CN111048755A - High-rate lithium ion battery cathode material and preparation method thereof - Google Patents
High-rate lithium ion battery cathode material and preparation method thereof Download PDFInfo
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- CN111048755A CN111048755A CN201911218190.3A CN201911218190A CN111048755A CN 111048755 A CN111048755 A CN 111048755A CN 201911218190 A CN201911218190 A CN 201911218190A CN 111048755 A CN111048755 A CN 111048755A
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- 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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a high-rate lithium ion battery cathode material and a preparation method thereof, wherein the preparation method comprises the steps of firstly preparing a mixed solution of potassium carbonate and nitrogen-phosphorus-containing organic matters, then adding the mixed solution into a hydrochloric acid solution, uniformly stirring, adding crystalline flake graphite, uniformly mixing to prepare a graphite mixed solution, filtering, carbonizing, and modifying the surface of gas to obtain a graphite composite material; the nitrogen and phosphorus substances formed after the carbonization of the nitrogen and phosphorus compounds improve the conductivity of the material, and the nanometer micron holes left by the oxidation of the gas surface improve the lithium ion embedding channel, so the multiplying power performance and the cycle performance of the negative electrode material are improved.
Description
Technical Field
The invention belongs to the field of preparation of lithium ion battery materials, and particularly relates to a high-rate lithium ion battery cathode material and a preparation method thereof.
Background
With the improvement of the market requirements on the fast charge, low temperature performance and cycle performance of electric automobiles, the negative electrode material used by the lithium ion battery is required to have the characteristics of high rate performance, good cycle performance and the like, while the current commercial negative electrode material of the lithium ion battery mainly takes a carbon material as a main material, the carbon negative electrode material comprises graphite, soft carbon and hard carbon, wherein the graphite capacity is the highest in gram capacity, the theoretical capacity is 372mAh/g, and the actual capacity plays more than 365 mAh/g. However, lithium ions can only enter and exit from the graphite layer structure from the edge of the graphite layer, i.e. from the direction parallel to the graphite layer, and cannot enter and exit from the direction perpendicular to the graphite layer, so that the diffusion coefficient of lithium ions entering and exiting from the graphite layer is small, directly resulting in poor rate performance of the lithium ion battery. In addition, when lithium ions do not have time to diffuse into the graphite layers during charge and discharge at a high rate, the lithium ions are concentrated on the surface of the negative electrode and reduced into metallic lithium dendrites having extremely high activity. The lithium dendrite is easy to react with the electrolyte, consumes the electrolyte, reduces the capacity of the battery and seriously shortens the cycle life of the battery. Therefore, it is necessary and urgent to solve the rate capability of the graphite negative electrode material, either in terms of charge/discharge rate or cycle performance. At present, the field of electric automobiles puts forward higher requirements on the energy density, the quick charging performance and the service life of the next generation of lithium ion batteries, and through the coating and modification of graphite materials, nitrogen and phosphorus materials with high conductivity are coated on the surfaces of the graphite materials, and the nano-pore graphite and the micro-pore graphite of the materials are modified, so that the high-power requirement of the lithium ion batteries is met. The material with high conductivity and structural stability is coated on the surface of the graphite, so that the occurrence probability of side reaction is reduced, the lithium ion intercalation and deintercalation rate is improved, and the lithium ion intercalation and deintercalation rate and the rate capability are improved by forming pores on the surface of the graphite through oxidation. For example, patent CN 101908627a discloses a negative electrode material of a lithium ion secondary battery and a preparation method thereof, which mainly adds an additive and a pore-forming agent for increasing graphitization degree into raw coke after carbonization treatment, the prepared graphite negative electrode material has a porous structure and higher graphitization degree, a certain amount of pore-forming agent is added before graphitization treatment, and the graphite negative electrode material has a nano-porous structure, which can effectively improve the lithium-intercalation removing performance of the negative electrode material and the liquid absorption performance of a pole piece, but because pores prepared by the pore-forming agent are of a micro-structure, the uniformity is poor, and the application of the material is affected.
Disclosure of Invention
Aiming at the defects of poor rate performance and the like of the conventional graphite composite material, the invention improves the lithium ion intercalation and deintercalation rate and the electrical conductivity thereof by coating a nitrogen-phosphorus compound on the surface of graphite, and improves the liquid absorption capacity of the material and the lithium ion intercalation and deintercalation channel thereof by pore-forming on the surface of gas, thereby improving the rate performance of the lithium ion cathode material.
The high-rate lithium ion battery negative electrode material is characterized by comprising an inner core and a shell coated outside the inner core, wherein the inner core is crystalline flake graphite, and the shell is a porous complex containing nitrogen, phosphorus and carbon.
