CN113830761A - Preparation method of artificial graphite negative electrode material - Google Patents
Preparation method of artificial graphite negative electrode material Download PDFInfo
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- CN113830761A CN113830761A CN202110938899.1A CN202110938899A CN113830761A CN 113830761 A CN113830761 A CN 113830761A CN 202110938899 A CN202110938899 A CN 202110938899A CN 113830761 A CN113830761 A CN 113830761A
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- 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
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- 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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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention provides a preparation method of an artificial graphite cathode material, the artificial graphite cathode material has a core-shell structure which takes coke powder as a core and a coating binding material as a shell, and the coke powder is crushed to D50Is 11 +/-1 mu m, is uniformly mixed with the coating binding material according to the proportion of 100:0-100:10, and is gradually heated to T at the speed of 3-5 ℃/min under the stirring speed of 10-35rpm1The temperature is used for leading the coating binding material to be fully softened and coated with the coke powder, and then the temperature is continuously increased to T at the speed of 2-3.5 ℃/min2The temperature realizes the carbonization of the coating bonding material, and then the graphitization of the coke powder is completed sequentially through three gradually-increased temperature gradients; by adopting the scheme, the coated bonding material can be uniformly and firmly coatedThe coke powder surface is decorated and protected, the energy density of the battery is improved by improving the tap density of the material, the graphite layer is effectively prevented from falling off, and the cycle performance of the cathode material is improved.
Description
Technical Field
The invention belongs to the technical field of electrode production, and particularly relates to a preparation method of an artificial graphite negative electrode material.
Background
Currently, newly developed lithium ion battery negative electrode materials such as titanium base, tin base, silicon base, nitride and the like have infinite development potential due to excellent performances. However, in terms of current market development, carbon materials are still mainstream in the development of negative electrode material markets for a long time, and particularly, artificial graphite negative electrode materials are of interest to research of various enterprises and scientific research institutions due to the characteristics of good low compatibility with electrolyte, good rate capability, durable cycle stability and the like.
However, the performance of the current artificial graphite cathode material cannot meet the expectations of people for high-end 3C products and new energy vehicles for high capacity and fast charging performance, and therefore, the development of the artificial graphite cathode material and the development process thereof is urgent.
The present invention has been made in view of this situation.
Disclosure of Invention
One of the objectives of the present invention is to provide a method for preparing an artificial graphite negative electrode material, which is to perform graphitization on a negative electrode material having a core-shell structure to obtain an artificial graphite negative electrode material having a core-shell structure with a graphite layer inside and a carbon layer outside, so as to improve the cycle life and charge first efficiency of the negative electrode material.
In order to solve the problems in the prior art, the invention provides a preparation method of an artificial graphite negative electrode material, which comprises the following steps:
s1, mixing the coke powder and the coating binding material to obtain a mixture, and performing gradient heating on the mixture to obtain semi-finished anode material particles;
s2, heating the semi-finished anode material particles to a graphitization temperature in a gradient heating manner to obtain a crude artificial graphite anode material;
and S3, demagnetizing and screening the coarse product of the artificial graphite cathode material to obtain the artificial graphite cathode material.
According to the scheme, the semi-finished negative electrode material particles with the core-shell structure are graphitized to obtain the artificial graphite negative electrode material, so that the carbon layer coated on the surface of the artificial graphite is more uniform.
Further, in the step S1, the pulverized coke is mixed with a coating binder, and the semi-finished particles of the negative electrode material with the core-shell structure are obtained through a heating coating process and a carbonization process in an inert atmosphere.
According to the scheme, coating and carbonization are carried out in an inert atmosphere, so that the contact between the coating binding material and oxygen in the carbonization process is fully avoided, and the influence on the integrity of the core-shell structure due to nonuniform oxidation coating is avoided.
Further, in the step S1, the coke powder is pulverized to D50After being mixed with the coating binding material, the mixture is mixed after being equal to 11 +/-1 mu m.
According to the scheme, the particle size of the artificial graphite anode material with the core-shell structure is finely controlled by limiting the particle size of pulverized coke powder, the particle size of agglomerated particles is controlled, and the influence of the excessive particle size on the compaction density of the anode material is avoided.
