CN111029549A - High-performance lithium ion battery cathode structure and preparation method thereof - Google Patents
High-performance lithium ion battery cathode structure and preparation method thereof Download PDFInfo
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- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H—ELECTRICITY
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The invention discloses a high-performance lithium ion battery cathode structure and a preparation method thereof, the lithium ion battery cathode structure comprises an inner core and an outer shell, the inner core is composed of graphite, the outer shell comprises red phosphorus, carbon nano tubes, an inorganic lithium compound and a binder, the thickness ratio of the inner core to the outer shell is 20: x, wherein X is greater than or equal to 1 and less than or equal to 4. The lithium ion battery cathode has the advantages of high gram capacity, good rate capability, excellent low-temperature performance and good cycle performance.
Description
Technical Field
The invention relates to the field of preparation of lithium ion battery materials, in particular to a high-performance lithium ion battery cathode structure and a preparation method thereof.
Background
With the rapid development of electric vehicles, lithium ion batteries are required to have higher energy density and rapid charging and discharging capabilities. The method for improving the energy density of the lithium ion battery mainly comprises the following steps: 1) the high-capacity anode and cathode materials are adopted, such as a silicon-carbon anode material, but the silicon-carbon anode material has high expansion rate, so that the cycle performance is poor and the industrialization is difficult to realize; 2) high-voltage electrolyte is adopted, for example, organic electrolyte with the voltage of more than 4.35V is adopted, but the current technical conditions are difficult to break through; 3) thinner positive and negative current collectors are adopted, but the difficulty of the preparation process is larger, so that great breakthrough is difficult to make in the near term. The method for improving the rapid charge and discharge of the lithium ion battery mainly comprises the following steps: 1) adopting a multiplying power type anode and cathode material; 2) adopting electrolyte with high lithium ion conductivity; 3) adopting a current collector prime coat coating technology; 4) and optimizing the design of the battery. The measures can show that the energy density and the quick charging performance of the material can be fundamentally improved by adopting the anode and cathode materials. However, while the gram volume of the material is increased, the rate capability, low temperature performance and cycle performance of the material are adversely affected. Therefore, it is necessary to develop a material which can improve the capacity and also improve the rate capability and low temperature performance.
Disclosure of Invention
The invention provides a high-performance lithium ion battery cathode structure and a preparation method thereof for solving the technical problems, and the lithium ion battery cathode has the advantages of high gram capacity, good rate capability, excellent low-temperature performance and good cycle performance.
The invention is realized by the following technical scheme:
the high-performance lithium ion battery cathode structure comprises an inner core and an outer shell, wherein the inner core is made of graphite, the outer shell comprises red phosphorus, carbon nano tubes, inorganic lithium compounds and a binder, and the thickness ratio of the inner core to the outer shell is 20: x, wherein X is greater than or equal to 1 and less than or equal to 4. The scheme adopts a coating principle, and the surface of the cathode material is coated with the functional substance, so that the electrochemical performance of the material is improved. The coating layer is too thin, and the effect of improving the performance is not ideal; the coating layer is too thick, so that the preparation process is not well realized, and the particle surface is not coated but agglomerated and granulated under the condition, the structure is changed, the characteristics of the material are changed along with the change, and the thickness ratio of the inner core to the outer shell is set within the range in order to improve the chemical performance of the cathode structure.
A preparation method of a high-performance lithium ion battery cathode adopts the structure, and comprises the following steps:
preparing a red phosphorus mixed solution: weighing 6-8 g of polyvinylidene fluoride and 2-4 g of polyamide, adding the polyvinylidene fluoride and the polyamide into 50g of N-methyl pyrrolidone, uniformly dispersing at a high speed to obtain a binder with a solid content of 20%, weighing 60-70 g of red phosphorus, 5-10 g of carbon nano tube, 10-30 g of inorganic lithium compound and 500g of N-methyl pyrrolidone, adding the red phosphorus, the carbon nano tube, the inorganic lithium compound and the N-methyl pyrrolidone into 25-50 g of the binder, and dispersing for 1-3 h by using a high-speed dispersion machine to obtain a red phosphorus mixed solution;
and (3) graphite coating: weighing 500g of graphite, adding the graphite into the red phosphorus mixed solution, stirring at 80 ℃ for 2h, transferring the mixture into a tubular furnace, heating to 200-300 ℃ at a heating rate of 1-10 ℃/min under the protection of nitrogen, preserving heat for 1-3 h, heating to 1000-1500 ℃ at 1-10 ℃/min, preserving heat for 1-3 h, and cooling to room temperature to obtain the graphite composite material coated with the phosphorus, lithium and carbon nano tubes.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the negative electrode structure of the lithium ion battery is coated by adopting the phosphorus, lithium and carbon nano tubes, and the gram capacity of the negative electrode material and the transmission rate of lithium ions under a high-rate condition are improved by utilizing the characteristics of high gram capacity and large interlayer spacing of red phosphorus, so that the rate performance of the negative electrode material is improved; meanwhile, the doped inorganic lithium compound provides sufficient lithium ions in the high-rate charge-discharge process, and the first efficiency, rate performance and low-temperature performance of the material are improved; and the carbon nano tube improves the conductivity of the doped phosphorus, so that the electronic conductivity of the coating layer is improved, and a synergistic effect is generated between the carbon nano tube and the lithium ion conductivity of the inorganic lithium compound, so that the rate capability and the cycle performance of the lithium ion battery can be improved while the energy density of lithium ions is improved.