The mass of the flake graphite is 85-99% of that of the negative electrode material.
The thickness of the shell is 200-2000 nm.
A high-rate lithium ion battery cathode material and a preparation method thereof are disclosed, wherein the preparation process comprises the following steps:
1) weighing 10-50 g of nitrogen and phosphorus organic matters, 1-5 g of sodium dodecyl benzene sulfonate and 1-5 g of potassium carbonate, adding the mixture into 500g of organic solvent, and uniformly stirring to obtain a mixed solution (marked as solution A); then adding (20-40) ml of 1.0mol/L hydrochloric acid solution, and uniformly stirring to obtain a mixed solution B; then adding 100-200 g of crystalline flake graphite into the mixed solution B, performing ultrasonic dispersion for 10-60 min, filtering and washing to obtain a modified graphite composite material, heating to 700-900 ℃ at a heating rate of 1-5 ℃/min in an inert atmosphere, preserving heat for 1-3 h, and naturally cooling to room temperature to obtain a graphite composite material C;
2) and then transferring the composite material C into a tubular furnace, introducing inert gas, heating to 300-400 ℃, then introducing gas modifier/inert gas mixed gas (in a volume ratio of 1: 1), heating to 600-900 ℃, preserving heat for 1-6 hours, then stopping introducing the mixed gas, introducing the inert gas, and then naturally cooling to room temperature to obtain the graphite composite material D.
The nitrogen and phosphorus organic matter in the step (1) is one of phosphatidylethanolamine, cyclophosphamide, triethanolamine phosphate, hexadecanol phosphate diethanolamide, phosmet, phosphorodiamidate, phosphoramidite, phosmet, melamine phosphate and pyrrole amine phosphate;
the gas modifier in the step (2) is one of fluorine gas, chlorine gas and bromine gas;
has the advantages that:
the surface of the graphite is coated with the nitrogen-phosphorus compound, the conductivity of the material and the compatibility of the material and an electrolyte are improved by using the nitrogen-phosphorus substance formed after the nitrogen-phosphorus compound is carbonized, and meanwhile, nano/micron holes are left in gas generated after the reaction of potassium carbonate and dilute hydrochloric acid, so that the lithium ion intercalation rate of the material is improved, and the rate capability of the material is improved; meanwhile, the gas oxidant is oxidized on the outer surface of the material to form nano holes, so that the lithium ion intercalation channel is further improved, and the rate capability and gram capacity of the material are improved.
Drawings
Fig. 1 is an SEM image of the graphite composite material prepared in example 1.
Detailed Description
Example 1
1) Weighing 30g of phosphatidylethanolamine, 3g of sodium dodecyl benzene sulfonate and 3g of potassium carbonate, adding the mixture into 500g of carbon tetrachloride organic solvent, uniformly stirring to obtain a mixed solution (marked as solution A), then adding 30ml of 1.0mol/L hydrochloric acid solution into the solution A, and uniformly stirring to obtain a mixed solution B; adding 150g of crystalline flake graphite into the mixed solution B, ultrasonically dispersing for 30min, filtering and washing to obtain a modified graphite composite material, heating to 800 ℃ at a heating rate of 3 ℃/min under an argon atmosphere, preserving heat for 2h, and naturally cooling to room temperature to obtain a graphite composite material C;
2) and then transferring the composite material C into a tubular furnace, introducing argon inert gas, heating to 350 ℃, introducing a chlorine/argon mixed gas (in a volume ratio of 1: 1), heating to 800 ℃, keeping the temperature for 3 hours, stopping introducing the mixed gas, introducing the argon inert gas, and naturally cooling to room temperature to obtain a graphite composite material D.
Example 2
1) Weighing 10g of cyclic amine phosphate, 1g of sodium dodecyl benzene sulfonate and 1g of potassium carbonate, adding the mixture into 500g of N-methyl pyrrolidone organic solvent, and uniformly stirring to obtain a mixed solution (marked as solution A); then adding 20ml of 1.0mol/L hydrochloric acid solution into the solution A, and uniformly stirring to obtain a mixed solution B; then adding 100g of crystalline flake graphite into the mixed solution B, ultrasonically dispersing for 10min, filtering and washing to obtain a modified graphite composite material, heating to 700 ℃ at a heating rate of 1 ℃/min under an argon atmosphere, preserving heat for 3h, and naturally cooling to room temperature to obtain a graphite composite material C;
2) and then transferring the composite material C to a tubular furnace, introducing argon inert gas, heating to 300 ℃, introducing fluorine gas/argon gas mixed gas (in a volume ratio of 1: 1), heating to 600 ℃, keeping the temperature for 6 hours, stopping introducing the mixed gas, introducing argon inert gas, and naturally cooling to room temperature to obtain the graphite composite material D.
