CN115924902A - Artificial graphite negative electrode material, preparation method and application thereof, and battery - Google Patents
Artificial graphite negative electrode material, preparation method and application thereof, and battery Download PDFInfo
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Abstract
The invention discloses an artificial graphite cathode material, a preparation method and application thereof, and a battery. The preparation method of the artificial graphite negative electrode material comprises the following steps: mixing, granulating and graphitizing the first particles, the second particles and the third particles; the first, second and third particles may be prepared by calcining and pulverizing the raw material; the calcination temperature of the first particles is 300-700 ℃; the calcination temperature of the second particles is 700-1100 ℃; the calcining temperature of the third particles is 1100-1500 ℃; the crushed first, second and third particles Dv50 are each independently 5.0-12.0 μm; the mass part of the first particles is 10-60 parts during mixing; 20-70 parts of second particles; 30-50 parts of third particles; the sum of the mass parts of the first, second and third particles is 90 parts; and adding a binder during mixing. The prepared artificial graphite cathode material has high discharge capacity, high discharge efficiency and low cyclic expansion rate.
Description
Technical Field
The invention relates to an artificial graphite cathode material, a preparation method and application thereof, and a battery.
Background
At present, with the higher dependence of people on consumer electronics, the public demand also puts higher demands on the cruising ability of batteries. For example, the popularization of 5G technology has led to a significant increase in the power consumption of mobile phone batteries. Therefore, the energy density of the existing mobile phone battery is improved, and the energy density is very important for the electric quantity storage quantity and the size of the mobile phone body. In addition, when the energy density meets the actual requirement, how to reduce the cycle expansion rate of the battery and prolong the service life of the battery is a problem to be solved urgently. Therefore, it is very urgent to improve the performance of the battery, which is the mutual constraint of the energy density and the cycle expansion level. The energy density and the cyclic expansion level of the battery are closely related to the negative electrode material of the battery, and the negative electrode material which is most widely applied at present is the artificial graphite negative electrode material.
The preparation process of the artificial graphite has important influence on the performance of the finally obtained graphite cathode material. In practical use, due to the characteristics of the artificial graphite anode material, when one property is outstanding, the other properties are generally deteriorated. Therefore, in the industry, different types of materials are generally mixed according to a certain proportion for use, and the mixed final product can generally integrate the advantages of each product and avoid the disadvantages caused by a single material.
However, the above mixing method is relatively simple. In the prior art, two materials are usually mixed, for example, a green coke secondary particle finished product and a green coke primary particle are mixed, or a cooked coke secondary particle finished product and a green coke primary particle are mixed. The compounding effect is difficult to achieve beyond the predicted effect of geometric proportion, especially in the aspects of energy density and cyclic expansion. The key factor is that when the proportion of the materials mixed is the same, the performance of different materials can be displayed at the same time. When the proportion of one of the materials involved in compounding is large, the disadvantage thereof appears to a large extent, and the weakening effect by the other components is insufficient to offset the appearing disadvantage. But when the proportion is reduced, the advantages are not sufficiently realized. Thus, when two materials are selected for mixing, a contradiction is always present. How to select the components and the proportion to mix the components can exert the advantages, and the key point of mixing is to avoid the disadvantages.
The prior art generally avoids the above disadvantages by selecting the compounding ratio of the individual materials, but no selection of compounding components has been mentioned. Three gradient products are selected in the patent, and are mixed according to a certain proportion, so that the problem of the performance defect of a single material can be effectively solved, and the comprehensive performance of the material in the aspects of energy density and cyclic expansion can be obviously improved.
Disclosure of Invention
The invention aims to overcome the defect that the artificial graphite cathode material prepared by mixing in the prior art cannot simultaneously realize the effects of high discharge capacity and low cycle expansion rate, and provides the artificial graphite cathode material, and a preparation method, application and a battery thereof. The artificial graphite cathode material prepared by the invention has higher discharge capacity and discharge efficiency and low cycle expansion rate.
The present invention mainly solves the above technical problems by the following technical means.
