CN114050264A - Negative electrode material and negative plate containing same - Google Patents
Negative electrode material and negative plate containing same Download PDFInfo
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- CN114050264A CN114050264A CN202111350744.2A CN202111350744A CN114050264A CN 114050264 A CN114050264 A CN 114050264A CN 202111350744 A CN202111350744 A CN 202111350744A CN 114050264 A CN114050264 A CN 114050264A
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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
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/205—Preparation
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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
-
- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on 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
- H01M4/36—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
- 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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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 provides a negative electrode material and a negative electrode sheet containing the same. The invention satisfies D by controlling the particle size distribution of the cathode materialV99And DV50Ratio D ofV99/DV502 to 2.6; by designing the thickness (D) of the negative electrode active material layer to be suitable for the particle diameter distributionV50X 9.8 is not less than the thickness of the negative electrode active material layer≥DV99X 3.4) to achieve the optimal pole piece design, and ensure the particle integrity under the high-compaction-density negative pole to improve the cycle performance. The size of the large particles is controlled to ensure that local expansion abnormality caused by local overpressure under high compaction density, so that high volume energy density is realized, and the requirement of long-cycle low expansion can be met.
Description
Technical Field
The invention belongs to the field of lithium ion batteries, and particularly relates to a negative electrode material and a negative plate containing the same.
Background
In recent years, with the increasing of energy density of lithium ion batteries, the use compaction density of a negative electrode material is gradually increased, so that the expansion of the batteries is increased in a long cycle process, and finally, the interface of the batteries is damaged, and the lithium ion batteries fail. It is therefore necessary to investigate the design anew for the negative electrode material of a high energy density battery.
Disclosure of Invention
The invention provides a negative electrode material and a negative electrode sheet comprising the same, aiming at solving the problems that a lithium ion battery assembled by the conventional negative electrode material is low in energy density and large in expansion rate of the battery in a long-cycle process. The negative electrode material is obtained by coating graphite, and the lithium ion battery with high energy density and long cycle performance is obtained by regulating the particle size of the negative electrode material, regulating the thickness of the negative electrode active material layer of the negative electrode sheet and regulating the ratio (OI value) of the peak intensity of the (004) surface and the peak intensity of the (110) surface of the negative electrode active material layer of the negative electrode sheet.
The purpose of the invention is realized by the following technical scheme:
the negative electrode material is graphite coated with amorphous carbon, and the volume distribution D of the negative electrode materialV99And DV50Ratio D ofV99/DV502 to 2.6.
According to an embodiment of the present invention, when DV99/DV50When the thickness is more than 2.6, in the rolling process of the formed negative plate, large particles can cause uneven pore distribution at local parts on the surface of the negative plate due to overpressure and uneven lithium embedding at local parts, so that the inconsistent expansion of the particles is influenced, and finally the thickness of the battery is deteriorated, so that the performance of the battery is sharply reduced; when D is presentV99/DV50When the particle size distribution of the negative electrode material is less than 2, the particle size distribution of the negative electrode material is too narrow, and the compacted density of the negative electrode material is significantly reduced, which affects the energy density of the battery.
According to an embodiment of the present invention, DV99/DV50Measuring D of the negative electrode material with a particle size analyzer, specifically, a laser particle size analyzer such as Malvern-3000 particle size testerV99And DV50Then said D is obtainedV99/DV50。
According to an embodiment of the present invention, D of the anode materialV509 to 15 μm, for example 9, 10, 11, 12, 13, 14 or 15 μm.
According to an embodiment of the present invention, the amorphous carbon layer has a thickness of 50nm to 70 nm.
According to the embodiment of the invention, the powder compaction density of the negative electrode material under the pressure of 5 tons is more than or equal to 1.9 g/cc.
The invention also provides a preparation method of the anode material, which comprises the following steps:
mixing coke and petroleum asphalt, heating in inert atmosphere, granulating, cooling the reaction product to room temperature, and graphitizing at 3000 deg.C to obtain the cathode material.
According to an embodiment of the invention, the coke is selected from at least one of petroleum coke, calcined needle coke, green coke, asphalt mastic.
According to an embodiment of the invention, D of said cokeV506 to 9 mu m.
According to an embodiment of the invention, D of the petroleum pitchV502-5 μm.
