CN108232175B - Graphite/lithium titanate composite negative electrode material for lithium ion battery and preparation method - Google Patents
Graphite/lithium titanate composite negative electrode material for lithium ion battery and preparation method Download PDFInfo
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Abstract
The invention provides a graphite/lithium titanate composite negative electrode material for a lithium ion battery and a preparation method thereof, wherein the graphite/lithium titanate negative electrode material is a composite material which takes a graphite material as a core and takes lithium titanate and an organic cracking carbon coating layer as a shell structure and is formed by forming lithium titanate and an organic cracking carbon coating layer on the surfaces of graphite material particles; the preparation method comprises the following steps: (1) mixing a graphite material, lithium titanate and an organic cracking carbon source according to the weight ratio of 100: 1-10: adding 1-5 mass percent of the mixture into an inorganic solvent or an organic solvent, mixing and drying; (2) heating the obtained composite material to 600-1050 ℃ at the speed of 1-20 ℃/min under the protection of inert gas atmosphere for sintering, and preserving heat for 1-10h to obtain the composite material; the graphite/lithium titanate composite negative electrode material can effectively improve the safety, rate capability, cycle performance and high and low temperature performance of graphite negative electrode materials, and meanwhile, the preparation method has the advantages of simple and controllable process, low cost and easiness in batch industrial production.
Description
Technical Field
The invention relates to the field of lithium ion battery cathode materials, in particular to a graphite/lithium titanate composite cathode material for a lithium ion battery and a preparation method thereof.
Background
The carbonaceous material has the advantages of low lithium intercalation potential, good cycle performance, relatively low price, environmental friendliness and the like, and is widely applied to the negative electrode material of the lithium ion battery. The graphite material is a mainstream negative electrode material at present due to the outstanding advantages in the aspects of reversible discharge specific capacity, first charge and discharge efficiency, voltage platform, manufacturing cost and the like, and is also an important candidate for a lithium ion battery negative electrode material in a future period. However, the graphite material has the characteristics of low lithium intercalation potential and easy formation of an SEI film with an electrolyte on the surface, so that the graphite material is deficient in safety and rate capability. Thus, modification treatment of graphite-based materials is required to improve their electrochemical properties.
The lithium titanate material has a higher discharge platform, a higher ion diffusion coefficient, extremely low volume expansion, an ultra-long cycle life and good low-temperature charge and discharge performance, so that the lithium ion battery adopting the lithium titanate material as the negative electrode material has higher safety, multiplying power and a wider service temperature range, thereby occupying a place in the negative electrode material of the lithium ion battery. However, the lithium titanate material has low energy density due to the lower theoretical specific capacity (175 mAh/g) and the higher lithium intercalation potential (1.5V), and the application field of the lithium titanate material is greatly limited. The graphite material is modified by using the lithium titanate material, so that the graphite material has good safety and rate capability, and is a good modification way.
At present, the modification of graphite materials by using lithium titanate materials has been reported. The domestic invention patent of application number 201210124713.X discloses a lithium titanate-coated modified graphite composite anode material and a preparation method and application thereof; the domestic invention patent of application No. 201410344991.5 discloses a lithium titanate-coated graphite cathode material with surface treatment, a preparation method and an application thereof, the cathode material forms a lithium titanate coating layer on the surface of graphite base cathode material particles with surface treatment so as to overcome the safety problems of lithium precipitation and the like in the application of the graphite cathode material, overcome the defect that the existing graphite cathode material and a battery system are unmatched when used at an over-high temperature or an over-low temperature, and improve the problems of lithium titanate particle agglomeration caused by the existing modification or modification method, uneven coating caused by anisotropy on the surface of the graphite particles and the like; the domestic invention patent with the application number of 201710178160.9 discloses a preparation method of a lithium titanate graphite composite negative electrode material, which distributes lithium titanate in a three-dimensional conductive network formed by graphite through means of mechanical mixing, isostatic pressing fusion, crushing spheroidization, high-temperature sintering and the like. However, in the former two methods, a more complex sol-gel process is used for preparing the lithium titanate material and compounding the lithium titanate material with the graphite material, so that uniform coating of the lithium titanate material on the surface of the graphite material is difficult to realize, and the operation difficulty is high in industrial mass production, which is not favorable for large-scale production; in the latter method, the lithium titanate material is placed inside the composite material structure, and the characteristics of lithium titanate cannot be fully utilized to effectively modify the graphite material.