The invention provides a preparation method of an artificial graphite cathode material, which comprises the following steps:
mixing, granulating and graphitizing the first particles, the second particles and the third particles;
the preparation method of the first particles, the second particles and the third particles comprises the steps of calcining and crushing raw materials;
wherein the calcination temperature of the first particles is 300-700 ℃; the calcination temperature of the second particles is 700-1100 ℃; the calcination temperature of the third particles is 1100-1500 ℃; the Dv50 of the first, second and third particles after comminution are each independently from 5.0 to 12.0 μm;
wherein, when in mixing, the mass part of the first particles is 10 to 60 parts; the mass part of the second particles is 20-70 parts; the mass part of the third particles is 30-50 parts; the sum of the mass parts of the first particles, the second particles and the third particles is 90 parts;
in the mixing process, a binder is added during mixing.
In the present invention, the raw materials of the first, second and third particles may be raw materials conventionally used in the art for preparing artificial graphite anode materials, preferably needle coke, more preferably oil-based needle coke or coal-based needle coke, such as oil-based needle coke.
In the present invention, the calcination temperature of the first particles is preferably 500 to 600 ℃, for example, 520 ℃, 560 ℃ or 580 ℃. The calcination temperature of the second particles is preferably 800 to 1000 ℃, such as 850 ℃, 900 ℃ or 950 ℃. The calcination temperature of the third particles is preferably 1300 to 1500 ℃, for example 1350 ℃, 1400 ℃ or 1480 ℃.
In a preferred embodiment, the calcination temperature of the first particle is 600 ℃, the calcination temperature of the second particle is 900 ℃, and the calcination temperature of the third particle is 1300 ℃.
In the present invention, preferably, the calcination time of the first particle, the second particle and the third particle may be conventional in the art, and each independently ranges from 12 to 48 hours, such as 12 hours, 24 hours, 36 hours or 48 hours.
In the present invention, the pulverization may be carried out conventionally in the art, for example, in a pulverizer such as a roll mill.
In the present invention, preferably, the Dv50 of the first, second and third particles after comminution are each independently 6 to 10 μm, for example 7 μm, 8 μm or 9 μm.
In the present invention, the mass part of the first particles is preferably 10 to 40 parts, more preferably 20 to 40 parts, for example 30 parts.
In the present invention, the mass part of the second particles is preferably 20 to 60 parts or 30 to 70 parts, more preferably 20 to 50 parts, for example 30 parts.
In the present invention, the mass part of the third particles is preferably 30 to 40 parts or 50 parts.
In a preferred embodiment, the mass portion of the first particles is 20 to 40 parts, the mass portion of the second particles is 20 to 50 parts, and the mass portion of the third particles is 30 to 40 parts.
In a preferred embodiment, the mass part of the first particles is 30 parts, the mass part of the second particles is 30 parts, and the mass part of the third particles is 30 parts.
In the present invention, the kind of the binder added at the time of compounding may be conventional in the art, for example, asphalt. The bitumen may be conventional in the art, and is preferably a bitumen having a softening point of from 150 to 280 ℃, for example a bitumen having a softening point of 200 ℃.
In the present invention, the amount of the binder added during the mixing is preferably 5 to 20 parts by mass, for example, 8 parts, 10 parts or 15 parts.
In the invention, the granulation can bond different particles, thereby increasing the isotropy of the artificial graphite negative electrode material and reducing the expansion performance of the artificial graphite negative electrode material.
In the present invention, the granulation may be conventional in the art, preferably in a roller oven. The temperature of the granulation may be 500 to 600 ℃, for example 550 ℃.
In the present invention, the graphitization temperature may be 2500-3500 ℃, preferably 2800-3400 ℃, for example 3200 ℃.
In the present invention, the graphitization step further comprises a step of mixing and screening, which is conventional in the art.
In a preferred embodiment, the raw material is needle coke, and the preparation of the artificial graphite negative electrode material comprises the following steps:
(1) Calcining the needle coke at 300-700 ℃, 700-1100 ℃ and 1100-1500 ℃ respectively, and crushing to obtain first particles, second particles and third particles respectively; the Dv50 of the first, second and third particles obtained by crushing was 9 μm;
(2) The mass parts of the first particles are 10-30 parts, the mass parts of the second particles are 30-40 parts, and the mass parts of the third particles are 30-50 parts;
(3) Adding 10 parts of asphalt with the softening point of 200 ℃ for mixing;
(4) Granulating at 550 ℃;
(5) After graphitization treatment at 3200 ℃, the finished product is mixed and sieved to obtain the artificial graphite cathode material.
