CN114583161A - Composite graphite negative electrode material and preparation method and application thereof - Google Patents
Composite graphite negative electrode material and preparation method and application thereof Download PDFInfo
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- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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Abstract
The invention provides a composite graphite cathode material and a preparation method and application thereof, wherein the composite graphite cathode material comprises a graphite core and a solid electrolyte coating layer arranged on the surface of the graphite core, and the thickness of the solid electrolyte coating layer is 20-120 nm. Compared with an alumina coating layer, the solid electrolyte coating layer has lower influence on the capacity of the graphite cathode, lower energy consumption and lower cost, and is easy to popularize on a large scale.
Description
Technical Field
The invention belongs to the field of lithium ion battery cathode materials, and relates to a composite graphite cathode material, and a preparation method and application thereof.
Background
Lithium ion batteries have become one of the most important energy storage devices in the present generation due to their important advantages of high energy density, high output voltage, long cycle life, no memory effect, low self-discharge rate, etc., and thus have received much attention. The graphite cathode has the characteristics of low cost, convenient processing, low lithium intercalation potential, no pollution and the like, and is widely used as a cathode material of a lithium ion battery.
The graphite negative electrode and the SEI film formed by the graphite negative electrode have the characteristics of easy reaction and easy decomposition with electrolyte at a lower temperature. Coating aluminum oxide on the surface of graphite is a relatively common method, but aluminum oxide is an inert material and can bring great influence on the electrochemical performance of the electrode. Therefore, on the premise of not greatly reducing the electrochemical performance of the material, the coating of the graphite cathode material can improve the overall thermal stability of the material and reduce the electronic conductivity, so that the improvement of the safety performance of the lithium ion battery has great research significance.
The solid electrolyte is an ion conductor which can provide a path for lithium ion transmission, is a non-inert material per se, and has better thermal stability. The lithium ion battery cathode material solves the safety problems that in the prior art, graphite cathode materials are poor in thermal stability, the contact resistance of a cathode pole piece in a lithium ion battery is small, and the lithium ion battery adopting the graphite cathode materials is easy to catch fire or explode when short circuit or hard object puncture occurs.
CN108134060A discloses a composite material of a solid electrolyte interface film coated negative electrode material, a preparation method and application thereof. A layer of compact and uniformly coated SEI film is prepared on the surface of a negative electrode material by a solid-phase film forming method, a liquid-phase film forming method or a chemical film forming method, the negative electrode material coated by the SEI film has higher structural stability and thermal stability, and a lithium ion battery taking the material as a negative electrode shows excellent cycling stability.
CN113540416A discloses a solid electrolyte coated graphite composite material, a preparation method and an application thereof, and a lithium ion battery, wherein an intermediate layer containing a solid electrolyte is disposed between a graphite core and a carbon layer, because the solid electrolyte is of a cubic structure, and has many lithium ion insertion and extraction channels and a stable structure, the method can effectively improve safety and reduce capacity loss, but has high cost, high energy consumption, and is not easy to popularize.
The graphite composite material provided by the scheme has the problems of poor safety or high cost, so that the development of the rechecked graphite cathode material with good safety, low cost and good stability is necessary.
Disclosure of Invention
The invention aims to provide a composite graphite negative electrode material and a preparation method and application thereof. Compared with an alumina coating layer, the solid electrolyte coating layer has lower influence on the capacity of the graphite cathode, lower energy consumption and lower cost, and is easy for large-scale popularization.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a composite graphite anode material, including a graphite core and a solid electrolyte coating layer disposed on a surface of the graphite core, where a thickness of the solid electrolyte coating layer is 20-120 nm, for example: 20nm, 40nm, 60nm, 80nm, 100nm or 120nm, etc.
In the composite graphite cathode material, the solid electrolyte coating layer is introduced, so that the side reaction between the electrolyte and graphite can be effectively inhibited, and the thermal runaway risk caused by the terminal conditions such as short circuit of a battery can be prevented. Compared with an alumina coating layer, the solid electrolyte coating layer has lower influence on the capacity of the graphite cathode, lower energy consumption and lower cost, and is easy for large-scale popularization.
