CN113955750A - Preparation method of artificial graphite and lithium ion battery - Google Patents
Preparation method of artificial graphite and lithium ion battery Download PDFInfo
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Abstract
The invention discloses a preparation method of artificial graphite and a lithium ion battery. The preparation method of the artificial graphite comprises the following steps: s10, graphitizing the raw coke powder to obtain an intermediate; s20, uniformly mixing the second raw material and the intermediate to obtain a composite precursor; s30, carbonizing the composite precursor at 900-1400 ℃ under the protection of protective gas to obtain artificial graphite; wherein the second raw material comprises a liquid phase coating agent. The appearance of the surface of the artificial graphite can be effectively improved through liquid phase coating, the specific surface area is reduced, the active sites of side reactions are reduced, gas generation of the lithium ion battery is reduced, the volume expansion is reduced, and the safety performance of the lithium ion battery is improved; in addition, the artificial graphite prepared by graphitization treatment and coating is better in liquid absorption performance, so that the internal resistance is reduced, the low-temperature performance is improved, the reduction of the internal resistance is beneficial to the movement of lithium ions, and the prepared lithium ion battery is better in quick charge performance.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a preparation method of artificial graphite and a lithium ion battery.
Background
The new energy automobile industry is well accepted by national policies and markets, and the lithium ion battery is a core energy component of the new energy automobile industry and has the advantages of environmental friendliness. Along with the popularization of new energy vehicles and charging piles, the high-speed development of science and technology and the continuous improvement of living standard, people have higher requirements on the quick charging performance and the safety performance of batteries. The fast charge and safety performance of the lithium ion battery mainly depends on the performance of the material, and the negative electrode material plays an important role in the material.
The graphite cathode material has the advantages of high cycle efficiency, good cycle performance, rich resources, low price and the like, and is an ideal cathode material of the lithium ion battery. However, the common single-particle artificial graphite powder has irregular shape, large specific surface area and high anisotropy, which leads to poor material processing performance, easy expansion in the using process and poor dynamic performance of lithium ion transportation, thereby causing poor quick charge performance and safety performance of the lithium ion battery.
Disclosure of Invention
The invention mainly aims to provide a preparation method of artificial graphite and a lithium ion battery, and aims to provide a negative electrode material capable of improving the safety performance and the quick charge performance of lithium ions.
In order to achieve the purpose, the invention provides a preparation method of artificial graphite, which comprises the following steps:
s10, graphitizing the raw coke powder to obtain an intermediate;
s20, uniformly mixing the second raw material with the intermediate to obtain a composite precursor;
s30, carbonizing the composite precursor at 900-1400 ℃ under the protection of protective gas to obtain artificial graphite;
wherein the second raw material comprises a liquid phase coating agent.
Optionally, before step S10, the method further includes the following steps:
and (3) crushing and shaping the raw coke to obtain raw coke powder.
Optionally, the particle size of the raw coke powder is 4-15 μm; and/or the presence of a gas in the gas,
the raw coke powder includes at least one of needle coke and petroleum coke.
Optionally, the temperature of the graphitization treatment is 2800-3200 ℃.
Optionally, the second raw material further comprises a conductive agent.
Optionally, in the second raw material, the mass fraction of the conductive agent is not higher than 50%; and/or the presence of a gas in the gas,
the conductive agent includes at least one of carbon black, carbon nanotubes, and graphene paste.
Optionally, the liquid phase coating agent comprises at least one of coal tar, bitumen oil, and liquid pitch.
Optionally, the mass ratio of the second raw material to the intermediate is 1-10: 90-99 parts.
Optionally, the carbonization treatment time is 4-24 h.
Furthermore, the invention also provides a lithium ion battery, wherein the negative electrode material in the lithium ion electrode comprises graphite, and the graphite is prepared by the preparation method of the artificial graphite.