In a preferred embodiment, the raw material is needle coke, and the preparation of the artificial graphite negative electrode material comprises the following steps:
(1) Calcining the needle coke at 600 ℃, 900 ℃ and 1300 ℃ respectively, and crushing to obtain first particles, second particles and third particles respectively; the Dv50 of the first, second and third particles obtained after the pulverization are all 9 μm;
(2) The mass parts of the first particles are 30 parts, the mass parts of the second particles are 30 parts, and the mass parts of the third particles are 30 parts;
(3) Adding 10 parts of asphalt with the softening point of 200 ℃ for mixing;
(4) Granulating at 550 ℃;
(5) After graphitization treatment at 3200 ℃, the finished product is mixed and sieved to obtain the artificial graphite cathode material.
In a preferred embodiment, the raw material is needle coke, and the preparation of the artificial graphite negative electrode material comprises the following steps:
(1) Calcining the needle coke at 600 ℃, 900 ℃ and 1300 ℃ respectively, and crushing to obtain first particles, second particles and third particles respectively; the Dv50 of the first, second and third particles obtained after the pulverization are all 9 μm;
(2) The mass parts of the first particles are 10 parts, the mass parts of the second particles are 30 parts, and the mass parts of the third particles are 50 parts;
(3) Adding 10 parts of asphalt with the softening point of 200 ℃ for mixing;
(4) Granulating at 550 ℃;
(5) After graphitization treatment at 3200 ℃, the finished product is mixed and sieved to obtain the artificial graphite cathode material.
In a preferred embodiment, the raw material is needle coke, and the preparation of the artificial graphite negative electrode material comprises the following steps:
(1) Calcining the needle coke at 300 ℃, 700 ℃ and 1100 ℃ respectively, and crushing to obtain first particles, second particles and third particles respectively; the Dv50 of the first, second and third particles obtained by crushing was 9 μm;
(2) The mass parts of the first particles are 30 parts, the mass parts of the second particles are 30 parts, and the mass parts of the third particles are 30 parts;
(3) Adding 10 parts of asphalt with the softening point of 200 ℃ for mixing;
(4) Granulating at 550 ℃;
(5) After graphitization treatment at 3200 ℃, the finished product is mixed and sieved to obtain the artificial graphite cathode material.
In a preferred embodiment, the raw material is needle coke, and the preparation of the artificial graphite negative electrode material comprises the following steps:
(1) Calcining the needle coke at 700 ℃, 1100 ℃ and 1500 ℃ respectively, and crushing to obtain first particles, second particles and third particles respectively; the Dv50 of the first, second and third particles obtained by crushing was 9 μm;
(2) The mass parts of the first particles are 30 parts, the mass parts of the second particles are 30 parts, and the mass parts of the third particles are 30 parts;
(3) Adding 10 parts of asphalt with the softening point of 200 ℃ for mixing;
(4) Granulating at 550 ℃;
(5) After graphitizing treatment at 3200 ℃, mixing and screening the finished product to obtain the artificial graphite cathode material.
The invention provides an artificial graphite cathode material which is prepared by the preparation method of the artificial graphite cathode material.
In the invention, the artificial graphite negative electrode material simultaneously meets the following indexes:
the first discharge capacity of the artificial graphite material can be more than 360mAh/g, preferably 360-365mAh/g; the discharge efficiency of the artificial graphite material can be more than 92%, and is preferably 92% -96%; the artificial graphite material has a normal temperature cyclic expansion rate of less than 9% at 800 weeks, preferably 5% -9%.
In the present invention, the artificial graphite anode material may be in the form of particles of secondary particles.
The invention also provides an application of the artificial graphite cathode material in a battery.
The invention also provides a battery which comprises the artificial graphite negative electrode material.