Further, the mixing mass ratio of the coke powder to the coating binding material is 100:0-100: 10.
the mass ratio of the coke powder to the coating binding material in the scheme is a preferable mass ratio obtained by technical personnel on the basis of a large number of experiments, in a mixture prepared by the mass ratio, the coating binding material can fully coat the coke powder, and meanwhile, the coating binding material can be matched with the particle size of the coke powder to realize finer control on the particle size of the artificial graphite cathode material, so that the consistency of the particle size of the produced artificial graphite cathode material is further improved;
even if the coating binding material is not added, the coal tar can also replace the coating binding material to coat the coke powder because the volatile matter in the coke powder can discharge the coal tar when being heated.
Further, in step S1, the gradient heating includes,
a first temperature gradient, raising the temperature from room temperature to T at a stirring speed of 10-35rpm1(ii) temperature;
a second temperature gradient from T at a stirring speed of 10-35rpm1The temperature is raised to T2(ii) temperature;
the T is1The temperature is higher than the softening temperature of the coating binding material and lower than the carbonization temperature of the shell material, and the T is2The temperature is higher than the carbonization temperature of the coating bonding material, and the coating bonding material is at T2A carbonization layer is formed outside the coke powder at the temperature, so that when the artificial graphite negative electrode material is used as a negative electrode material of a lithium battery, lithium ions can be effectively prevented from being embedded, a graphite layer is prevented from falling off, and the cycle performance of the artificial graphite negative electrode material is improved; meanwhile, the thickness of an SEI film generated on the surface of the artificial graphite cathode material is reduced through the carbonization layer, and the first effect of the cathode material is improved.
Further, in the first temperature rising gradient, the temperature is gradually raised from room temperature to T at the speed of 3-5 ℃/min1(ii) temperature;
in the second temperature rising gradient, the temperature is controlled from T at the speed of 2-3.5 ℃/min1The temperature is raised to T2And (3) temperature.
According to the scheme, the temperature is gradually increased at the speed of 3-5 ℃/min, so that the coating bonding material which is originally in a solid state is fully heated and is completely softened in a short time when reaching the softening temperature, the coating uniformity is further improved, the phenomenon that part of the coating bonding material is not softened when the temperature is increased too fast is avoided, and the condition of uneven coating is further generated, so that the product quality is reduced.
Further, when the coating binding material is asphalt, T1The temperature is 250 ℃ and 300 ℃, T2The temperature is 600-800 ℃.
Further, in the first temperature rise gradient, the temperature rises to T1Preserving heat for 1-4h after the temperature is reached;
in the second temperature gradient, the temperature is raised to T2Keeping the temperature for 2-8h after the temperature is reached.
D of the anode material semi-finished particles prepared by the step S150＝17±2μm，TD≥0.5g/cm3。
The artificial graphite anode material is directly obtained after the anode material semi-finished product particles are subjected to graphitization treatment and demagnetizing screening, wherein no agglomeration or decomposition is generated, so that the granularity and tap density of the anode material semi-finished product particles are directly related to the granularity and tap density of the finally prepared artificial graphite anode material; d of the anode material semi-finished product particles in the scheme50And the TD range is a more preferable range obtained by a skilled person on the basis of a large number of experiments by dividing D of the anode material semifinished product particles50And TD is controlled in the range, so that the control on the granularity and the processing performance of the artificial graphite cathode material can be realized, and the consistency of the performance of the artificial graphite cathode material is improved.
Further, the coke powder comprises one of metallurgical coke, petroleum coke and isotropic coke; the coated binder material includes one of pitch, phenolic resin, and sucrose.
Further, in the step S2, in the step S2, the temperature of the semi-finished anode material particles is raised to a temperature higher than the graphitization temperature through at least three temperature gradients, so as to obtain a crude artificial graphite anode material.
The plurality of temperature gradients include 1100-; 1800 ℃ and 2000 ℃; and 2800-3000 ℃.
Further, the three temperature gradients are specifically,
a first temperature gradient, heating from room temperature to 1100-1300 ℃ at a heating rate of 2-5 ℃/min;
a second temperature gradient, heating to 1800-2000 ℃ at a heating rate of 0.5-3 ℃/min;
a third temperature gradient, heating to 2800-3000 ℃ at a heating rate of 1-4 ℃/min.
