1 hour, and drying to obtain the polymer composite lithium iron phosphate material.
The positive electrode materials prepared in examples 1 and 4 and comparative example 1 were mixed with conductive carbon black and binder PVDF in a mass ratio of 80: 10: after uniformly mixing the materials according to the proportion of 10, adding a proper amount of 1-methyl-2-pyrrolidone, then carrying out ball milling for 2 hours to prepare anode slurry, uniformly coating the anode slurry on an aluminum sheet, drying and tabletting to prepare an anode sheet. Then, a 2032 button cell is assembled by taking the lithium metal as the cathode. The electrolyte of the battery comprises the following components: EC/EMC 30/70 (v/v); LiPF6，1M；VC，2wt％。
And (4) carrying out charge and discharge tests on the button cell. The capacity retention rates of the button cells assembled by the positive electrode materials in examples 1-5 in the cycle of 100 weeks are all 100%, the capacity retention rates of the button cells assembled by the positive electrode materials in comparative example 1 in the cycle of 100 weeks are 95%, and compared with the capacity retention rates of the button cells assembled by the positive electrode materials in comparative example 1, the capacity retention rates of the button cells assembled by the positive electrode materials in the examples are excellent in cycle performance, and the service life of the cells can be greatly prolonged.
Table 1 shows the results of the electrolyte infiltration time tests of the positive electrode materials prepared in the examples and comparative examples at room temperature, and it can be seen that the polymer composite lithium iron phosphate material prepared in the present invention has better electrolyte infiltration performance and faster infiltration speed, and can greatly save the time cost for battery assembly.
TABLE 1 electrolyte wetting time
| Serial number | Comparative example 1 | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 |
| Average infiltration time(s) | 115 | 110 | 98 | 95 | 105 | 109 |
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, it should be noted that, for those skilled in the art, many modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A polymer composite lithium iron phosphate material is characterized in that: the lithium iron phosphate-carbon composite material comprises a carbon-coated lithium iron phosphate composite material LixFeyMzPO4Wherein x is more than or equal to 0.7 and less than or equal to 1.3, y is more than or equal to 0.7 and less than or equal to 1.3, z is more than or equal to 0 and less than or equal to 0.3, and M is selected from at least one of Mg, Ti, Zr, Cr, Al, Si, B and Mn.
2. The polymer composite lithium iron phosphate material of claim 1, wherein: in the lithium iron phosphate-carbon composite material, carbon accounts for 0.5-10% of the mass fraction of the lithium iron phosphate-carbon composite material.
3. The polymer composite lithium iron phosphate material of claim 1, wherein: the polymer is selected from at least one of polyacetylene, polypyrrole and polyaniline.
4. The polymer composite lithium iron phosphate material of claim 1, wherein: the polymer accounts for 0.1-5% of the mass fraction of the lithium iron phosphate-carbon composite material.
5. The polymer composite lithium iron phosphate material according to any one of claims 1 to 4, wherein the preparation method comprises the following steps:
(1) when z is 0, uniformly mixing an iron source, a phosphorus source, a lithium source and a carbon source, when z is more than 0 and less than or equal to 0.3, uniformly mixing the iron source, the phosphorus source, the lithium source, the carbon source and a substance containing an M element, drying the obtained mixed substance, and then sintering at high temperature in an inert or reducing atmosphere to obtain the lithium iron phosphate-carbon composite material; the high-temperature sintering temperature is 600-800 ℃;
(2) and uniformly mixing the lithium iron phosphate-carbon composite material and a polymer in a solvent, and drying to obtain the polymer composite lithium iron phosphate material.
6. The polymer composite lithium iron phosphate material of claim 5, wherein: in the step (1), the carbon source is at least one of sucrose, glucose, fructose and starch.
7. The polymer composite lithium iron phosphate material of claim 5, wherein: in the step (1), the iron source is at least one of iron, ferric sulfate, ferrous sulfate, ferric chloride, ferrous chloride and ferric phosphate; the phosphorus source is at least one of phosphoric acid, ammonium phosphate and ammonium hydrogen phosphate, and the lithium source is at least one of lithium hydroxide, lithium sulfate and lithium carbonate.
8. The use of the polymer composite lithium iron phosphate material of any one of claims 1 to 4 as a positive electrode material for a lithium ion battery.
9. A positive electrode of a lithium ion battery, comprising the polymer composite lithium iron phosphate material according to any one of claims 1 to 4.
10. A lithium ion battery comprising the lithium ion battery positive electrode according to claim 9.
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Cited By (2)
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| CN114784249A (en) * | 2022-04-29 | 2022-07-22 | 楚能新能源股份有限公司 | Lithium iron phosphate composite positive electrode material and preparation method thereof |
| WO2024036911A1 (en) * | 2022-08-19 | 2024-02-22 | 广东邦普循环科技有限公司 | Easy-to-process lithium iron phosphate composite material and prepartion method therefor |
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