Example 3
1) Weighing 50g of triethanolamine phosphate, 5g of sodium dodecyl benzene sulfonate and 5g of potassium carbonate, adding into 500g of toluene organic solvent, and uniformly stirring to obtain a mixed solution (marked as solution A); then adding 40ml of 1.0mol/L hydrochloric acid solution into the solution A, and uniformly stirring to obtain a mixed solution B; then adding 200g of crystalline flake graphite, ultrasonically dispersing for 60min, filtering and washing to obtain a modified graphite composite material, then heating to 900 ℃ at a heating rate of 5 ℃/min under an argon atmosphere, preserving heat for 1h, and then naturally cooling to room temperature to obtain a graphite composite material C;
2) and then transferring the composite material C to a tubular furnace, introducing argon inert gas, heating to 400 ℃, introducing bromine gas/argon mixed gas (in a volume ratio of 1: 1), heating to 900 ℃, keeping the temperature for 1h, stopping introducing the mixed gas, introducing argon inert gas, and naturally cooling to room temperature to obtain a graphite composite material D.
Comparative example: weighing 30g of asphalt, adding into 100ml of carbon tetrachloride, adding 150g of flake graphite, coating by a coating machine, filtering, heating to 500 ℃ under argon atmosphere, carbonizing for 3h, and crushing and grading to obtain the graphite composite material.
1) SEM test
FIG. 1 is an SEM image of the graphite composite material prepared in example 1, and it can be seen from the SEM image that the material is spherical, the particle size is (10-14) mum, and the size distribution is reasonable.
2) Testing the physical and chemical properties of the material:
assembling the lithium ion battery negative electrode materials obtained in the examples 1-3 and the comparative example into button batteries A1, A2, A3 and B1 respectively; the preparation method comprises the following steps: adding a binder, a conductive agent and a solvent into the negative electrode material, stirring and pulping, coating the mixture on a copper foil, and drying and rolling the copper foil to obtain the copper-clad laminate. 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 as follows: and (3) anode material: SP: LA 132: double distilled water =95 g: 1 g: 4 g: 220mL, and preparing a negative pole piece; the electrolyte is LiPF6The battery is characterized in that the battery comprises/EC + DEC (volume ratio is 1:1, concentration is 1.3 mol/L), a metal lithium sheet is a counter electrode, a diaphragm adopts a Polyethylene (PE), polypropylene (PP) or polyethylene propylene (PEP) composite film, a simulation battery is assembled in a glove box filled with argon, electrochemical performance is carried out on a Wuhan blue electricity CT2001A type battery tester, the charging and discharging voltage range is 0.005V-2.0V, and the charging and discharging rate is 0.1C. The liquid absorption and retention capacity was also tested and is detailed in table 1.
Test methods reference: GB/T-2433one 2009 graphite cathode material for lithium ion batteries:
wherein: the method for testing the liquid absorbing capacity comprises the following steps: and (3) adopting a 1ml burette, absorbing the electrolyte Vml, then dripping one drop on the surface of the pole piece, timing until the electrolyte on the surface of the pole piece is absorbed, and recording time (t) to obtain the liquid absorption speed V/t.
TABLE 1 comparison of the Power-on test for examples and comparative examples
As can be seen from table 1, the first discharge capacity and the first efficiency of the rechargeable battery using the negative electrode materials obtained in examples 1 to 3 are significantly higher than those of the comparative examples, because the surface of the material of the examples is coated with the nitrogen-phosphorus-carbon composite material having high conductivity, the conductivity of the material of the examples is improved, the gram capacity of the negative electrode material is improved, and meanwhile, the nano-pores formed on the surface can accommodate a part of lithium ions; meanwhile, oxidizing the defect part of the material by oxidizing gas, so that the defect degree of the material is reduced, and the first efficiency of the material is improved; and the surface of the material is subjected to pore-forming by using oxidizing gas to improve the specific surface area of the material and further improve the liquid absorption capacity of the material.
3) Testing the soft package battery:
the materials obtained in example 1, example 2, example 3 and comparative example were used as negative electrode materials, lithium iron phosphate was used as positive electrode material, and LiPF was used6The electrolyte is prepared from/EC + DEC (volume ratio of 1:1, concentration of 1.3 mol/L) and the diaphragm is prepared from Celgard 2400 membrane, and 5Ah soft-package batteries C1, C2, C3 and D1 are tested for cycle performance (charge-discharge rate of 1.0C/1.0C) and rate performance (charge rate of 1C/3C/5C/10C/15C).