On the basis of the common knowledge in the field, the above preferred conditions can be combined randomly to obtain the preferred embodiments of the invention.
The raw materials used in the present invention are commercially available.
The positive progress effects of the invention are as follows:
in the invention, the raw materials are creatively calcined and crushed at different temperatures to respectively obtain a first particle, a second particle and a third particle, and the first particle, the second particle and the third particle are mixed according to a certain mass part, namely the mixing is carried out in a raw material section, which is obviously different from the mixing way of finished products of different particles in the prior art; then adding a binder to carry out mixing, granulation and graphitization treatment to obtain the artificial graphite negative electrode material. The prepared artificial graphite cathode material fully exerts the advantages of different particles, avoids the disadvantages of different particles, realizes the effect of 1+ 3, and ensures that the material simultaneously has high first discharge capacity, high discharge efficiency and low cyclic expansion rate.
Drawings
FIG. 1 is a scanning electron microscope image of the artificial graphite negative electrode material prepared in example 1.
FIG. 2 is a graph showing electrochemical charge and discharge curves of the artificial graphite negative electrode material prepared in example 1.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
Example 1 preparation of artificial graphite negative electrode material
Step (1): calcining three parts of needle coke at different temperatures; wherein the calcining temperature is 600 ℃, 900 ℃ and 1300 ℃ respectively;
step (2): crushing and grading the three raw materials calcined at different temperatures to obtain first particles, second particles and third particles respectively; wherein, the Dv50 of the first, second and third particles after crushing and classification are all 9.0 μm;
and (3): mixing, granulating, graphitizing and screening the first particles, the second particles and the third particles to obtain a graphite cathode material; wherein the softening point of the asphalt used in the mixing is 200 ℃, the part of the asphalt is 10 parts, the granulation temperature is 550 ℃, the graphitization temperature is 3200 ℃, and the mixed parts by mass of the first particles, the second particles and the third particles are 30 parts.
The artificial graphite negative electrode material prepared in example 1 was subjected to a scanning electron microscope test, and the test results are shown in fig. 1.
The artificial graphite negative electrode material obtained in example 1 was subjected to a charge-discharge curve test, and the test results are shown in fig. 2.
Example 2 preparation of artificial graphite negative electrode material
The only difference from example 1 is: in the step (3), the mass part of the first particles is 10 parts, the mass part of the second particles is 30 parts, and the mass part of the third particles is 50 parts.
Example 3 preparation of artificial graphite negative electrode Material
The only difference from example 1 is: the calcination temperature in the step (1) is 300 ℃, 700 ℃ and 1100 ℃.
Example 4 preparation of artificial graphite negative electrode Material
The only difference from example 1 is: the calcination temperature in the step (1) is 700 ℃, 1100 ℃ and 1500 ℃ respectively.
Comparative example 1 preparation of artificial graphite negative electrode Material
The only difference from example 1 is that the calcination temperature in step (1) was 200 deg.C, 600 deg.C, and 900 deg.C, respectively.
Comparative example 2 preparation of artificial graphite negative electrode Material
The only difference from example 1 is that in step (3), the mass part of the first granules is 10 parts, the mass part of the second granules is 70 parts, and the mass part of the third granules is 20 parts.
Comparative example 3 preparation of artificial graphite negative electrode Material
The only difference from example 1 is that Dv50 of the first particles, the second particles and the third particles after pulverization classification in step (2) were all 13 μm.
Comparative example 4 preparation of artificial graphite negative electrode Material
The preparation method of the green coke secondary particle finished product comprises the following steps: the needle coke which is the same as the needle coke obtained in the embodiment 1 is crushed, mixed, granulated, graphitized and sieved; wherein, the Dv50 of the needle coke after being crushed is 9 μm, the softening point of the asphalt used in the mixing process is 200 ℃, the part of the asphalt is 10 parts, the granulation temperature is 550 ℃, and the graphitization temperature is 3200 ℃.
The preparation method of the green coke primary particles comprises the following steps: the needle coke same as that in the example 1 is crushed, graphitized and mixed and sieved to obtain the needle coke; wherein the Dv50 of the needle coke after pulverization is 9 μm, and the temperature of the graphitization treatment is 3200 ℃.
