CN111362259A - Limit low specific surface area lithium ion battery negative electrode material and preparation method thereof - Google Patents
Limit low specific surface area lithium ion battery negative electrode material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a lithium ion battery cathode material with a limited low specific surface area. The material is realized by carrying out surface repair on the graphite material twice, and the first repair is realized by mixing with a hard carbon precursor material before the material is graphitized, so that the heat treatment step of the repair process is combined with the graphitization process of the material, the process and the manufacturing cost of the material are simplified, and the surface repair effect is preliminarily achieved; and after the graphitization process, the material is repaired in a gas-phase accurate and uniform repairing mode for the second time, so that the defects on the surface of the graphite material are completely filled. The invention has the advantages that the activity of the graphite material at normal temperature is ensured, and simultaneously, the activity of the graphite material at high temperature is improved, so that the high-temperature use range of the battery is further improved, and the safety performance of the battery is further improved.
Description
Technical Field
The invention relates to the field of lithium ion batteries, in particular to a lithium ion battery cathode material with a limited low specific surface area and a preparation method thereof.
Background
Lithium ion battery is full of lithium ion batteries in the market at present, and the fields related to the lithium ion battery comprise high-end digital products, power automobiles and the like. However, the use temperature (especially high temperature) of lithium ion batteries has great limitations, such as Apple brand mobile electronic products, the optimum operating temperature specified by the official website is 0 ℃ to 35 ℃, and particular emphasis is placed on avoiding the devices from being in a place with an ambient temperature higher than 35 ℃, otherwise the battery capacity is permanently damaged. The temperature impact of the safety requirement of lithium ion storage batteries for electric vehicles is 85 +/-2 ℃ under the extremely high temperature condition of lithium ion battery pack or system test. The limitation of the high temperature of the lithium ion battery is a main factor limiting the wider application of the lithium ion battery, and becomes one of the key technologies for the development of the lithium ion battery.
In view of the electrolyte, many researchers raise the decomposition temperature of the electrolyte by adjusting the solvent system of the electrolyte and/or adding a catalyst so as to raise the high-temperature service temperature of the battery. As documented in Yi's efforts (phosphate-coated LiNi)1/3Co1/3Mn1/3O2Preparation and performance research of the material, 6 months in 2013), high-temperature electrolyte salt is developed by adding functional groups on the surface of the electrolyte salt for modification, and a flame-retardant organic solvent, an ionic liquid and a flame-retardant additive are added into the electrolyte, so that the high-temperature usability of the electrolyte is improved. However, this only solves the high temperature response capability of the electrolyte, but still cannot avoid the side reaction between the electrode material, especially the carbon negative electrode material, and the electrolyte under high temperature conditions.
Disclosure of Invention
The scheme provided by the invention is improved from the aspect of electrode materials, and the occurrence of side reactions is reduced by reducing the specific surface area of the electrode materials and reducing the reaction interface between the electrode materials and the electrolyte, so that the overall high-temperature adaptability of the lithium ion battery can be better improved. The invention aims to improve the high-temperature cycle performance of a carbon negative electrode material, and provides a negative electrode material which keeps the activity level of a conventional negative electrode material at normal temperature and improves the activity at high temperature so as to improve the high-temperature applicability of a lithium ion battery.
According to the invention, the particle size distribution, the specific surface area and the morphology of the negative electrode material are controlled, so that the activity of the section of the graphite crystal is changed, the reaction interface between the graphite material and the electrolyte is reduced, and a stable SEI film is formed.
In order to achieve the purpose, the technical scheme of the invention is as follows: provides a limit low specific surface area lithium ion battery cathode material, which has a specific surface area of 0.1-1m2Graphite material per gram.
The preparation method of the anode material comprises the following steps: the graphite negative electrode material with limited low specific surface area is realized by carrying out surface repair on the graphite material twice. Specifically, the first repair of the method is realized by mixing with a hard carbon precursor material before graphitization of the material, so that the heat treatment step of the repair process is combined with the graphitization process of the material, the process and the manufacturing cost of the material are simplified, and the surface repair effect is preliminarily achieved; after the graphitization process, the material is repaired in a gas-phase accurate and uniform repairing mode for the second time, so that the defects on the surface of the graphite material are completely filled; in addition, the method of the present invention also reduces the specific surface area of the starting material by primarily treating the carbon raw material to increase the degree of spheroidization. Finally, the specific surface area of the anode material of the present invention is made nearly extremely low.