According to the embodiment of the invention, the mass ratio of the coke to the petroleum asphalt is (70-90) to (30-10).
According to an embodiment of the invention, the mixing time is between 1 hour and 3 hours.
According to an embodiment of the invention, the temperature of the heat treatment is 600 ℃ to 900 ℃, for example 700 ℃.
According to an embodiment of the present invention, the time of the heat treatment is 12 hours to 18 hours, for example, 15 hours.
According to an embodiment of the invention, the inert atmosphere is selected from at least one of nitrogen, argon.
The invention also provides a negative plate which comprises the negative electrode material.
According to an embodiment of the present invention, the negative electrode sheet includes a negative electrode current collector and a negative electrode active material layer coated on one or both surfaces of the negative electrode current collector, the negative electrode active material layer includes a negative electrode active material, a conductive agent, and a binder, and the negative electrode active material includes the above-described negative electrode material.
According to an embodiment of the present invention, the thickness of the negative electrode active material layer of the negative electrode sheet satisfies the following relational expression: dV50X 9.8 is not less than DV99X 3.4. When the thickness of the negative electrode active material layer is within this range, the lithium ion battery assembled by the negative electrode active material layer can realize high volume energy density and can meet the requirements of long cycle and low expansion.
According to the embodiment of the invention, the ratio (OI value) of the peak intensity of the (004) surface and the peak intensity of the (110) surface of the negative electrode active material layer, which is measured by an X-ray diffraction spectrum of the negative electrode sheet under the compaction of 1.75g/cc, is 8-14. Research shows that if the OI value is larger than 14, the pole piece of the battery expands too much in the thickness direction, and finally the thickness of the whole battery changes greatly and the performance fails. If the OI value is less than 8, the transverse expansion of the battery pole piece is large, which can cause S-shaped deformation and performance failure of the wound battery.
The invention also provides a lithium ion battery which comprises the negative electrode material and/or the negative electrode sheet.
The invention has the beneficial effects that:
the invention provides a negative electrode material and a negative electrode plate containing the same. The invention satisfies D by controlling the particle size distribution of the cathode materialV99And DV50Ratio D ofV99/DV502 to 2.6; by designing the thickness (D) of the negative electrode active material layer to be suitable for the particle diameter distributionV50X 9.8 is not less than DV99X 3.4) to achieve the optimal pole piece design, and ensure the particle integrity under the high-compaction-density negative pole to improve the cycle performance. The size of the large particles is controlled to ensure that local expansion abnormality caused by local overpressure under high compaction density, so that high volume energy density is realized, and the requirement of long-cycle low expansion can be met.
Detailed Description
The present invention will be described in further detail with reference to specific examples. It is to be understood that the following examples are only illustrative and explanatory of the present invention and should not be construed as limiting the scope of the present invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; reagents, materials and the like used in the following examples are commercially available unless otherwise specified.
Preparation example
(1) Preparing a negative electrode material:
will DV50Petroleum coke of 6-9 μm, DV50Petroleum pitch of 3 μm was premixed in a mixer at a mass ratio of 90:10 (corresponding to the negative electrode materials of examples 1 to 21) for 2 hours. And heat-treating at 700 deg.C for 15 hr, granulating, cooling to room temperature, graphitizing at 3000 deg.C, sieving to obtain negative electrode materials with different particle sizes, and mixing to obtain the final product DV50And DV90。
Examples 1 to 48
(1) Preparing a negative plate:
uniformly mixing the negative electrode material prepared in the preparation example, acetylene black serving as a conductive agent, sodium carboxymethyl cellulose (CMC) serving as a thickening agent and Styrene Butadiene Rubber (SBR) serving as a binder according to the mass ratio of 97:1:1:1 to prepare battery negative electrode slurry; uniformly coating the negative electrode slurry on a copper foil of a negative electrode current collector according to the requirements of a comparative example, drying at 85 ℃, and then compacting according to the density of 1.75g/cm3And carrying out cold pressing and splitting to prepare the battery negative plate.