The heating rate in the scheme is the preferable heating rate obtained by technicians on the basis of a large number of experiments, the heating rate of the first temperature gradient is set to be 2-5 ℃/min, so that the preheating is completed at a higher speed while cracks caused by over-high heating of the semi-finished particles of the cathode material are avoided, and the production period is shortened; because the second temperature gradient is a key stage of graphitization, the temperature rise rate of the second temperature rise gradient is set to be 0.5-3 ℃/min, the crystal structure of the semi-finished product particles of the cathode material can fully realize graphitization transformation at a lower temperature rise rate, the graphitization degree is improved, the crystal structure is prevented from being damaged under the action of thermal stress due to too fast temperature rise, and the integrity of the graphitization structure is improved; the temperature rise rate of the third temperature gradient is 1-4 ℃/min, the graphitization degree is improved, the production efficiency is improved, and the production cost is reduced.
Further, after the graphitization is completed, the product is demagnetized and screened in sequence to obtain the artificial graphite cathode material.
Furthermore, the content of the magnetic substance in the artificial graphite negative electrode material after the demagnetization is finished is lower than 0.1 ppm.
Further, the particle size parameters of the screened artificial graphite cathode material are as follows:
D10：5-8μm；
D50：14-16μm；
D90：25-30μm；
D100：≤50μm。
furthermore, the specific surface area SSA of the artificial graphite anode material prepared by the scheme is less than or equal to 1.3m2(ii)/g; tap densityDegree TD is more than or equal to 1g/cm3。
In the scheme, the coating binding material in the artificial graphite cathode material covers the coke powder, so that the shielding of a cavity generated on the graphitized coke powder is realized, the specific surface area of the artificial graphite cathode material is obviously reduced, the quantity of lithium ions embedded into a cathode when an SEI (solid electrolyte interphase) film is formed is further reduced, the reversible capacity of a battery manufactured by using the artificial graphite cathode material is further improved, and the first efficiency of the battery is improved; meanwhile, the surface of the artificial graphite cathode material is modified by coating the binding material and coating the coke powder, so that the tap density of the material is improved, and the energy density of the battery is further improved; meanwhile, the coating binding material can protect the coke powder, so that the graphite layer is prevented from falling off, and the cycle performance of the cathode material is improved.
The beneficial effects of the above technical scheme are:
firstly, the coating binding material and the coke powder are mixed to form a core-shell structure, and then graphitization is carried out, so that the graphitized core layer is uniformly coated by the surface carbon layer, and the coating stability and consistency of the prepared artificial graphite cathode material are improved; the particle size of the prepared artificial graphite cathode material is accurately controlled by controlling the particle size of the coke powder and the proportion of the coating binding material to the coke powder, so that the consistency of the product is further improved; the temperature is increased at a certain speed to carbonize the coating bonding material, so that the coating uniformity of the coating bonding material is further improved; the coating binding material is used for modifying the surface of the focusing powder, so that the specific surface area of the artificial graphite cathode material is reduced, the quantity of lithium ions embedded into a cathode when an SEI (solid electrolyte interphase) film is formed is reduced, the reversible capacity of a battery manufactured by using the artificial graphite cathode material is improved, and the first effect of the battery is improved.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention, are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention without limiting the invention to the right. It is obvious that the drawings in the following description are only some embodiments, and that for a person skilled in the art, other drawings can be derived from them without inventive effort.
Fig. 1 is a process flow chart of the preparation method of the artificial graphite anode material of the invention.
Fig. 2 is a 500-fold SEM image of an artificial graphite anode material prepared using the method of the present invention.
Fig. 3 is a 1000-fold SEM image of an artificial graphite negative electrode material prepared using the method of the present invention.
Detailed Description
To make the objects, technical solutions and advantages of the present invention clearer and more fully described below with reference to some examples, it will be understood by those skilled in the art that the following embodiments are only used for explaining the technical principles of the present invention and are not intended to limit the scope of the present invention. For example, although the present application describes the steps of the method of the invention in a particular order, these orders are not limiting, and one skilled in the art can perform the steps in a different order without departing from the underlying principles of the invention.