The specific preparation method comprises the following steps:
(1) mixing a carbon material raw material, which is an intermediate phase carbon material prepared from asphalt or a carbon material obtained by performing morphology improvement on coke, with a hard carbon precursor, wherein the mass ratio of the carbon material to the hard carbon precursor is 80: 20-99: 1;
(2) carrying out graphitization treatment on the mixture obtained in the step (1) to obtain a graphite material;
(3) introducing carbon gas and protective gas into the graphite material obtained in the step (2), and performing gas phase repair in a heat treatment mode;
(4) and (4) stirring/mixing the repaired graphite material obtained in the step (3) (so as to ensure the uniformity of the material), sieving and demagnetizing to finally prepare the lithium ion battery negative electrode material with the limited low specific surface area.
The particle size distribution of the carbon material selected in the step (1) is 2-60 mu m.
In the step (1), medium-temperature coal pitch with the softening point range of 60-120 ℃ and the quinoline insoluble range of 1% -10% is adopted, and the anisotropic intermediate phase carbon material is generated through heat treatment at 300-500 ℃.
And (1) performing morphology improvement on the coke in the step (1) by crushing, grinding and mechanically spheroidizing to prepare the morphology-improved carbon material with spheroidization degree.
The hard carbon precursor in the step (1) comprises: resins, specifically epoxy resin, phenolic resin, polyfurfuryl PFA-C; or organic polymer, such as polyacrylonitrile, polyvinyl alcohol, polystyrene, polyvinylpyrrolidone, polyacrylic acid, and polyvinyl chloride; or a mixture of one or more of these materials.
The temperature of the graphitization treatment in the step (2) is 2500-3200 ℃.
And (3) the carbon gas for gas phase repair in the step (3) is one or more of acetylene, methane and propylene, and the protective gas is one or more of argon or nitrogen.
The volume ratio of the carbon gas to the protective gas in the step (3) is 1:2-1: 10.
And (3) raising the temperature of the gas phase repairing in the step (3) to 600-700 ℃ at the rate of 150-300 ℃/h, and keeping the temperature at the highest temperature for 30-180 min.
The time of the mixing/stirring procedure in the step (4) is 30 min-120 min.
And (4) controlling the temperature of the demagnetizing process in the step (4) to be 50-70 ℃.
In the obtained negative electrode material, the mass ratio of the carbon addition amount of the carbon repairing agent (hard carbon precursor and carbon gas) to the raw material carbon material is 1:20-1: 50.
Further, the invention also provides a lithium ion battery which comprises the negative electrode material with the limited low specific surface area.
The battery of the invention reduces the reaction interface between the graphite material and the electrolyte by reducing the specific surface area of the graphite material to near the limit value. The invention has the advantages that the activity of the graphite material at normal temperature is maintained, and simultaneously, the activity of the graphite material at high temperature is improved, so that the high-temperature use range of the battery is improved, and the safety performance of the battery is further improved.
Drawings
Fig. 1 is a particle size distribution diagram of a limiting low specific surface area anode material prepared in example 1 of the present invention.
Fig. 2 is an SEM image (a) of a graphite material prepared in a reference example of the present invention and an SEM image (b) of a limiting low specific surface area negative electrode material prepared in example 1, in scale bar: 2 μm.
Fig. 3 is an SEM image of the microspherical anode material prepared in example 1 of the present invention, the scale bar: 50 μm.
Fig. 4 is a high temperature cycle plot (cycle temperature 45 ℃) of a graphite material according to a reference example of the present invention and a limited low specific surface area negative electrode material prepared in example 1.
Fig. 5 is a capacity curve of the graphite material of the reference example and the limiting low ratio negative electrode material prepared in example 1.
Detailed Description
The technical solution of the present invention is further described and illustrated by the following specific examples, but the present invention is not limited to the following examples.
Reference example
1) The mesophase carbon material is prepared by adopting medium temperature coal pitch with the softening point of 80 ℃ and 4 percent of pitch quinoline insoluble, the spheroidization temperature is 450 ℃, and the prepared sphere particle size distribution D50 is 25 mu m.
2) The prepared spheres are graphitized at 2800 ℃, the particle size distribution D50 of the graphitized spheres is 25 mu m, and the specific surface area is 2.5m2/g。
3) And mixing the graphitized material for 60min, and demagnetizing to obtain the conventional mesocarbon microbeads.
Example 1
1) The mesophase carbon material is prepared by adopting medium temperature coal pitch with the softening point of 80 ℃ and 4 percent of pitch quinoline insoluble, the spheroidization temperature is 450 ℃, and the prepared sphere particle size distribution D50 is 25.0 mu m.
2) And mixing the carbon material and the phenolic resin, wherein the mass ratio of the intermediate phase carbon material to the phenolic resin is 95: 5.
3) And (3) carrying out graphitization treatment on the carbon material mixed with the hard carbon precursor, wherein the highest graphitization temperature is 2800 ℃.