(2) Preparing a positive plate:
uniformly mixing a positive electrode active material lithium cobaltate, a conductive agent acetylene black and a binder polyvinylidene fluoride (PVDF) according to a mass ratio of 97:2:1, and adding the mixture into N-methyl-2-pyrrolidone (NMP) serving as a solvent to prepare positive electrode slurry with certain viscosity; and uniformly coating the positive slurry on a positive current collector aluminum foil, drying at 90 ℃, cold-pressing, splitting to prepare a battery positive pole piece, welding an aluminum tab at the head position, and pasting an insulating adhesive tape at the tab position.
(3) The separator was a commercially available PE-based ceramic separator.
(4) Preparing a roll core: and rolling the positive pole piece, the coated diaphragm, the negative pole piece and the diaphragm containing the coating slurry into a roll core corresponding to the front two-fold positions of the positive and negative pole pieces, packaging the prepared roll core by using an aluminum-plastic film, injecting liquid, sealing, and testing the prepared battery core.
Comparative example
The other operations are the same as those of the above embodiment except that Dv99/Dv50The thickness of the negative electrode active material layer and the OI value were varied, and are shown in table 2.
Table 1 performance parameters of the negative electrode material prepared in the example and its performance test after assembling into a battery
The test method comprises the following steps:
1. particle size testing-a sample of the negative active material is dispersed in a dispersant ethanol, and after 5 minutes of ultrasonic treatment, the sample is added into a Malvern (3000) particle size tester to test the Dv of the negative active material50And Dv99。
An X-ray diffraction pattern tests the ratio of the peak intensity of the battery pole piece at 1.7g/cc compacted density (004) plane to the peak intensity at (110) plane.
3. Thickness test of negative electrode active material layer-unit of measurement in ten-thousandths of a ruler (μm) was used.
4. Battery charge-discharge cycle test-a lithium ion battery was charged to 4.45V at 1C, stopped at 0.02C for 10 minutes, and then discharged to 3.0V at 1C was recorded as one cycle.
5. Cell thickness test-pressure 600g ± 60g was measured using a parallel plate dynamometer for calculation of cell energy density and cyclic expansion.
From examples 1 to 21, it can be seen that the design within the design range of the present invention, the long cycle retention of the battery, and the cycle expansion thickness all exhibited good performance. As the thickness of the negative electrode active material layer of the negative electrode sheet increases, the energy density of the battery gradually increases, and the cycle expansion of the battery increases as the group OI values of different particle diameters increase.
Table 2 comparative examples the performance parameters of the negative electrode materials prepared and their performance tests after assembling into batteries
From the experimental data of examples 5, 6 and 9, it can be found that the thickness of the negative electrode active material layer of the negative electrode sheet is designed to be 90 μm, and the energy density of the battery is close to 720 wh/L; in comparative examples 1 and 2 in which the particle size of the material is not within the particle size control range of the present invention, although the thickness of the negative electrode active material layer is designed to be 90 μm, the energy density is significantly low, and even if the OI value is satisfied, the battery cycle expansion is still large, resulting in a low capacity retention rate. This is because the large particles of comparative example 1 and comparative example 2 were too large, and the rebound of the sheet after rolling and the expansion after charging were both large, eventually affecting the performance of the battery.
As can be seen from examples 16 and 17, the energy density of the battery in which the thickness of the anode active material layer of the anode is designed to be 120 μm within the range of the present invention can reach 760 wh/L; however, the energy density reduction of comparative examples 3 and 4 was close to 10wh/L, because the large particles of comparative examples 3 and 4 were too small, the compaction density of the material was too low, resulting in the case of overpressure in the material made under the same compaction, the capacity exertion of the final battery was too low, and the cycle expansion of the final battery was too large when the spring back became large.
From the experimental data of comparative examples 5 and 6, it can be concluded that although the particle diameter of the material is within the control range, the thickness of the anode active material layer is designed to be outside the control range, and the cycle capacity retention rate and the cycle expansion of the final battery are inferior to those of examples 20 and 21 although the energy density of the final battery is high. This is because the porosity and the tortuosity of the pole piece both affect the polarization of the battery under high compaction density of the negative electrode, and the performance of the battery is significantly reduced when the polarization is increased, so that the particle size of the material and the thickness of the negative electrode active material layer need to be reasonably controlled under high compaction.