Preferably, the specific surface area of the composite graphite negative electrode material is 1.54-2 m2G, for example: 1.54m2/g、1.56m2/g、1.6m2/g、1.8m2In g or 2m2And/g, etc.
Preferably, the graphite core size of the composite graphite negative electrode material is 10-20 nm, for example: 10nm, 12nm, 15nm, 18nm or 20nm, etc.
Preferably, the conductivity of the composite graphite negative electrode material is 5.3-6.4S/cm, for example: 5.3S/cm, 5.5S/cm, 5.8S/cm, 6S/cm, 6.2S/cm, 6.4S/cm, or the like.
In a second aspect, the present invention provides a method for preparing the composite graphite anode material according to the first aspect, wherein the method comprises the following steps:
(1) mixing graphite with a solvent to obtain a graphite dispersion liquid;
(2) mixing the graphite dispersion liquid obtained in the step (1) with a lithium source, an aluminum source, a phosphorus source and a transition metal source to obtain a mixed solution, evaporating the solvent to dryness, and sintering to obtain the composite graphite cathode material;
wherein, the transition metal source in the step (2) comprises tetrabutyl titanate and/or tetrabutyl germanate.
The method adopted by the solid electrolyte coated graphite cathode material prepared by the invention is an in-situ synthesis method, the graphite cathode material with the surface coated with the solid electrolyte is prepared by the in-situ synthesis method, in the preparation process, the reaction occurs at the molecular level, the reaction condition is mild, the solid electrolyte is uniformly distributed on the surface of the graphite core in the prepared composite graphite cathode material, the thickness of the solid electrolyte layer can be accurately controlled by controlling the concentration of various reactants and the reaction condition, and further the specific surface area, the conductivity and the capacity loss of the material are regulated and controlled.
Preferably, the solvent of step (1) comprises ethanol and/or NMP.
Preferably, the mass concentration of graphite in the graphite dispersion liquid in the step (1) is 20-80 wt%, for example: 20 wt%, 30 wt%, 40 wt%, 50 wt%, 60 wt%, 70 wt%, or 80 wt%, etc.
Preferably, the lithium source of step (2) comprises lithium acetate and/or lithium nitrate.
Preferably, the aluminum source comprises aluminum nitrate.
Preferably, the source of phosphorus comprises ammonium dihydrogen phosphate.
Preferably, the mass ratio of the graphite dispersion liquid, the lithium source, the aluminum source, the phosphorus source and the transition metal source in the step (2) is 200 (0.4-1.4): (0.4-1.5): (0.9-3.5): 1.4-5.4), for example: 200:0.4:0.4:0.9:1.4, 200:0.6:0.8:2:3, 200:1:1:2.4:4, 200:1.2:1.3:2.5:4, or 200:1.4:1.5:3.5:5.4, etc.
Preferably, the pH of the mixed solution is 2-7, such as: 2. 3, 4, 5, 6, or 7, etc.
Preferably, the temperature of the sintering treatment in the step (2) is 800-1000 ℃, for example: 800 deg.C, 850 deg.C, 900 deg.C, 950 deg.C or 1000 deg.C.
Preferably, the time of the sintering treatment is 2-4 h, for example: 2h, 2.5h, 3h, 3.5h or 4h and the like.
In a third aspect, the invention provides a negative electrode plate, which comprises the composite graphite negative electrode material according to the first aspect.
In a fourth aspect, the invention provides a lithium ion battery, which comprises the negative electrode plate according to the third aspect.
Compared with the prior art, the invention has the following beneficial effects:
(1) the solid electrolyte coating layer is introduced through the in-situ synthesis method, so that the side reaction between the electrolyte and the graphite can be effectively inhibited, and the thermal runaway risk caused by the terminal conditions such as battery short circuit and the like can be prevented. Compared with an alumina coating layer, the solid electrolyte coating layer has lower influence on the capacity of the graphite cathode, lower energy consumption and lower cost, and is easy for large-scale popularization.
(2) The invention introduces the solid electrolyte coating layer on the graphite surface by the in-situ synthesis method, increases the specific surface area of the graphite material, and correspondingly accelerates the wettability of the graphite and the electrolyte and the electrochemical reaction kinetics of the material. However, the solid electrolyte itself does not provide capacity, but is a good conductor of lithium ions, and can reduce capacity loss.