Drawings
The accompanying drawings, which are included to provide a further understanding of the embodiments of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention.
Fig. 1 is a scanning electron microscope test chart of the composite anode material prepared by the method of example 2.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples and accompanying drawings, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not meant to limit the present invention.
Example 1
A high-performance lithium ion battery cathode structure comprises an inner core and an outer shell, wherein the inner core is made of graphite, the outer shell comprises red phosphorus, carbon nano tubes, inorganic lithium compounds and a binder, and the thickness ratio of the inner core to the outer shell is 20: x, wherein X is greater than or equal to 1 and less than or equal to 4.
Wherein the weight ratio of the red phosphorus to the carbon nano tube to the inorganic lithium compound to the binder is A to B to C to D, wherein A is more than or equal to 60 and less than or equal to 70, B is more than or equal to 5 and less than or equal to 10, C is more than or equal to 5 and less than or equal to 10, and D is more than or equal to 10 and less than or equal to 30. The adhesive comprises the following components in percentage by weight: 6-8 parts of polyvinylidene fluoride, 2-4 parts of polyamide and 50 parts of N-methyl pyrrolidone. The inorganic lithium compound is one or more of lithium metaaluminate, lithium carbonate and lithium hydroxide.
Specifically, the preparation method of the lithium ion battery cathode comprises the following steps:
preparing a red phosphorus mixed solution: weighing 6-8 g of polyvinylidene fluoride and 2-4 g of polyamide, adding the polyvinylidene fluoride and the polyamide into 50g of N-methyl pyrrolidone, uniformly dispersing at a high speed to obtain a binder with a solid content of 20%, weighing 60-70 g of red phosphorus, 5-10 g of carbon nano tube, 10-30 g of inorganic lithium compound and 500g of N-methyl pyrrolidone, adding the red phosphorus, the carbon nano tube, the inorganic lithium compound and the N-methyl pyrrolidone into 25-50 g of the binder, and dispersing for 1-3 h by using a high-speed dispersion machine to obtain a red phosphorus mixed solution;
and (3) graphite coating: weighing 500g of graphite, adding the graphite into the red phosphorus mixed solution, stirring at 80 ℃ for 2h, transferring the mixed solution into a tubular furnace, heating to 200-300 ℃ at a heating rate of 1-10 ℃/min under the protection of nitrogen, preserving heat for 1-3 h, heating to 1000-1500 ℃ at 1-10 ℃/min, preserving heat for 1-3 h, and then cooling to room temperature.
Example 2
Based on the above structure and preparation method, this example discloses a specific implementation manner.
Preparing a red phosphorus mixed solution: weighing 7g of polyvinylidene fluoride and 3g of polyamide, adding the polyvinylidene fluoride and the polyamide into 50g of N-methyl pyrrolidone, and uniformly dispersing at a high speed to obtain a binder with the solid content of 20%; weighing 65g of red phosphorus, 8g of carbon nano tube, 20g of inorganic lithium compound and 500g of N-methyl pyrrolidone, adding into 40g of binder, and dispersing for 2h by a high-speed dispersion machine to obtain a red phosphorus mixed solution;
and (3) graphite coating: weighing 500g of graphite, adding the graphite into the red phosphorus mixed solution, stirring for 2h at 80 ℃, transferring the mixed solution into a tubular furnace, heating to 250 ℃ at a heating rate of 5 ℃/min under the protection of nitrogen, preserving heat for 2h, heating to 1200 ℃ at 5 ℃/min, preserving heat for 2h, and then naturally cooling to room temperature.