Example one
As an embodiment of the present invention, this embodiment provides an artificial graphite anode material, and the preparation method thereof includes the following steps:
(1) selecting the coke powder with ash content less than 0.6%, sulfur content less than 1% and volatile content less than 15% as raw material, grinding the raw material by using a roll mill, and drying the pulverized coke powder to obtain the material A, wherein D50 of the pulverized coke powder is 11.
(2) Feeding the material A and asphalt with the magnetic substance content of less than 0.8ppm and the softening point of 180-3Negative electrode material ofAnd (4) feeding the semi-finished product particles C.
(3) Then feeding the cathode material semi-finished product particles C into a graphitization furnace, and finishing graphitization transformation of the cathode material semi-finished product particles C by three temperature gradients; firstly, heating to 1100 ℃ from room temperature at a heating rate of 2 ℃/min; then continuously heating to 1800 ℃ at the heating rate of 0.5 ℃/min; and finally heating to 3000 ℃ at the heating rate of 4 ℃/min to obtain a crude product D of the artificial graphite cathode material.
(4) Demagnetizing the crude product D of the artificial graphite negative electrode material, screening the crude product D of the artificial graphite negative electrode material to obtain an artificial graphite negative electrode material E, and mixing multiple batches of the artificial graphite negative electrode materials E.
Example two
As another embodiment of the present invention, this embodiment provides an artificial graphite negative electrode material, which is prepared by the same method as that described in the first embodiment, except that in this embodiment, the coating binder material in step (1) is a phenolic resin.
The method specifically comprises the following steps:
(2) feeding the material A and phenolic resin into a reaction kettle according to the mass ratio of 100:3, fully mixing the material A and asphalt in a stirring manner to obtain a mixture B, then under the protection of nitrogen, under the condition of stirring the mixture B at the stirring speed of 15rpm, gradually raising the temperature from room temperature to 150 ℃ at the heating rate of 5 ℃/min, preserving the temperature for 4 hours, then stirring and stirring the mixture B at the speed of 25rpm, raising the temperature to 800 ℃ at the heating rate of 3.5 ℃/min, and keeping the temperature for 8 hours to obtain the product D50 of 18.26 mu m and the tap density of 0.86g/cm3The anode material semifinished product particles C.
EXAMPLE III
As another embodiment of the present invention, this embodiment provides an artificial graphite negative electrode material, which is prepared in the same manner as described in the first embodiment, except that in this embodiment, no coating binder is added to the coke powder in step (2).
The method specifically comprises the following steps:
(2) the material A is reacted in a kettle, then under the protection of nitrogen, the temperature is gradually increased from room temperature to 250 ℃ at the heating rate of 5 ℃/min under the condition that the material A is stirred at the stirring speed of 10rpm, the temperature is kept for 4h, then the temperature is increased to 800 ℃ at the heating rate of 3.5 ℃/min while the material A is stirred at the speed of 25rpm, and the temperature is kept for 8h, so that D50 is 13.52 mu m, and the tap density is 0.81g/cm3The anode material semifinished product particles C.
(3) Then feeding the cathode material semi-finished product particles C into a graphitization furnace, and finishing graphitization transformation of the cathode material semi-finished product particles C by three temperature gradients; firstly, heating to 1300 ℃ from room temperature at a heating rate of 5 ℃/min; then continuously heating to 1800 ℃ at the heating rate of 0.5 ℃/min; and finally heating to 3000 ℃ at the heating rate of 4 ℃/min to obtain a crude product D of the artificial graphite cathode material.
Example four
As another example of the present invention, this example provides an artificial graphite negative electrode material, which is prepared in the same manner as described in the first example, except that the mixing ratio of the coke powder and the coating binder material, and the stirring speed and temperature in steps (2) and (3) are different in this example.
The method specifically comprises the following steps:
(2) feeding the material A and asphalt with the magnetic substance content of less than 0.8ppm and the softening point of 180-class asphalt at 250 ℃ into a reaction kettle according to the mass ratio of 100:10, fully mixing the material A and the asphalt in a stirring manner to obtain a mixture B, gradually heating the mixture B from room temperature to 280 ℃ at the heating rate of 3 ℃/min under the protection of nitrogen under the condition of stirring the mixture B at the stirring speed of 25rpm, preserving heat for 4h, heating the mixture B to 700 ℃ at the heating rate of 2 ℃/min while stirring the mixture B at the speed of 10rpm, and keeping the temperature for 8h to obtain D50 of 19.69 mu m and the tap density of 0.83g/cm3The anode material semifinished product particles C.