According to the technical scheme provided by the invention, the raw material coke powder is graphitized to obtain an intermediate, the intermediate and a second raw material are uniformly mixed, a liquid-phase coating agent is coated on the intermediate, and finally, the artificial graphite is obtained through carbonization, the surface morphology of the artificial graphite can be effectively improved through liquid-phase coating, the specific surface area is reduced, the active sites of side reactions are reduced, so that the side reactions are reduced, the gas production of the lithium ion battery is reduced, the volume expansion is reduced, and the safety performance of the lithium ion battery is improved; in addition, the artificial graphite prepared by graphitization treatment and coating is better in liquid absorption performance, so that the internal resistance is reduced, the low-temperature performance is improved, the reduction of the internal resistance is beneficial to the movement of lithium ions, and the prepared lithium ion battery is better in quick charge performance.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other related drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic flow chart illustrating an embodiment of a method for preparing artificial graphite according to the present invention;
FIG. 2 is a scanning electron micrograph of the artificial graphite obtained in example 1 of the present invention.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In addition, the meaning of "and/or" appearing throughout includes three juxtapositions, exemplified by "A and/or B" including either A or B or both A and B. In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The graphite cathode material has the advantages of high cycle efficiency, good cycle performance, rich resources, low price and the like, and is an ideal cathode material of the lithium ion battery. However, the common single-particle artificial graphite powder has irregular shape, large specific surface area and high anisotropy, which leads to poor material processing performance, easy expansion in the using process and poor dynamic performance of lithium ion transportation, thereby causing poor quick charge performance and safety performance of the lithium ion battery.
In view of the above, the present invention provides a method for preparing artificial graphite, which in one embodiment comprises the following steps:
step S10, graphitizing the raw coke powder to obtain an intermediate;
step S20, uniformly mixing the second raw material and the intermediate to obtain a composite precursor;
and S30, carbonizing the composite precursor at 900-1400 ℃ under the protection of protective gas to obtain the artificial graphite.
In the embodiment, the particle size of the raw coke powder is 4-15 μm, and the raw coke with a small particle size can shorten the channel resistance of lithium ions entering graphite layers, so that the prepared artificial graphite has more excellent rate capability and low-temperature performance. Wherein the temperature of the graphitization treatment is 2800-3200 ℃.
In one embodiment, the powdered raw coke comprises at least one of needle coke and petroleum coke, and the needle coke and the petroleum coke are easily available and low in cost.
The present invention is not limited to the source of the raw coke powder, and the raw coke powder may be obtained by direct purchase or may be prepared by itself, and in this embodiment, the method further includes the following steps before step S10:
and A1, crushing and shaping the raw coke to obtain raw coke powder.
It is understood that the raw coke is at least one of needle coke and petroleum coke.
Wherein the second raw material comprises a liquid phase coating agent. Further, the liquid phase coating agent comprises at least one of coal tar, asphalt oil and liquid asphalt.
In step S30, the mass ratio of the second raw material to the intermediate is 1 to 10: 90-99 parts. Wherein the shielding gas comprises any one of helium, nitrogen and argon. In order to improve the effect of the carbonization treatment, in the present embodiment, the time of the carbonization treatment is 4 to 24 hours.
According to the technical scheme provided by the invention, the raw material coke powder is graphitized to obtain an intermediate, the intermediate and a second raw material are uniformly mixed, a liquid-phase coating agent is coated on the intermediate, and finally, the artificial graphite is obtained through carbonization, the surface morphology of the artificial graphite can be effectively improved through liquid-phase coating, the specific surface area is reduced, the active sites of side reactions are reduced, so that the side reactions are reduced, the gas production of the lithium ion battery is reduced, the volume expansion is reduced, and the safety performance of the lithium ion battery is improved; in addition, the artificial graphite prepared by graphitization treatment and coating is better in liquid absorption performance, so that the internal resistance is reduced, the low-temperature performance is improved, the reduction of the internal resistance is beneficial to the movement of lithium ions, and the prepared lithium ion battery is better in quick charge performance.
In another embodiment, the second raw material further comprises a conductive agent, and the addition of the conductive agent is beneficial to the movement of electrons, so that the prepared artificial graphite has good electron and lithium ion conductivity, and the high-rate charge-discharge effect is good, thereby further improving the charge-discharge performance of the lithium ion battery; in addition, the internal resistance can be further reduced by adding the conductive agent, so that the heat productivity is reduced, and the safety performance of the conductive agent is further improved.
Further, in the second raw material, the mass fraction of the conductive agent is not higher than 50%. Wherein the conductive agent comprises at least one of carbon black, carbon nanotubes, and graphene paste.
The invention does not limit the concrete implementation mode of uniformly mixing the liquid phase coating agent, the conductive agent and the intermediate, and only needs to be uniformly mixed. In order to facilitate the mixing and achieve a better mixing effect, in this embodiment, the liquid-phase conductive agent and the liquid-phase coating agent are first mixed uniformly and then mixed with the intermediate. Specifically, in the present embodiment, step S20 includes the following steps:
step S21, uniformly mixing the liquid phase coating agent and the conductive agent to obtain a second raw material;
and step S22, uniformly mixing the second raw material and the intermediate to obtain the composite precursor.