A scanning electron microscope test chart of the composite cathode material prepared by the method is shown in FIG. 1, and the composite cathode material is spherical, smooth in surface, reasonable in particle distribution and small in particle size (5-10) mu m.
Example 3
This example discloses a specific embodiment based on the structure and preparation method of example 1.
Preparing a red phosphorus mixed solution: weighing 6g of polyvinylidene fluoride and 4g of polyamide, adding the polyvinylidene fluoride and the polyamide into 50g of N-methyl pyrrolidone, and uniformly dispersing at a high speed to obtain a binder with the solid content of 20%; weighing 60g of red phosphorus, 5g of carbon nano tube, 30g of inorganic lithium compound and 500g of N-methyl pyrrolidone, adding into 25g of binder, and dispersing for 2 hours by a high-speed dispersion machine to obtain a red phosphorus mixed solution;
and (3) graphite coating: weighing 500g of graphite, adding the graphite into the red phosphorus mixed solution, stirring for 2h at 80 ℃, transferring the mixed solution into a tubular furnace, heating to 200 ℃ at a heating rate of 1 ℃/min under the protection of nitrogen, preserving heat for 1h, heating to 1000 ℃ at 1 ℃/min, preserving heat for 1h, and then naturally cooling to room temperature.
Example 4
This example discloses a specific embodiment based on the structure and preparation method of example 1.
Preparing a red phosphorus mixed solution: weighing 8g of polyvinylidene fluoride and 2g of polyamide, adding the polyvinylidene fluoride and the polyamide into 50g of N-methyl pyrrolidone, and uniformly dispersing at a high speed to obtain a binder with the solid content of 20%; weighing 70g of red phosphorus, 10g of carbon nano tube, 10g of inorganic lithium compound and 500g of N-methyl pyrrolidone, adding into 50g of binder, and dispersing for 3h by a high-speed dispersion machine to obtain a red phosphorus mixed solution;
and (3) graphite coating: weighing 500g of graphite, adding the graphite into the red phosphorus mixed solution, stirring for 2h at 80 ℃, transferring the mixed solution into a tubular furnace, heating to 300 ℃ at a heating rate of 10 ℃/min under the protection of nitrogen, preserving heat for 1h, heating to 1500 ℃ at 10 ℃/min, preserving heat for 3h, and then naturally cooling to room temperature.
The lithium ion battery cathode materials prepared by the methods of examples 2 to 4 are respectively assembled into button batteries A1, A2, A3 and B1; the negative electrode material used in the comparative example was commercially available artificial graphite.
The preparation method comprises the following steps: and adding a binder, a conductive agent and a solvent into the negative electrode material, stirring and pulping, coating the mixture on a copper foil, drying and rolling, and assembling the simulated battery in a glove box. The binder is LA132 binder, the conductive agent SP, the negative electrode material is respectively the negative electrode material prepared in the embodiment 1-3 and the comparative example, the solvent is secondary distilled water, and the proportion is that the negative electrode material: SP: LA 132: double distilled water =95 g: 1 g: 4 g: 220 mL; the electrolyte is LiPF6/EC + DEC (1: 1), the metal lithium sheet is a counter electrode, the diaphragm is a Polyethylene (PE), polypropylene (PP) or polyethylene propylene (PEP) composite film, the electrochemical performance is carried out on a battery tester of the Wuhan blue electricity CT2001A type, the charge-discharge voltage range is 0.005V-2.0V, and the charge-discharge rate is 0.1C. The test results are detailed in table 1:
TABLE 1 comparison of the Power-on test for examples and comparative examples
As can be seen from Table 1, the discharge capacity and efficiency of the rechargeable battery using the negative electrode materials obtained in examples 1-3 are significantly higher than those of the comparative examples. Experimental results show that the modified negative electrode material has higher discharge capacity and efficiency, because the artificial graphite surface is coated with a high-capacity phosphorus material, the discharge capacity of the composite negative electrode material is improved, meanwhile, the red phosphorus material is doped with a carbon nano tube conductive agent with high conductivity, the conductivity of the material is improved, lithium ions are consumed due to the SEI film formed in the negative electrode material, and the inorganic lithium compound is coated on the graphite surface to provide the lithium ions, so that the first efficiency of the material is improved, and the gram capacity exertion of the material and the first efficiency of the material are finally improved.