And mixing 60 parts by mass of the green coke secondary particle finished product with 30 parts by mass of the green coke primary particles to obtain the artificial graphite cathode material.
Comparative example 5 preparation of artificial graphite negative electrode Material
The preparation method of the finished product of the cooked coke secondary particles comprises the following steps: calcining, crushing, mixing, granulating, graphitizing and screening the needle coke which is the same as the needle coke obtained in the embodiment 1; wherein the calcining temperature is 1300 ℃, the Dv50 of the crushed needle coke is 9 μm, the softening point of the asphalt used in the mixing process is 200 ℃, the part of the asphalt is 10 parts, the granulating temperature is 550 ℃, and the graphitizing treatment temperature is 3200 ℃.
The preparation method of the green coke primary particles comprises the following steps: the needle coke same as that in the example 1 is crushed, graphitized and mixed and sieved to obtain the needle coke; wherein the Dv50 of the needle coke after pulverization is 9 μm, and the temperature of the graphitization treatment is 3200 ℃.
And mixing 60 parts by mass of the finished product of the secondary particles of the cooked coke with 30 parts by mass of the primary particles of the green coke to obtain the artificial graphite cathode material.
Effects of the embodiment
In the present invention, the test methods of the first discharge capacity and the first discharge efficiency are conventional test methods in the art. The method specifically comprises the following steps: dissolving PVDF in NMP solvent, adding a certain amount of SP, uniformly stirring, adding the composite graphite negative electrode material, uniformly stirring, namely mixing slurry, coating, preheating, drying, rolling for two times, die cutting, cutting into pieces, and assembling the button cell to obtain the button cell. Wherein the electrolyte adopts 1M LiPF6, EC: DEC: DMC =1 (volume ratio), counter electrode is a metallic lithium sheet, charge/discharge potential is 0.005 to 2.000V, and charge/discharge rate is 0.1C.
In the present invention, the cycle performance test method is a conventional test method in the art. The method specifically comprises the following steps: the composite graphite cathode material is subjected to slurry mixing, coating, preheating and drying, rolling, drying, secondary rolling, die cutting, winding and battery assembly by the same method as the button battery to obtain the full battery. Wherein, the anode material adopts lithium cobaltate, and the charge-discharge multiplying power is 1C. The cycle performance test results are shown in table 1.
The artificial graphite anode materials obtained in examples 1 to 4 and comparative examples 1 to 5 were subjected to electrochemical performance tests, and the specific results are shown in table 1.
TABLE 1
As can be seen from the above table, the properties of the artificial graphite anode material of the present invention are summarized as follows: (1) the first discharge capacity is more than 360 mAh/g; (2) the discharge efficiency is more than 92%; (3) the cyclic expansion rate is less than 9%.
The discharge capacity of examples 1 to 4 was greatly improved (by 0.3 to 10.2 mAh/g) as compared with comparative examples 1 to 5.
In comparative example 1, the calcination temperatures of the first, second, and third particles were all low, and the obtained artificial graphite negative electrode material had a low discharge capacity and a cycle expansion rate of not more than 9%, although the discharge efficiency was high.
In comparative example 2, when the mass fraction of the third particles was small, the obtained artificial graphite negative electrode material had a low discharge capacity although the cycle expansion rate was 9% or less and the discharge efficiency was 92% or more.
In comparative example 3, when the particle diameters of the first, second and third particles were large, the obtained artificial graphite anode material was low in discharge capacity and even reached a cycle expansion rate of 12.9%, although the discharge efficiency was high.
In comparative example 4, when the finished green coke secondary particles were mixed with the primary green coke particles, the discharge capacity of the artificial graphite negative electrode material was much lower than that of the artificial graphite negative electrode materials obtained in examples 1 to 4 of the present application, although the cycle expansion rate was 9% or less and the discharge efficiency was 92% or more.
In comparative example 5, when the finished product of the secondary coke particles and the primary coke particles were mixed, the discharge capacity of the obtained artificial graphite negative electrode material was much lower than that of the artificial graphite negative electrode materials obtained in examples 1 to 4 of the present application, and the cyclic expansion rate thereof could not reach 9% or less, although the discharge efficiency was 92% or more.