TABLE 2 comparison of the cycling performance of the examples and comparative examples
As can be seen from Table 2, the cycle performance of examples 1-3 is superior to that of the comparative example in each stage because the materials of examples contain micro/nano pores inside and on the surface, so that more electrolyte can be stored, more electrolyte can be provided in the charging and discharging process, and the cycle performance of the materials can be improved.
TABLE 3 multiplying power charging comparison table
As can be seen from table 3, the soft package battery made of the material prepared in the example has a better constant current ratio, and the reason is that the surface of the material of the example is coated with the nitrogen-phosphorus carbon material with large interlayer spacing and many nano holes, so that the quick charge performance of the material is improved, that is, the constant current ratio of the lithium ion battery is improved.
Claims (6)
1. The high-rate lithium ion battery cathode material is characterized by comprising an inner core and a shell coated outside the inner core, wherein the inner core is crystalline flake graphite, and the shell is a porous complex containing nitrogen, phosphorus and carbon.
2. The high-rate lithium ion battery negative electrode material as claimed in claim 1, wherein the mass of the crystalline flake graphite is 85-99% of the mass of the negative electrode material.
3. The high-rate lithium ion battery negative electrode material as claimed in claim 1, wherein the thickness of the shell is 200-2000 nm.
4. The preparation method of the high-rate lithium ion battery negative electrode material according to claim 1, characterized by comprising the following steps:
weighing 10-50 g of nitrogen and phosphorus organic matters, 1-5 g of sodium dodecyl benzene sulfonate and 1-5 g of potassium carbonate, adding the mixture into 500g of organic solvent, and uniformly stirring to obtain a mixed solution (marked as solution A); then adding (20-40) ml of 1.0mol/L hydrochloric acid solution, and uniformly stirring to obtain a mixed solution B; then adding 100-200 g of crystalline flake graphite into the mixed solution B, performing ultrasonic dispersion for 10-60 min, filtering and washing to obtain a modified graphite composite material, heating to 700-900 ℃ at a heating rate of 1-5 ℃/min in an inert atmosphere, preserving heat for 1-3 h, and naturally cooling to room temperature to obtain a graphite composite material C;
and then transferring the graphite composite material C into a tubular furnace, introducing inert gas, heating to 300-400 ℃, then introducing gas modifier/inert gas mixed gas (volume ratio is 1: 1), heating to 600-900 ℃, preserving heat for 1-6 hours, then stopping introducing the mixed gas, introducing the inert gas, and then naturally cooling to room temperature to obtain the graphite composite material D.
5. The preparation method of the high-rate lithium ion battery negative electrode material according to claim 4, wherein the nitrogen-phosphorus organic substance in the step (1) is one of phosphatidylethanolamine, cyclophosphamide, diethanolamine phosphate, hexadecanol phosphate diethanolamide, phosmet, phosphorodiamidate, phosphoramidite, phosmet, melamine phosphate and pyrrole amine phosphate.
6. The method for preparing the high-rate lithium ion battery negative electrode material according to claim 4, wherein the gas modifier in the step (2) is one of fluorine gas, chlorine gas and bromine gas.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112467123A (en) * | 2020-08-14 | 2021-03-09 | 珠海中科兆盈丰新材料科技有限公司 | High-capacity lithium ion battery cathode material and preparation method thereof |
| CN112467135A (en) * | 2020-09-09 | 2021-03-09 | 珠海中科兆盈丰新材料科技有限公司 | Silicon-carbon composite material, preparation method and lithium ion battery thereof |
| WO2022170346A1 (en) * | 2021-02-04 | 2022-08-11 | Global Graphene Group, Inc. | Elastic flame-retardant polymer-encapsulated anode particles for lithium batteries and method of manufacturing |
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| CN105932320A (en) * | 2016-05-18 | 2016-09-07 | 河南田园新能源科技有限公司 | Method for preparing composite cathode material by modification of graphite |
| CN106450311A (en) * | 2016-10-14 | 2017-02-22 | 焦作聚能能源科技有限公司 | Graphite composite anode material and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112467123A (en) * | 2020-08-14 | 2021-03-09 | 珠海中科兆盈丰新材料科技有限公司 | High-capacity lithium ion battery cathode material and preparation method thereof |
| CN112467123B (en) * | 2020-08-14 | 2022-06-10 | 珠海中科兆盈丰新材料科技有限公司 | High-capacity lithium ion battery cathode material and preparation method thereof |
| CN112467135A (en) * | 2020-09-09 | 2021-03-09 | 珠海中科兆盈丰新材料科技有限公司 | Silicon-carbon composite material, preparation method and lithium ion battery thereof |
| WO2022170346A1 (en) * | 2021-02-04 | 2022-08-11 | Global Graphene Group, Inc. | Elastic flame-retardant polymer-encapsulated anode particles for lithium batteries and method of manufacturing |
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