Disclosure of Invention
Aiming at the prior technical problems, the invention provides a graphite/lithium titanate composite negative electrode material for a lithium ion battery and a preparation method thereof, wherein the graphite/lithium titanate composite negative electrode material can effectively improve the safety, rate capability, cycle performance and high and low temperature performance of graphite negative electrode materials, and meanwhile, the preparation method has the advantages of simple and controllable process, low cost and easy batch industrial production.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a graphite/lithium titanate composite negative electrode material for a lithium ion battery is characterized in that lithium titanate and an organic cracking carbon coating layer are formed on the surface of graphite material particles to form a graphite/lithium titanate composite material which takes the graphite material as a core and takes the lithium titanate and the organic cracking carbon coating layer as a shell structure;
the raw materials for preparing the graphite/lithium titanate composite negative electrode material comprise a graphite material, lithium titanate and an organic cracking carbon source; the mass ratio of the graphite material to the lithium titanate to the organic cracking carbon source is 100: 1-10: 1-5.
Preferably, the graphite material is one or a mixture of at least two of natural graphite, artificial graphite, mesocarbon microbeads and soft carbon, the particle size of the graphite material is 5-30 mu m, and the purity of the graphite material is more than or equal to 99%.
Preferably, the lithium titanate has the particle size of 10-500nm and the purity of more than or equal to 99.0%.
Preferably, the organic cracking carbon source is one or a mixture of two or more of glucose, sucrose, polyethylene glycol, polyvinylpyrrolidone, polyacrylic acid, polyacrylonitrile, epoxy resin, phenolic resin and asphalt.
A preparation method of a graphite/lithium titanate composite negative electrode material for a lithium ion battery comprises the following steps:
(1) mixing a graphite material, lithium titanate and an organic cracking carbon source according to the weight ratio of 100: 1-10: adding the materials into an inorganic solvent or an organic solvent according to the mass ratio of 1-5, mixing the materials by using a high-speed stirrer, and drying the mixture to obtain a graphite/carbon source coating layer/lithium titanate composite material;
(2) and (2) heating the composite material obtained in the step (1) to 600-1050 ℃ at the speed of 1-20 ℃/min under the protection of inert gas atmosphere for sintering, and preserving heat for 1-10h to obtain the graphite/lithium titanate composite cathode material.
Preferably, the inorganic solvent is water, and the organic solvent is one or a mixture of two or more of an alcohol organic solvent, an ether organic solvent, a ketone organic solvent and an aromatic organic solvent.
Preferably, the alcohol organic solvent is one or more of methanol, ethanol, ethylene glycol, n-propanol, isopropanol, propylene glycol, glycerol, n-butanol and isobutanol; the ether organic solvent is one or more of diethyl ether, n-propyl ether and n-butyl ether; the ketone organic solvent is one or more of acetone, butanone and pentanone; the aromatic organic solvent is one or more of benzene, toluene, xylene and ethylbenzene.
Preferably, the inert gas is one or a mixture of two or more of nitrogen, argon and helium.
The invention has the beneficial effects that:
(1) according to the invention, lithium titanate particles are tightly bonded on the cracked carbon layer on the surface of the graphite core, and are not easy to fall off, so that a firm coating layer is formed, the contact area between the graphite material interface and the electrolyte is favorably reduced, and the contact area between the lithium titanate material and the electrolyte is increased, thereby reducing the generation thickness of an SEI (solid electrolyte interphase) film, enhancing the diffusion rate of lithium ions, and improving the safety, rate capability and cycle performance of the graphite cathode material.