Claims (10)
1. The preparation method of the artificial graphite negative electrode material is characterized by comprising the following steps of: mixing, granulating and graphitizing the first particles, the second particles and the third particles;
the preparation method of the first particles, the second particles and the third particles comprises the steps of calcining and crushing raw materials;
wherein the calcination temperature of the first particles is 300-700 ℃; the calcination temperature of the second particles is 700-1100 ℃; the calcination temperature of the third particles is 1100-1500 ℃; the Dv50 of the first, second and third particles after comminution are each independently from 5.0 to 12.0 μm;
wherein, when in mixing, the mass part of the first particles is 10 to 60 parts; the mass part of the second particles is 20-70 parts; the mass part of the third particles is 30-50 parts; the sum of the mass parts of the first particles, the second particles and the third particles is 90 parts;
wherein, a binder is added during the mixing.
2. The method for preparing the artificial graphite anode material according to claim 1, wherein the raw material of the first particles, the second particles and the third particles is needle coke, preferably oil-based needle coke or coal-based needle coke, such as oil-based needle coke;
and/or the Dv50 of the first, second and third particles after comminution are each independently 6 to 10 μm, for example 7 μm, 8 μm or 9 μm.
3. The method for preparing an artificial graphite anode material according to claim 1, wherein the calcination temperature of the first particles is 500 to 600 ℃, for example 520 ℃, 560 ℃ or 580 ℃; the second particles have a calcination temperature of 800 to 1000 ℃, e.g., 850 ℃, 900 ℃ or 950 ℃; the calcination temperature of the third particles is 1300-1500 ℃, such as 1350 ℃, 1400 ℃ or 1480 ℃;
and/or the calcination time of the first, second and third particles is each independently from 12 to 48h, for example 12h, 24h, 36h or 48h.
4. The method for preparing the artificial graphite anode material according to claim 1, wherein the mass part of the first particles is 10 to 40 parts, preferably 20 to 40 parts, for example 30 parts;
and/or the mass part of the second particles is 20 to 60 parts or 30 to 70 parts, preferably 20 to 50 parts, for example 30 parts;
and/or the third particles are 30-40 parts or 50 parts by mass;
preferably, the mass part of the first particles is 20 to 40 parts, the mass part of the second particles is 20 to 50 parts, and the mass part of the third particles is 30 to 40 parts; more preferably, the mass part of the first particles is 30 parts, the mass part of the second particles is 30 parts, and the mass part of the third particles is 30 parts.
5. The method for preparing the artificial graphite anode material according to claim 1, wherein the kind of the binder added in the mixing is asphalt; the asphalt is preferably asphalt with a softening point of 150-280 ℃, such as asphalt with a softening point of 200 ℃;
and/or the mass part of the binder is 5-20 parts, such as 8 parts, 10 parts or 15 parts.
6. The method for preparing the artificial graphite negative electrode material according to claim 1, wherein the granulation is performed in a roller furnace;
and/or the granulation temperature is 500 to 600 ℃, for example 550 ℃;
and/or the graphitization temperature is 2500-3500 ℃, preferably 2800-3400 ℃, for example 3200 ℃;
and/or, further comprising a step of mixing and screening after the graphitization.
7. An artificial graphite negative electrode material, characterized in that it is produced by the method for producing an artificial graphite negative electrode material according to any one of claims 1 to 6.
8. The artificial graphite anode material according to claim 7, wherein the artificial graphite anode material satisfies the following criteria at the same time:
the first discharge capacity of the artificial graphite material is more than 360mAh/g, preferably 360-365mAh/g; the discharge efficiency of the artificial graphite material is more than 92%, preferably 92% -96%; the normal temperature cycle expansion rate of the artificial graphite material at 800 weeks is less than 9%, preferably 5% -9%;
and/or the artificial graphite anode material is in the form of particles of secondary particles.
9. Use of the artificial graphite negative electrode material according to claim 7 or 8 in a battery.
10. A battery comprising the artificial graphite negative electrode material according to claim 7 or 8.
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