Drawings
Fig. 1 is an SEM image of the composite graphite anode material according to example 1 of the present invention.
Fig. 2 is a high-magnification SEM image of the composite graphite anode material according to example 1 of the present invention.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides a composite graphite anode material, and a preparation method of the composite graphite anode material comprises the following steps:
(1) mixing graphite and ethanol to obtain 33 wt% graphite ethanol dispersion liquid;
(2) and (2) mixing the ethanol dispersion liquid of the graphite obtained in the step (1) with 0.357 parts by mass of lithium acetate, 0.375 parts by mass of aluminum nitrate, 0.863 parts by mass of ammonium dihydrogen phosphate and 1.36 parts by mass of tetrabutyl titanate, evaporating the solvent to dryness, and sintering at 800 ℃ for 2 hours to obtain the composite graphite cathode material.
The SEM image of the composite graphite negative electrode material is shown in figures 1-2.
Example 2
The embodiment provides a composite graphite anode material, and a preparation method of the composite graphite anode material comprises the following steps:
(1) mixing graphite and ethanol to obtain a graphite ethanol dispersion liquid with the mass concentration of 56 wt%;
(2) and (2) mixing the ethanol dispersion of the graphite obtained in the step (1) with 0.714 mass part of lithium acetate, 0.75 mass part of aluminum nitrate, 1.73 mass parts of ammonium dihydrogen phosphate and 2.72 mass parts of tetrabutyl germanate, evaporating the solvent to dryness, and sintering at 900 ℃ for 3 hours to obtain the composite graphite negative electrode material.
Example 3
The embodiment provides a composite graphite anode material, and a preparation method of the composite graphite anode material comprises the following steps:
(1) mixing graphite and ethanol to obtain a graphite ethanol dispersion liquid with the mass concentration of 45 wt%;
(2) and (2) mixing the ethanol dispersion of the graphite obtained in the step (1) with 1.43 parts by mass of lithium acetate, 1.5 parts by mass of aluminum nitrate, 3.45 parts by mass of ammonium dihydrogen phosphate and 5.44 parts by mass of tetrabutyl titanate, evaporating the solvent to dryness, and sintering at 1000 ℃ for 4 hours to obtain the composite graphite negative electrode material.
Example 4
This example differs from example 1 only in that the sintering temperature in step (2) is 700 ℃, and other conditions and parameters are exactly the same as those in example 1.
Example 5
This example is different from example 1 only in that the sintering temperature in step (2) is 1100 ℃, and other conditions and parameters are exactly the same as those in example 1.
Comparative example 1
This comparative example uses only graphite.
Comparative example 2
This comparative example differs from example 1 only in that a conventional solid phase coating method is employed, and other conditions and parameters are exactly the same as those of example 1.
And (3) performance testing:
the composite graphite negative electrode materials obtained in the examples 1 to 5 and the comparative examples 1 to 2, acetylene black, SBR and CMC were mixed with solvent water in a mass ratio of 93:2:3:2, stirred uniformly, and the slurry was coated on an aluminum foil with a thickness of 200 micrometers by a doctor blade and a thickness of 8 micrometers, and was dried in a vacuum drying oven at 110 ℃ for 24 hours to test the first effect and the capacity, and the test results are shown in Table 1:
TABLE 1
As can be seen from Table 1, the following examplesThe specific surface area of the composite graphite negative electrode material can reach 1.54m as obtained in examples 1-52More than g, the capacity of 0.1C gram can reach more than 345mAh/g, the grain size can reach less than 18nm, the thickness of the coating layer can reach less than 110nm, meanwhile, the conductivity can reach more than 5.35S/cm, the thickness of the coating layer is correspondingly increased along with the increase of the coating amount, the coating layer is thicker, but the conductivity is lower, and the composite graphite cathode material can achieve both the coating effect and the conductivity.
Compared with the embodiment 1 and the embodiment 4-5, the sintering temperature can influence the performance of the prepared composite graphite cathode material, the sintering temperature is controlled to be 800-1000 ℃, the performance of the prepared composite graphite cathode material is good, and AlPO is easily generated if the sintering temperature is too high4、TiO2And if the sintering temperature is too low, the LATP synthesis reaction is incomplete, and the generated impurities have great influence on the graphite capacity.