(2) The graphite/lithium titanate composite negative electrode material with the shell structure taking the graphite material as the core and the lithium titanate and carbon material coating layer as the shell structure is prepared by adopting conventional means such as stirring dispersion, drying, high-temperature sintering and the like which are widely used in industry, and the preparation method has the advantages of simple and controllable process, low cost and easiness in batch industrial production.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a schematic structural diagram of a graphite/lithium titanate composite anode material of example 1;
fig. 2 is a scanning electron microscope SEM image of the graphite/lithium titanate composite negative electrode material of example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a preparation method of a graphite/lithium titanate composite negative electrode material for a lithium ion battery comprises the following steps:
(1) mixing a natural graphite powder material (with the particle size of 20 mu m and the purity of 99.5%), a lithium titanate powder material (with the particle size of 100nm and the purity of 99.5%) and a polyethylene glycol material according to the weight ratio of 100: 10: 5, adding the mixture into water, mixing the mixture by using a high-speed stirrer, and then performing spray drying to obtain a graphite/organic carbon source coating layer/lithium titanate composite material;
(2) and (2) heating the composite material obtained in the step (1) to 850 ℃ at a speed of 5 ℃/min in a high-temperature furnace under the protection of nitrogen protection atmosphere, sintering, and preserving heat for 4h to obtain the graphite/lithium titanate composite negative electrode material.
Example 2:
a preparation method of a graphite/lithium titanate composite negative electrode material for a lithium ion battery comprises the following steps:
(1) mixing a natural graphite powder material (with the particle size of 25 mu m and the purity of 99.0 percent), a lithium titanate powder material (with the particle size of 200nm and the purity of 99.5 percent) and a polyethylene glycol material according to the weight ratio of 100: 5: 5, adding the mixture into water, mixing the mixture by using a high-speed stirrer, and then performing spray drying to obtain a graphite/organic carbon source coating layer/lithium titanate composite material;
(2) and (2) heating the composite material obtained in the step (1) to 900 ℃ at a speed of 10 ℃/min in a high-temperature furnace under the nitrogen protection atmosphere, sintering, and preserving heat for 2 hours to obtain the graphite/lithium titanate composite negative electrode material.
Example 3:
a preparation method of a graphite/lithium titanate composite negative electrode material for a lithium ion battery comprises the following steps:
(1) mixing a natural graphite powder material (with the particle size of 30 mu m and the purity of 99.5 percent), a lithium titanate powder material (with the particle size of 400nm and the purity of 99.5 percent) and a polyacrylic acid material according to the weight ratio of 100: 1: 2, adding the mixture into ethanol, mixing the mixture by using a high-speed stirrer, and then performing spray drying to obtain a graphite/organic carbon source coating layer/lithium titanate composite material;
(2) and (2) heating the composite material obtained in the step (1) to 700 ℃ at a speed of 15 ℃/min in a high-temperature furnace under the argon protection atmosphere, sintering, and preserving heat for 1h to obtain the graphite/lithium titanate composite negative electrode material.
Example 4:
a preparation method of a graphite/lithium titanate composite negative electrode material for a lithium ion battery comprises the following steps:
(1) mixing mesocarbon microbeads (the particle size is 10 mu m and the purity is 99.5%), a lithium titanate powder material (the particle size is 50nm and the purity is 99.5%) and a phenolic resin material according to the weight ratio of 100: 3: adding the mixture into acetone according to the mass ratio of 1, mixing the mixture by using a high-speed stirrer, and then performing spray drying to obtain a graphite/organic carbon source coating layer/lithium titanate composite material;
(2) and (2) heating the composite material obtained in the step (1) to 1050 ℃ at a speed of 20 ℃/min in a high-temperature furnace under the argon protection atmosphere, sintering, and keeping for 7 hours to obtain the graphite/lithium titanate composite negative electrode material.
Example 5:
in this example, the natural graphite powder material in step (1) in example 1 was replaced with an artificial graphite powder material having a particle size of 20 μm and a purity of 99.5%, and the other preparation steps were kept unchanged.
Example 6:
in this example, the polyethylene glycol material in step (1) in example 1 was replaced with a polyvinylpyrrolidone material, and the other preparation steps were all kept unchanged.
Comparative example 1:
a natural graphite powder material having a particle size of 20 μm and a purity of 99.5% was used as comparative example 1.
Comparative example 2:
a lithium titanate powder material with a particle size of 100nm and a purity of 99.5% was used as comparative example 2.