Therefore, in order to achieve high energy density and good performance at high compaction density of the negative electrode, the particle size distribution of the material needs to be regulated. The thickness of the negative electrode active material layer corresponding to the particle diameter of the material also needs to be within a certain range in order to exert the optimum performance.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. The negative electrode material is graphite coated with amorphous carbon, and the volume distribution D of the negative electrode materialV99And DV50Ratio D ofV99/DV502 to 2.6.
2. The negative electrode material of claim 1, wherein D of the negative electrode materialV50Is 9-15 μm.
3. The anode material according to claim 1 or 2, wherein the amorphous carbon layer has a thickness of 50nm to 70 nm.
4. The negative electrode material of any of claims 1-3, wherein the negative electrode material has a powder compaction density ≥ 1.9g/cc at 5 ton pressure.
5. A negative electrode sheet comprising the negative electrode material according to any one of claims 1 to 4.
6. The negative electrode sheet according to claim 5, wherein the negative electrode sheet comprises a negative electrode current collector and a negative electrode active material layer coated on one or both surfaces of the negative electrode current collector, the negative electrode active material layer comprising a negative electrode active material, a conductive agent and a binder, the negative electrode active material comprising the negative electrode material according to any one of claims 1 to 4.
7. The negative electrode sheet according to claim 5 or 6, wherein the thickness of the negative electrode active material layer of the negative electrode sheet satisfies the following relational expression: dV50X 9.8 is not less than DV99×3.4。
8. The negative electrode sheet of any one of claims 5 to 7, wherein the negative electrode sheet has an OI value of 8 to 14.
9. A lithium ion battery, wherein the lithium ion battery comprises the negative electrode material of any one of claims 1 to 4 and/or the negative electrode sheet of any one of claims 5 to 8.
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| CN202111350744.2A CN114050264A (en) | 2021-11-15 | 2021-11-15 | Negative electrode material and negative plate containing same |
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| CN202111350744.2A CN114050264A (en) | 2021-11-15 | 2021-11-15 | Negative electrode material and negative plate containing same |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1520621A (en) * | 2001-06-27 | 2004-08-11 | 株式会社三德 | Nonaqueous electrolyte secondary battery-use anode active matter, prodn. method therefor, nonaqueous electrolyte secondary battery, and prodn, method for anode |
| CN108807849A (en) * | 2018-05-16 | 2018-11-13 | 宁德时代新能源科技股份有限公司 | Negative electrode plate and secondary battery containing same |
| CN109449446A (en) * | 2018-10-17 | 2019-03-08 | 宁德时代新能源科技股份有限公司 | Secondary battery |
| CN113437293A (en) * | 2021-06-21 | 2021-09-24 | 宁德新能源科技有限公司 | Negative electrode active material, secondary battery, and electronic device |
| CN113497230A (en) * | 2020-03-20 | 2021-10-12 | 宁德新能源科技有限公司 | Negative electrode active material, and electrochemical device and electronic device using same |
| WO2021217620A1 (en) * | 2020-04-30 | 2021-11-04 | 宁德时代新能源科技股份有限公司 | Negative electrode active material and preparation method therefor, secondary battery, and device including secondary battery |
-
2021
- 2021-11-15 CN CN202111350744.2A patent/CN114050264A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1520621A (en) * | 2001-06-27 | 2004-08-11 | 株式会社三德 | Nonaqueous electrolyte secondary battery-use anode active matter, prodn. method therefor, nonaqueous electrolyte secondary battery, and prodn, method for anode |
| CN108807849A (en) * | 2018-05-16 | 2018-11-13 | 宁德时代新能源科技股份有限公司 | Negative electrode plate and secondary battery containing same |
| CN109449446A (en) * | 2018-10-17 | 2019-03-08 | 宁德时代新能源科技股份有限公司 | Secondary battery |
| CN113497230A (en) * | 2020-03-20 | 2021-10-12 | 宁德新能源科技有限公司 | Negative electrode active material, and electrochemical device and electronic device using same |
| WO2021217620A1 (en) * | 2020-04-30 | 2021-11-04 | 宁德时代新能源科技股份有限公司 | Negative electrode active material and preparation method therefor, secondary battery, and device including secondary battery |
| CN113437293A (en) * | 2021-06-21 | 2021-09-24 | 宁德新能源科技有限公司 | Negative electrode active material, secondary battery, and electronic device |
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