At present, the scheme of preparing the artificial graphite by coating, carbonizing and graphitizing raw materials at first exists, the prepared artificial graphite is all graphite from inside to outside, belongs to a crystal structure, and has high capacity and high compaction, but the liquid absorption performance is poor. In the invention, the raw materials are graphitized, and then the amorphous carbon layer of the conductive agent is uniformly distributed on the graphitized surface by a liquid phase coating method, so that a good conductive coating network is constructed, the prepared artificial graphite can effectively reduce the diffusion resistance of lithium ions in the material and the surface polarization of particles, and meanwhile, the electronic conductivity is improved, the internal resistance of the material is reduced, and the power, the multiplying power, the circulation, the safety and other properties of the prepared lithium ion battery are obviously improved. Specifically, the index parameters of the prepared artificial graphite are that the particle size D50 is 6-20 mu m, and the specific surface is less than or equal to 2.0m2G, gram capacity is more than or equal to 350mAh/g, and compaction density is more than or equal to 1.60g/cm3The capacity retention rate is more than or equal to 80 percent at the normal temperature in a cycle of 5C/5C for 2000 weeks.
In addition, at present, there is also a method of performing graphitization treatment on the raw material to obtain a graphitized substrate, and then depositing amorphous carbon on the surface of the graphitized substrate through vapor deposition. In the invention, through the design of the second raw material and the proportion of the raw materials, the artificial graphite with excellent comprehensive performance can be prepared by a simple liquid phase coating method.
Furthermore, the invention also provides a lithium ion battery, wherein the negative electrode material in the lithium ion electrode comprises graphite, and the graphite is prepared by the preparation method of the artificial graphite. The specific structure of the artificial graphite refers to the above embodiments, and since the lithium ion battery of the present invention adopts all the technical solutions of all the above embodiments, at least all the beneficial effects brought by the technical solutions of the above embodiments are achieved, and no further description is given here.
The technical solutions of the present invention are further described in detail below with reference to specific examples and drawings, it should be understood that the following examples are merely illustrative of the present invention and are not intended to limit the present invention.
Example 1
(1) And (3) putting the needle coke into a mechanical crushing and shaping machine for crushing and shaping to obtain needle coke powder, wherein the particle size D50 of the needle coke powder is 6 mu m.
(2) Graphitizing needle coke powder in an Acheson furnace at high temperature to obtain an intermediate, wherein the graphitization temperature is 3000 ℃.
(3) And (2) stirring and mixing a liquid phase coating agent (a mixture of coal tar and asphalt oil) and a conductive agent (carbon nano tube) at a high speed in a container, wherein the mass ratio of the liquid phase coating agent to the conductive agent is 1:1 (namely the mass fraction of the conductive agent is 50%), and obtaining a second raw material after compounding.
(4) And (3) mixing the intermediate and the second raw material in a mixer at a high speed in a nitrogen atmosphere, wherein the mass ratio of the second raw material to the intermediate is 5: and 95, obtaining the composite precursor.
(5) And carbonizing the composite precursor at 1000 ℃ for 12h in a nitrogen atmosphere to finally obtain the artificial graphite.
Example 2
(1) And (3) putting the needle coke into a mechanical grinding and shaping machine for grinding and shaping to obtain needle coke powder, wherein the particle size D50 of the needle coke powder is 10 mu m.
(2) Graphitizing needle coke powder in an Acheson furnace at high temperature to obtain an intermediate, wherein the graphitization temperature is 3000 ℃.
(3) And (2) stirring and mixing the liquid phase coating agent (liquid asphalt) and the conductive agent (carbon black) at a high speed in a container, wherein the mass ratio of the liquid phase coating agent to the conductive agent is 6:4 (namely the mass fraction of the conductive agent is 40%), and obtaining a second raw material after compounding.
(4) And (3) mixing the intermediate and the second raw material in a mixer at a high speed in a nitrogen atmosphere, wherein the mass ratio of the second raw material to the intermediate is 8: 92, obtaining the composite precursor.
(5) And carbonizing the composite precursor at 1200 ℃ for 16h in a nitrogen atmosphere to finally obtain the artificial graphite.
Example 3
(1) Putting raw coke (mixture of needle coke and petroleum coke) into a mechanical grinding and shaping machine for grinding and shaping to obtain raw coke powder, wherein the granularity D50 of the raw coke powder is 12 mu m.
(2) Graphitizing the raw material coke powder in an Acheson furnace at high temperature to obtain an intermediate, wherein the graphitization temperature is 3200 ℃.