Compared with the comparative example 1, the composite graphite cathode material of the invention has the advantages that the introduction of the solid electrolyte coating layer can effectively inhibit the side reaction between the electrolyte and the graphite, and prevent the thermal runaway risk caused by the terminal conditions such as battery short circuit. Compared with an alumina coating layer, the solid electrolyte coating layer has lower influence on the capacity of the graphite cathode, lower energy consumption and lower cost, and is easy for large-scale popularization.
Compared with the comparative example 2, the graphite cathode material with the surface coated with the solid electrolyte is prepared by adopting an in-situ synthesis method, the reaction occurs at a molecular level in the preparation process, the reaction conditions are mild, the solid electrolyte is uniformly distributed on the surface of the graphite core in the prepared composite graphite cathode material, the thickness of the solid electrolyte layer can be accurately controlled by controlling the concentration of various reactants and the reaction conditions, and the specific surface area, the conductivity and the capacity loss of the material are further regulated and controlled.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention disclosed herein fall within the scope and disclosure of the present invention.
Claims (10)
1. The composite graphite cathode material is characterized by comprising a graphite core and a solid electrolyte coating layer arranged on the surface of the graphite core, wherein the thickness of the solid electrolyte coating layer is 20-120 nm.
2. The composite graphite anode material of claim 1, wherein the specific surface area of the composite graphite anode material is 1.54-2 m2/g。
3. The composite graphite anode material according to claim 1 or 2, wherein a graphite core size of the composite graphite anode material is 10 to 20 nm.
4. The composite graphite anode material according to any one of claims 1 to 3, wherein the electrical conductivity of the composite graphite anode material is 5.3 to 6.4S/cm.
5. A method for preparing the composite graphite anode material as claimed in any one of claims 1 to 4, characterized by comprising the steps of:
(1) mixing graphite with a solvent to obtain a graphite dispersion liquid;
(2) mixing the graphite dispersion liquid obtained in the step (1) with a lithium source, an aluminum source, a phosphorus source and a transition metal source to obtain a mixed solution, evaporating the solvent to dryness, and sintering to obtain the composite graphite cathode material;
wherein, the transition metal source in the step (2) comprises tetrabutyl titanate and/or tetrabutyl germanate.
6. The method of claim 5, wherein the solvent of step (1) comprises ethanol;
preferably, the mass concentration of graphite in the graphite dispersion liquid is 20-80 wt%.
7. The method according to claim 5 or 6, wherein the lithium source of step (2) comprises lithium acetate and/or lithium nitrate;
preferably, the aluminum source comprises aluminum nitrate;
preferably, the source of phosphorus comprises ammonium dihydrogen phosphate;
preferably, the mass ratio of the graphite dispersion liquid to the lithium source to the aluminum source to the phosphorus source to the transition metal source is 200 (0.4-1.4): (0.4-1.5): (0.9-3.5): 1.4-5.4);
preferably, the pH of the mixed solution is 2-7.
8. The method according to any one of claims 5 to 7, wherein the temperature of the sintering treatment in the step (2) is 800 to 1000 ℃;
preferably, the time of the sintering treatment is 2-4 h.
9. A negative electrode tab, characterized in that it comprises the composite graphite negative electrode material of claim 1.
10. A lithium ion battery comprising the negative electrode tab of claim 9.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115966692A (en) * | 2023-01-19 | 2023-04-14 | 重庆长安新能源汽车科技有限公司 | High-load lithium battery negative electrode material, preparation method and application |
| CN116053481A (en) * | 2023-03-31 | 2023-05-02 | 中创新航技术研究院(江苏)有限公司 | Graphite composite material, battery cathode using same and battery |
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| CN115966692A (en) * | 2023-01-19 | 2023-04-14 | 重庆长安新能源汽车科技有限公司 | High-load lithium battery negative electrode material, preparation method and application |
| CN116053481A (en) * | 2023-03-31 | 2023-05-02 | 中创新航技术研究院(江苏)有限公司 | Graphite composite material, battery cathode using same and battery |
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