(3) Then feeding the cathode material semi-finished product particles C into a graphitization furnace, and finishing graphitization transformation of the cathode material semi-finished product particles C by three temperature gradients; firstly, heating to 1200 ℃ from room temperature at a heating rate of 2 ℃/min; then continuously heating to 2000 ℃ at the heating rate of 3 ℃/min; and finally heating to 2800 ℃ at the heating rate of 1 ℃/min to obtain a crude product D of the artificial graphite cathode material. Comparative example 1
This comparative example provides an artificial graphite negative electrode material, which is prepared by a method different from that of example one in that the respective steps of the preparation method in this comparative example are operated in the same order but in a different order.
The method specifically comprises the following steps:
(1) selecting the coke powder with ash content less than 0.6%, sulfur content less than 1% and volatile content less than 15% as raw material, grinding the raw material by using a roller mill, and drying the pulverized coke powder to obtain the material A, wherein D50 of the pulverized coke powder is 11 mu m.
(2) Then the material A is sent into a graphitization furnace, and graphitization transformation of the material A is completed by three temperature gradients; firstly, heating to 1100 ℃ from room temperature at a heating rate of 2 ℃/min; then continuously heating to 1800 ℃ at the heating rate of 0.5 ℃/min; and finally heating to 3000 ℃ at the heating rate of 4 ℃/min to obtain the graphitized material B.
(3) Sending the graphitized material B and asphalt with the magnetic substance content of less than 0.8ppm and the softening point of 180-class asphalt at 250 ℃ into a reaction kettle according to the mass ratio of 100:3, fully mixing the graphitized material B and the asphalt in a stirring manner to obtain a mixture C, gradually heating the mixture C from room temperature to 250 ℃ at the heating rate of 5 ℃/min under the protection of nitrogen under the condition of stirring the mixture C at the stirring speed of 10rpm, preserving heat for 4h, heating the mixture C to 800 ℃ at the heating rate of 3.5 ℃/min while stirring and stirring the mixture C at the speed of 25rpm, and keeping the temperature for 8h to obtain a crude product D of the artificial graphite cathode material.
(4) Demagnetizing the crude product D of the artificial graphite negative electrode material until the content of magnetic substances is less than or equal to 0.1ppm, then screening the crude product D of the artificial graphite negative electrode material to obtain an artificial graphite negative electrode material E, and then mixing a plurality of batches of artificial graphite negative electrode materials E.
Comparative example No. two
This comparative example provides an artificial graphite negative electrode material, the preparation method of which is different from that of example one in that step (2) is not included in this comparative example.
The method specifically comprises the following steps:
(1) selecting the coke powder with ash content less than 0.6%, sulfur content less than 1% and volatile content less than 15% as raw material, grinding the raw material by using a roll mill, and drying the pulverized coke powder to obtain the material A, wherein D50 of the pulverized coke powder is 11.
(2) Then the material A is sent into a graphitization furnace, and graphitization transformation of the material A is completed by three temperature gradients; firstly, heating to 1100 ℃ from room temperature at a heating rate of 2 ℃/min; then continuously heating to 1800 ℃ at the heating rate of 0.5 ℃/min; and finally heating to 3000 ℃ at the heating rate of 4 ℃/min to obtain the graphitized material B.
(3) Demagnetizing the graphitized material B, wherein the content of magnetic substances in the demagnetized graphitized material B is less than or equal to 0.1ppm, screening the graphitized material B to obtain an artificial graphite negative electrode material C, and mixing multiple batches of the artificial graphite negative electrode materials C.
Examples of the experiments
The experimental example aims to compare the performances of the artificial graphite anode materials obtained by different preparation methods, and the comparison results are shown in the following table:
as can be seen from the test results of the example one and the comparative example one, the artificial graphite anode material obtained by coating the coating binder material on the surface of the coke powder, carbonizing, granulating and graphitizing has a more stable coating layer and a better modification effect on the surface of the material, so the specific surface area and the first efficiency of the artificial graphite anode material prepared by the method of the example are significantly higher than those of the material prepared by the method of the comparative document one.