4) And (2) introducing an acetylene gas source and a nitrogen protective gas into the graphitized graphite material, wherein the volume ratio of the acetylene gas to the nitrogen is 1:8, the heating rate is 200 ℃/h, the temperature is increased to 650 ℃, the temperature is kept for 60min, the graphite material is naturally cooled to below 50 ℃ and taken out of the furnace, and the mass ratio of the graphitized carbon material to the carbon added in the carbon repairing agent is 96:4 through weighing and calculation.
5) And mixing the repaired intermediate phase graphite for 60min, and demagnetizing at 70 ℃. Finally, the microspheric graphite material with ultimate low specific surface area (figure 3) is prepared, the particle size distribution D50 is 24.0 mu m, and the specific surface area is 0.350m2/g。
Example 2
1) The mesophase carbon material is prepared by adopting medium temperature coal pitch with the softening point of 80 ℃ and 4 percent of pitch quinoline insoluble, the spheroidization temperature is 450 ℃, and the prepared sphere particle size distribution D50 is 25.0 mu m.
2) And mixing the intermediate phase carbon material with the phenolic resin, wherein the mass ratio of the intermediate phase carbon material to the phenolic resin is 92: 8.
3) And (3) carrying out graphitization treatment on the carbon material mixed with the hard carbon precursor, wherein the highest graphitization temperature is 2800 ℃.
4) And (2) introducing a methane gas source and a nitrogen protective gas into the graphitized graphite material, wherein the volume ratio of the methane gas to the nitrogen is 1:8, the heating rate is 250 ℃/h, the temperature is increased to 700 ℃, the temperature is kept for 30min, the graphite material is naturally cooled to below 50 ℃ and taken out of the furnace, and the mass ratio of the graphitized carbon material to the carbon added in the carbon repairing agent is 95:5 through weighing and calculation.
5) And mixing the repaired intermediate phase graphite for 100min, and demagnetizing at 60 ℃. Finally, the microspheric graphite material with the ultimate low specific surface area is prepared, the particle size distribution D50 is 24.5 mu m, and the specific surface area is 0.260m2/g。
Example 3
1) Needle coke is adopted to carry out the procedures of crushing, grinding and mechanical spheroidization, and the particle size distribution D50 of the prepared morphology-improved carbon material is 20.0 mu m.
2) Mixing the morphology improving carbon material with phenolic resin, wherein the mass ratio of the morphology improving carbon material to the phenolic resin is 92: 8.
3) And (3) carrying out graphitization treatment on the carbon material mixed with the hard carbon precursor, wherein the highest graphitization temperature is 2800 ℃.
4) And (2) introducing an acetylene gas source and a nitrogen protective gas into the graphitized graphite material, wherein the volume ratio of the acetylene gas to the nitrogen is 1:8, the heating rate is 150 ℃/h, the temperature is increased to 600 ℃, the temperature is kept for 180min, the graphite material is naturally cooled to below 50 ℃ and taken out of the furnace, and the mass ratio of the graphitized carbon material to the carbon added in the carbon repairing agent is 93:7 through weighing and calculation.
5) And mixing the repaired intermediate phase graphite for 40min, and demagnetizing at 60 ℃. Finally, the microspheric graphite material with the ultimate low specific surface area is prepared, the particle size distribution D50 is 22.0 mu m, and the specific surface area is 0.475m2/g。
Fig. 1 is a particle size distribution diagram of the material prepared in example 1, wherein D50 of the material is 24 μm, and the surface of the b-diagram after the material is repaired is observed to be smoother compared with the a-diagram in fig. 2, and fig. 4 is a high-temperature cycle of the button cell (the counter electrode is a lithium sheet) of the material prepared in example 1 under the condition of 45 ℃, compared with the button cell of the reference example formed in the same way, the high-temperature cycle performance of the material can be improved from 92% to 97% by reducing the specific surface area of the material through surface modification, and meanwhile, the particle size distribution diagram is confirmed by fig. 5: at room temperature, when the two batteries in fig. 4 are used for specific capacity-voltage tests, the first discharge capacity of the battery made of the material in example 1 is still 338mAh/g, which is equivalent to 340mAh/g of the battery in the reference example.
The embodiments described above were chosen and described in order to best explain the principles of the invention, but are not intended to be exhaustive or to limit the invention to the precise forms disclosed, and many modifications and variations are possible to those skilled in the art to best utilize the invention, the scope of which is defined by the appended claims.
Claims (12)
1. AThe lithium ion battery cathode material with limited low specific surface area is characterized in that the cathode material has a specific surface area of 0.1-1m2Graphite material per gram.