(3) And (2) stirring and mixing a liquid phase coating agent (a mixture of liquid asphalt and asphalt oil) and a conductive agent (graphene slurry) at a high speed in a container, wherein the mass ratio of the liquid phase coating agent to the conductive agent is 6:4 (namely the mass fraction of the conductive agent is 40%), and obtaining a second raw material after compounding.
(4) And (2) mixing the intermediate and the second raw material in a mixer at a high speed in a nitrogen atmosphere, wherein the mass ratio of the second raw material to the intermediate is 10: and 90, obtaining the composite precursor.
(5) And carbonizing the composite precursor at 1400 ℃ for 20h in a nitrogen atmosphere to finally obtain the artificial graphite.
Example 4
(1) And (3) putting the needle coke into a mechanical grinding and shaping machine for grinding and shaping to obtain needle coke powder, wherein the particle size D50 of the needle coke powder is 12 mu m.
(2) Graphitizing needle-shaped coke powder in an Acheson furnace at high temperature to obtain an intermediate, wherein the graphitization temperature is 3200 ℃.
(3) And (2) stirring and mixing the liquid phase coating agent (coal tar) and the conductive agent (the mixture of the carbon nano tube and the carbon black) at a high speed in a container, wherein the mass ratio of the liquid phase coating agent to the conductive agent is 1:1 (namely the mass fraction of the conductive agent is 50%), and obtaining a second raw material after compounding.
(4) And (2) mixing the intermediate and the second raw material in a mixer at a high speed in a nitrogen atmosphere, wherein the mass ratio of the second raw material to the intermediate is 10: and 90, obtaining the composite precursor.
(5) And carbonizing the composite precursor at 1400 ℃ for 24h in a nitrogen atmosphere to finally obtain the artificial graphite.
Example 5
(1) And (3) putting the needle coke into a mechanical grinding and shaping machine for grinding and shaping to obtain needle coke powder, wherein the particle size D50 of the needle coke powder is 12 mu m.
(2) Graphitizing needle-shaped coke powder in an Acheson furnace at high temperature to obtain an intermediate, wherein the graphitization temperature is 3200 ℃.
(4) And (2) mixing the intermediate and a second raw material (coal tar) at a high speed in a mixer under the nitrogen atmosphere, wherein the mass ratio of the second raw material to the intermediate is 10: and 90, obtaining the composite precursor.
(5) And carbonizing the composite precursor at 1400 ℃ for 24h in a nitrogen atmosphere to finally obtain the artificial graphite.
Example 6
(1) And (3) putting the petroleum coke into a mechanical grinding and shaping machine for grinding and shaping to obtain petroleum coke powder, wherein the granularity D50 of the raw material coke powder is 4 mu m.
(2) Graphitizing petroleum coke powder in an Acheson furnace at high temperature to obtain an intermediate, wherein the graphitization temperature is 3200 ℃.
(3) And (2) stirring and mixing the liquid phase coating agent (coal tar) and the conductive agent (the mixture of the carbon nano tube and the carbon black) at a high speed in a container, wherein the mass ratio of the liquid phase coating agent to the conductive agent is 1:1 (namely the mass fraction of the conductive agent is 50%), and obtaining a second raw material after compounding.
(4) And (3) mixing the intermediate and the second raw material in a mixer at a high speed in a nitrogen atmosphere, wherein the mass ratio of the second raw material to the intermediate is 1: and 90, obtaining the composite precursor.
(5) And carbonizing the composite precursor at 1400 ℃ for 4h in a nitrogen atmosphere to finally obtain the artificial graphite.
Example 7
Except that step (5) is changed to: the composite precursor was carbonized at 900 ℃ for 24 hours under argon atmosphere, and the rest of the procedure was the same as in example 6.
The artificial graphite materials prepared in examples 1 to 5 were subjected to coating, rolling, slitting, winding, and the like to complete the production of a flexible-package battery cell (i.e., a battery cell, i.e., a lithium ion battery cell without a protective circuit board), and the physical properties of the materials and the electrochemical properties of the battery cell were tested (the capacity of the battery cell was 2.0Ah), and the results are shown in table 1.