And (3) performance testing:
the graphite/lithium titanate composite negative electrode materials in the embodiments 1 to 6 of the invention and the powder materials in the comparative examples 1 and 2 are subjected to performance tests, and the test results are shown in table 1.
Table 1:
the test results show that the rate performance and the cycle performance of the graphite/lithium titanate composite negative electrode material prepared by the embodiment of the invention are greatly improved compared with those of a comparative example. The reason can be summarized as that lithium titanate material particles are not easy to fall off because of being tightly adhered on a cracking carbon layer on the surface of graphite, a firm lithium titanate coating layer is formed, the contact area of a graphite material interface and an electrolyte is reduced, the generation thickness of an SEI film is reduced, the lithium ion diffusion rate is enhanced, and the rate capability and the cycle performance of the composite material are improved.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (7)
1. A graphite/lithium titanate composite negative electrode material for a lithium ion battery is characterized in that: the graphite/lithium titanate composite negative electrode material is a graphite/lithium titanate composite material which takes a graphite material as a core and takes lithium titanate and an organic cracking carbon coating layer as a shell structure and is formed by forming lithium titanate and an organic cracking carbon coating layer on the surfaces of graphite material particles; the raw materials for preparing the graphite/lithium titanate composite negative electrode material comprise a graphite material, lithium titanate and an organic cracking carbon source, wherein the mass ratio of the graphite material to the lithium titanate to the organic cracking carbon source is 100: 1-10: 1-5, wherein the particle size of the graphite material is 5-30 mu m, and the particle size of the lithium titanate is 10-500nm;
the preparation method of the graphite/lithium titanate composite negative electrode material comprises the following steps:
(1) mixing a graphite material, lithium titanate and an organic cracking carbon source according to the weight ratio of 100: 1-10: adding the materials into an inorganic solvent or an organic solvent according to the mass ratio of 1-5, mixing the materials by using a high-speed stirrer, and drying the mixture to obtain a graphite/carbon source coating layer/lithium titanate composite material;
(2) and (2) heating the composite material obtained in the step (1) to 600-1050 ℃ at the speed of 1-20 ℃/min under the protection of inert gas or nitrogen atmosphere, sintering, and preserving heat for 1-10h to obtain the graphite/lithium titanate composite negative electrode material.
2. The graphite/lithium titanate composite negative electrode material for the lithium ion battery as claimed in claim 1, wherein the graphite material is one or a mixture of two of natural graphite and artificial graphite, and the purity of the graphite material is not less than 99%.
3. The graphite/lithium titanate composite negative electrode material for the lithium ion battery as claimed in claim 1, wherein the purity of the lithium titanate is not less than 99.0%.
4. The graphite/lithium titanate composite negative electrode material for the lithium ion battery according to claim 1, wherein the organic cracking carbon source is one or a mixture of two or more of glucose, sucrose, polyethylene glycol, polyvinylpyrrolidone, polyacrylic acid, polyacrylonitrile, epoxy resin, phenolic resin and asphalt.
5. The graphite/lithium titanate composite negative electrode material for the lithium ion battery according to claim 1, wherein the inorganic solvent is water, and the organic solvent is one or a mixture of two or more of an alcohol organic solvent, an ether organic solvent, a ketone organic solvent, and an aromatic organic solvent.
6. The graphite/lithium titanate composite negative electrode material for the lithium ion battery according to claim 5, wherein the alcohol organic solvent is one or more of methanol, ethanol, ethylene glycol, n-propanol, isopropanol, propylene glycol, glycerol, n-butanol and isobutanol; the ether organic solvent is one or more of diethyl ether, n-propyl ether and n-butyl ether; the ketone organic solvent is one or more of acetone, butanone and pentanone; the aromatic organic solvent is one or more of benzene, toluene, xylene and ethylbenzene.
7. The graphite/lithium titanate composite negative electrode material for the lithium ion battery according to claim 1, wherein the inert gas is one or a mixture of argon and helium.
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CN1585172A (en) * | 2004-06-12 | 2005-02-23 | 深圳市贝特瑞电子材料有限公司 | Graphite negative material of lithium ion battery and producing method thereof |
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