2. The negative electrode material of claim 1, wherein the negative electrode material is prepared by a method comprising:
(1) mixing an intermediate phase carbon material prepared from asphalt or a carbon material with improved morphology by using cokes as a carbon material with a hard carbon precursor, wherein the mass ratio of the carbon material to the hard carbon precursor is 80: 20-99: 1;
(2) carrying out graphitization treatment on the mixture obtained in the step (1) to obtain a graphite material;
(3) introducing carbon gas and protective gas into the graphite material obtained in the step (2), and performing gas phase repair in a heat treatment mode;
(4) and (4) carrying out stirring, mixing, sieving and demagnetizing on the repaired graphite material obtained in the step (3) to finally obtain the negative electrode material.
3. The anode material according to claim 1 or 2, wherein the hard carbon precursor in the step (1) comprises: resins, organic polymers or mixtures thereof.
4. The negative electrode material as claimed in claim 3, wherein the resin is selected from one or more of epoxy resin, phenolic resin, polyfurfuryl PFA-C; the organic polymer is selected from one or more of polyacrylonitrile, polyvinyl alcohol, polystyrene, polyvinylpyrrolidone, polyacrylic acid and polyvinyl chloride.
5. The negative electrode material according to any one of claims 1 to 4, wherein the temperature of the graphitization treatment in the step (2) is 2500 ℃ to 3200 ℃.
6. The negative electrode material of any one of claims 1 to 5, wherein the carbon gas in the step (3) is one or more of acetylene, methane and propylene, and the protective gas is one or a mixture of argon and nitrogen.
7. The anode material according to any one of claims 1 to 6, wherein a volume ratio of the carbon gas to the protective gas in the step (3) is 1:2 to 1: 10.
8. The negative electrode material of any one of claims 1 to 7, wherein the temperature rise rate of the gas phase repairing in the step (3) is 150 ℃ to 300 ℃/h, the temperature rises to 600 ℃ to 700 ℃, and the maximum temperature holding time is 30min to 180 min.
9. The negative electrode material of any one of claims 1 to 8, wherein the stirring and mixing time in the step (4) is 30 to 120 min; the temperature of the demagnetizing process is controlled to be 50-70 ℃.
10. The negative electrode material according to any one of claims 1 to 10, wherein a mass ratio of an amount of carbon added as a carbon-based repair agent to a raw material carbon material is 1:20 to 1:50, and the carbon-based repair agent refers to the hard carbon precursor and the carbon gas.
11. A preparation method of a lithium ion battery negative electrode material with a limited low specific surface area, which is characterized in that the negative electrode material is the lithium ion battery negative electrode material with the limited low specific surface area according to claims 1-10, and the method specifically comprises the following steps:
(1) mixing an intermediate phase carbon material prepared from asphalt or a carbon material with improved morphology by using cokes as a carbon material with a hard carbon precursor, wherein the mass ratio of the carbon material to the hard carbon precursor is 80: 20-99: 1;
(2) carrying out graphitization treatment on the mixture obtained in the step (1) to obtain a graphite material;
(3) introducing carbon gas and protective gas into the graphite material obtained in the step (2), and performing gas phase repair in a heat treatment mode;
(4) and (4) carrying out stirring, mixing, sieving and demagnetizing on the repaired graphite material obtained in the step (3) to finally obtain the negative electrode material.
12. A lithium ion battery, characterized in that the battery comprises a limiting low specific surface area lithium ion battery negative electrode material according to claims 1-10.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103199254A (en) * | 2013-04-03 | 2013-07-10 | 深圳市贝特瑞新能源材料股份有限公司 | Graphite negative material of lithium-ion battery and preparation method of negative material |
| CN107369823A (en) * | 2017-07-25 | 2017-11-21 | 广东海洋大学 | A kind of lithium ion battery artificial composite cathode material of silicon/carbon/graphite and preparation method thereof |
| CN107507979A (en) * | 2016-06-14 | 2017-12-22 | 上海杉杉科技有限公司 | A kind of preparation method of high jolt ramming artificial plumbago negative pole material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103199254A (en) * | 2013-04-03 | 2013-07-10 | 深圳市贝特瑞新能源材料股份有限公司 | Graphite negative material of lithium-ion battery and preparation method of negative material |
| CN107507979A (en) * | 2016-06-14 | 2017-12-22 | 上海杉杉科技有限公司 | A kind of preparation method of high jolt ramming artificial plumbago negative pole material |
| CN107369823A (en) * | 2017-07-25 | 2017-11-21 | 广东海洋大学 | A kind of lithium ion battery artificial composite cathode material of silicon/carbon/graphite and preparation method thereof |
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