Table 1 results of performance testing
As can be seen from Table 1, the particle size D50 of the artificial graphite obtained in examples 1 to 5 was 6 to 20 μm, and the specific surface area was not more than 2.0m2G, gram capacity is more than or equal to 350mAh/g, and compaction density is more than or equal to 1.60g/cm3The capacity retention rate at the normal temperature of 2000 cycles at 5C/5C is more than or equal to 80%, and the lithium ion battery prepared in the embodiment 1-4 shows that the internal resistance of the battery core is smaller, the capacity retention rate at 2000 cycles at 5C/5C is higher, the larger the particle size is, the smaller the specific surface area is, the smaller the expansion rate of gas generated at the high temperature of 60 ℃ is, and after the particle size is larger to a certain degree, the specific surface area and the expansion rate of gas generated at the high temperature of 60 ℃ are not reduced. As can be seen from examples 3 to 5, in example 5 without the conductive agent, compared with examples 3 and 4 with the conductive agent, the lithium ion battery prepared in example 5 has larger cell internal resistance and gas generation expansion rate, and smaller capacity retention rate after 2000 cycles.
FIG. 2 is a schematic view of the artificial graphite obtained in example 1, which is observed under a scanning electron microscope, and the conductive coating layer is clearly observed from FIG. 2.
It should be noted that the principles of examples 6 and 7 are similar to those of examples 1 to 4, and the parameters are within the scope of the present invention, so that the properties of the artificial graphite obtained are similar to those of examples 1 to 4.
In conclusion, the amorphous carbon layer is coated by the liquid phase coating method, so that the diffusion resistance of lithium ions in the material and the surface polarization of particles can be effectively reduced, the electronic conductivity is improved, the internal resistance of the material is reduced, the power, the multiplying power, the circulation and the safety performance are obviously improved, and various index requirements of a power market can be met; the conductive agent is uniformly distributed in the amorphous carbon layer, so that the internal resistance can be further reduced, the cycle performance can be improved, and the amorphous carbon layer has a good market application prospect.
The above is only a preferred embodiment of the present invention, and it is not intended to limit the scope of the invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall be included in the scope of the present invention.
Claims (10)
1. The preparation method of the artificial graphite is characterized by comprising the following steps:
s10, graphitizing the raw coke powder to obtain an intermediate;
s20, uniformly mixing the second raw material with the intermediate to obtain a composite precursor;
s30, carbonizing the composite precursor at 900-1400 ℃ under the protection of protective gas to obtain artificial graphite;
wherein the second raw material comprises a liquid phase coating agent.
2. The method of preparing artificial graphite according to claim 1, further comprising, before step S10, the steps of:
and (3) crushing and shaping the raw coke to obtain raw coke powder.
3. The method for preparing artificial graphite according to claim 1, wherein the particle size of the raw coke powder is 4 to 15 μm; and/or the presence of a gas in the gas,
the raw coke powder includes at least one of needle coke and petroleum coke.
4. The method for preparing artificial graphite according to claim 1, wherein the graphitization treatment temperature is 2800 to 3200 ℃.
5. The method of preparing artificial graphite according to claim 1, wherein the second raw material further comprises a conductive agent.
6. The method for producing artificial graphite according to claim 5, wherein the mass fraction of the conductive agent in the second raw material is not more than 50%; and/or the presence of a gas in the gas,
the conductive agent includes at least one of carbon black, carbon nanotubes, and graphene paste.
7. The method of preparing artificial graphite according to claim 1, wherein the liquid phase coating agent includes at least one of coal tar, pitch oil, and liquid pitch.
8. The method for preparing artificial graphite according to claim 1, wherein the mass ratio of the second raw material to the intermediate is 1-10: 90-99 parts.
9. The method for preparing artificial graphite according to claim 1, wherein the carbonization time is 4 to 24 hours.
10. A lithium ion battery, wherein the negative electrode material of the lithium ion battery comprises graphite, and the graphite is prepared by the preparation method of the artificial graphite according to any one of claims 1 to 9.
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| CN115010127A (en) * | 2022-07-20 | 2022-09-06 | 晖阳(贵州)新能源材料有限公司 | Preparation method of high-rate lithium ion battery negative electrode material |
| CN117361519A (en) * | 2023-10-23 | 2024-01-09 | 万向一二三股份公司 | Preparation method of graphite anode material |
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| CN113213470A (en) * | 2021-05-07 | 2021-08-06 | 上海杉杉新材料有限公司 | Artificial graphite secondary particle, coating agent, preparation method and application thereof |
Cited By (2)
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| CN115010127A (en) * | 2022-07-20 | 2022-09-06 | 晖阳(贵州)新能源材料有限公司 | Preparation method of high-rate lithium ion battery negative electrode material |
| CN117361519A (en) * | 2023-10-23 | 2024-01-09 | 万向一二三股份公司 | Preparation method of graphite anode material |
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