Secondly, as can be seen from the test results of the third embodiment and the second embodiment, the step (2) has a significant influence on the final performance of the material, in the step (2), the volatile components in the coke powder are heated to generate coal tar, and the coal tar is coated on the surface of the coke powder to form a carbonized coating layer, so that the specific surface area of the artificial graphite negative electrode material is significantly reduced, and the first effect is improved, while in the second embodiment, the step (2) is omitted, so that the specific surface area of the prepared artificial graphite negative electrode material is significantly improved, and the first effect is lower.
The above embodiments are only preferred embodiments of the present invention, and not intended to limit the present invention in any way, and although the present invention has been disclosed by the preferred embodiments, it is not intended to limit the present invention, and those skilled in the art can make various changes and modifications to the equivalent embodiments by using the technical contents disclosed above without departing from the technical scope of the present invention, and the embodiments in the above embodiments can be further combined or replaced, but any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention still fall within the technical scope of the present invention.
Claims (10)
1. A preparation method of an artificial graphite cathode material is characterized by comprising the following steps,
s1, mixing the coke powder and the coating binding material to obtain a mixture, and performing gradient heating on the mixture to obtain semi-finished anode material particles;
s2, heating the semi-finished anode material particles to a graphitization temperature in a gradient heating manner to obtain a crude artificial graphite anode material;
and S3, demagnetizing and screening the coarse product of the artificial graphite cathode material to obtain the artificial graphite cathode material.
2. The method for producing artificial graphite anode material according to claim 1, wherein in step S1, the coke powder is pulverized to D50After being mixed with the coating binding material, the mixture is mixed after being equal to 11 +/-1 mu m.
3. The preparation method of the artificial graphite anode material according to claim 1, wherein in the step S1, the mass ratio of the coke powder to the coating binder is 100:0-100: 10.
4. the method for preparing the artificial graphite anode material according to claim 1, wherein the step S1, the gradient temperature rise includes,
a first temperature gradient, raising the temperature from room temperature to T at a stirring speed of 10-35rpm1(ii) temperature;
a second temperature gradient from T at a stirring speed of 10-35rpm1The temperature is raised to T2(ii) temperature;
the T is1The temperature is higher than the softening temperature of the coating binding material and lower than the carbonization temperature of the shell material, and the T is2The temperature is higher than the carbonization temperature of the coating binding material.
5. The method for preparing the artificial graphite anode material according to claim 4, wherein in the first temperature-rising gradient, the temperature gradually rises from room temperature to T at a rate of 3-5 ℃/min1(ii) temperature;
in the second temperature rising gradient, the temperature is controlled from T at the speed of 2-3.5 ℃/min1The temperature is raised to T2(ii) temperature;
preferably, when the coated binder material is asphalt, T1The temperature is 200 ℃ and 300 ℃, T2The temperature is 600-800 ℃.
6. The method for preparing artificial graphite anode material according to claim 4, wherein D is the amount of the anode material semi-finished particles obtained in step S150＝17±2μm，TD≥0.5g/cm3。
7. The method for preparing the artificial graphite anode material according to claim 1, wherein the coke powder comprises one of metallurgical coke, petroleum coke, and isotropic coke; the coated binder material includes one of pitch, phenolic resin, and sucrose.
8. The method for preparing artificial graphite anode material according to any one of claims 1 to 7, wherein in step S2, the temperature of the semi-finished anode material particles is raised to a temperature higher than the graphitization temperature by at least three temperature gradients, so as to obtain a crude artificial graphite anode material.
9. The method for preparing the artificial graphite anode material according to claim 8, wherein the three temperature gradients are,
a first temperature gradient, heating from room temperature to 1100-1300 ℃ at a heating rate of 2-5 ℃/min;
a second temperature gradient, heating to 1800-2000 ℃ at a heating rate of 0.5-3 ℃/min;
a third temperature gradient, heating to 2800-3000 ℃ at a heating rate of 1-4 ℃/min.
10. The method for preparing the artificial graphite anode material according to claim 1, wherein D is the content of the prepared artificial graphite anode material50：14-16μm；SSA≤1.3m2/g；TD≥1.0g/cm3。
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| CN115676817B (en) * | 2022-12-01 | 2024-04-05 | 山西沁新能源集团股份有限公司 | Preparation method of artificial graphite negative electrode material |
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