The materials obtained by the methods of examples 2 to 4 and the artificial graphite purchased in the market are respectively used as a negative electrode material, lithium iron phosphate is used as a positive electrode material, LiPF6/EC + DEC (1: 1) is used as an electrolyte, a Celgard 2400 membrane is used as a diaphragm, 5Ah soft package batteries C1, C2, C3 and D1 are prepared, and the cycle performance (the charge-discharge rate is 1.0C/1.0C) and the rate performance of the negative electrode material are tested.
And (3) rate testing: the charge rate standard is (0.5C, 1.0C, 2.0C, 3.0C), the discharge rate is 0.3C, the temperature is 23 ± 5 ℃, the voltage range: 2.5-3.65V.
TABLE 2 comparison of the cycling performance of the examples and comparative examples
As can be seen from table 2, examples 2 to 4 are superior to the comparative example in cycle performance at each stage because the lithium compound coated on the surface of graphite provides sufficient lithium ions during charge and discharge to provide cycle performance thereof, and the carbon nanotubes have a large specific surface area to improve electron transport performance and liquid absorption and retention capacity thereof and further improve cycle performance thereof.
TABLE 3 rate charge Performance of pouch cells
As can be seen from table 3, the rate charge performance of the pouch cells in examples 2-4 is significantly better than the comparative example, i.e., the charge time is shorter, the analytical reason is that: the battery needs the migration of lithium ions in the charging process, and the coating layer contains the lithium ions and can provide sufficient lithium ions, so that the charging time is shortened, and the rate charging performance of the battery is improved.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (5)
1. The utility model provides a high performance lithium ion battery negative pole structure which characterized in that: the graphite composite material comprises an inner core and an outer shell, wherein the inner core is made of graphite, the outer shell comprises red phosphorus, carbon nano tubes, an inorganic lithium compound and a binder, and the thickness ratio of the inner core to the outer shell is 20: x, wherein X is greater than or equal to 1 and less than or equal to 4.
2. The negative electrode structure of the high-performance lithium ion battery of claim 1, wherein the weight ratio of the red phosphorus, the carbon nanotube, the inorganic lithium compound and the binder is A: B: C: D, wherein A is greater than or equal to 60 and less than or equal to 70, B is greater than or equal to 5 and less than or equal to 10, C is greater than or equal to 5 and less than or equal to 10, and D is greater than or equal to 10 and less than or equal to 30.
3. The negative electrode structure of the high-performance lithium ion battery as claimed in claim 1, wherein the binder comprises the following components in parts by weight: 6-8 parts of polyvinylidene fluoride, 2-4 parts of polyamide and 50 parts of N-methyl pyrrolidone.
4. The negative electrode structure of claim 1, wherein the inorganic lithium compound is one or more of lithium metaaluminate, lithium carbonate and lithium hydroxide.
5. A preparation method of a high-performance lithium ion battery cathode is characterized in that the lithium ion battery cathode adopts the structure of any one of claims 1 to 4, and the preparation method comprises the following steps:
preparing a red phosphorus mixed solution: weighing 6-8 g of polyvinylidene fluoride and 2-4 g of polyamide, adding the polyvinylidene fluoride and the polyamide into 50g of N-methyl pyrrolidone, uniformly dispersing at a high speed to obtain a binder with a solid content of 20%, weighing 60-70 g of red phosphorus, 5-10 g of carbon nano tube, 10-30 g of inorganic lithium compound and 500g of N-methyl pyrrolidone, adding the red phosphorus, the carbon nano tube, the inorganic lithium compound and the N-methyl pyrrolidone into 25-50 g of the binder, and dispersing for 1-3 h by using a high-speed dispersion machine to obtain a red phosphorus mixed solution;
and (3) graphite coating: weighing 500g of graphite, adding the graphite into the red phosphorus mixed solution, stirring at 80 ℃ for 2h, transferring the mixed solution into a tubular furnace, heating to 200-300 ℃ at a heating rate of 1-10 ℃/min under the protection of nitrogen, preserving heat for 1-3 h, heating to 1000-1500 ℃ at 1-10 ℃/min, preserving heat for 1-3 h, and then cooling to room temperature.
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| CN116283363A (en) * | 2023-03-21 | 2023-06-23 | 重庆长安新能源汽车科技有限公司 | High-energy-density quick-charging graphite composite material, preparation method and application |
| CN116632213A (en) * | 2023-06-30 | 2023-08-22 | 深圳市华明胜科技有限公司 | Modified graphite negative electrode material with high gram capacity and preparation process thereof |
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Application publication date: 20200417 |