CN113764640A - Production method of high-compaction and fast-charging type lithium ion battery cathode material - Google Patents
Production method of high-compaction and fast-charging type lithium ion battery cathode material Download PDFInfo
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- H—ELECTRICITY
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Abstract
The invention relates to a method for producing a high-compaction and fast-charging type lithium ion battery cathode material, which comprises the steps of mixing an artificial graphite raw material and a binder according to a certain proportion to obtain a mixture 1; under the protection of inert gas, carrying out chemical modification treatment to obtain secondary particles; mixing with a hard carbon coating agent to obtain a mixture 2; carrying out low-temperature curing treatment to obtain a hard carbon-coated secondary particle precursor; performing high-temperature graphitization treatment to obtain a graphitized product precursor; mixing with a liquid coating agent, and then carrying out spray drying to obtain a spray-dried precursor; carbonizing under the protection of inert gas to obtain the lithium ion battery cathode material. The prepared lithium ion battery cathode material has the characteristics of low specific surface area, high compaction density, high primary efficiency and good charging performance.
Description
Technical Field
The invention relates to a method for producing a high-compaction and fast-charging type lithium ion battery cathode material, and belongs to the technical field of lithium ion battery cathode materials.
Background
Under the background of the national strategy of energy development, lithium ion batteries have the advantages of high energy density, small volume, good cycle stability, no memory effect, good safety performance and the like, and are widely applied. With the strong support of national policies and the continuous improvement and increase of the living standard of people, higher requirements are put forward on lithium ion batteries: higher capacity, longer cycle life and faster charging speed.
Graphite is used as an important component of a lithium ion battery, and directly influences the performance of the battery, and the conventional graphite has a small interlayer spacing, so that the quick charging performance of the lithium ion battery is seriously influenced, the power performance of the lithium ion battery is poor, the large-current charging performance is low, and the application of the lithium ion battery in digital and new energy automobiles is limited. In order to solve the above problems, it is necessary to develop a graphite negative electrode material having a simple process and excellent quick charging properties.
Chinese patent document CN112421001A discloses a high-rate double-layer coated graphite negative electrode material, in which the inner layer of the double-layer coated layer is a soft carbon layer, and the outer layer is a hard carbon layer. Although the charging performance of the graphite is improved by utilizing the characteristic of large spacing between the soft carbon layer and the hard carbon layer, the double-layer coating is the coating before graphitization, and the soft carbon belongs to easily graphitizable carbon, so that the material only actually realizes the effect of coating the hard carbon by a single layer after graphitization.
Chinese patent document CN112490443A discloses a liquid phase coated graphite negative electrode material, in which graphitized petroleum coke products are mixed with liquid phenolic resin and then carbonized to obtain the liquid phase coating, and this coating method forms a pyrolytic carbon layer on the graphite surface, but only modifies a part of graphite defects, and needs to be further improved.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for producing a high-compaction and fast-charging type lithium ion battery cathode material.
In order to solve the above problems, the specific technical scheme of the invention is as follows: the high-compaction and fast-charging type lithium ion battery cathode material is characterized in that: the coating agent comprises graphite raw material powder, a hard carbon coating agent and a liquid coating agent, wherein the hard carbon coating agent comprises phenolic resin, and the liquid coating agent comprises a coating agent of asphalt dissolved in an aromatic solvent or a hydrocarbon solvent.
A method for producing a high-compaction and fast-charging type lithium ion battery cathode material comprises the following specific production processes:
s1: carrying out coarse crushing and fine crushing on an artificial graphite raw material, and then carrying out spheroidizing, shaping and grading to obtain graphite raw material powder;
s2: mixing the raw material powder obtained in the step S1 with a binder according to a certain ratio to obtain a mixture 1;
s3: carrying out chemical modification treatment on the mixture 1 obtained in the step S2 under the protection of inert gas to obtain secondary particles;
s4: mixing the secondary particles obtained in the step S3 with a hard carbon coating agent to obtain a mixture 2;
s5: carrying out low-temperature curing treatment on the mixture 2 obtained in the step S4 under the protection of inert gas to obtain a hard carbon coated secondary particle precursor;
s6: performing high-temperature graphitization treatment on the hard carbon-coated secondary particle precursor obtained in the step S5 to obtain a graphitized product precursor;
s7: mixing the graphitized product precursor obtained in the step S6 with a liquid coating agent, and then carrying out spray drying to obtain a spray-dried precursor;
s8: and (5) carbonizing the spray-dried precursor obtained in the step (S7) under the protection of inert gas to obtain the lithium ion battery cathode material.
In step S1, the artificial graphite raw material is raw coke or calcined coke, the raw coke is one or a combination of more of petroleum coke, pitch coke or needle coke, and the particle size value of the graphite raw material powder D50 is 6-10 μm.
In step S2, the ratio of the raw material powder to the binder is 85:15-99:1, the binder is petroleum asphalt or coal asphalt, and the D50 particle size of the binder is 2-6 μm.
In step S3, the temperature of the chemical modification treatment is 500-700 ℃, the treatment time is 8-15h, and the particle size D50 of the secondary particles is 12-20 μm.
In step S4, the hard carbon coating agent is phenolic resin, and the ratio of the secondary particles to the hard carbon coating agent is 92:8-99: 1.
In step S5, the low-temperature curing temperature is 90-300 ℃, and the curing time is 3-6 h.
In step S6, the graphitization temperature is 3000-3200 ℃, and the graphitization treatment time is 60-75 h.
In step S7, the liquid coating agent is a coating agent in which asphalt is dissolved in an aromatic solvent or a hydrocarbon solvent, and the temperature of the spray drying is 90 to 180 ℃.
In step S8, the carbonization temperature is 1050-1250 ℃, and the constant temperature time is 6-10 h.
The invention has the following beneficial effects: by the method of shaping and secondary granulation of the raw materials, particles form a random structure, the orientation of the materials is changed, and lithium ions can enter the graphite from all directions, so that the charging performance of the materials is improved;
the hard carbon is coated on the surface of the secondary particles before graphitization and the soft carbon is coated after graphitization, so that the interlayer spacing on the surface of the graphite particles is more favorably increased, the polarization during large-current charging is greatly reduced, and the accumulation of lithium ions on the surface of the graphite is avoided.
The coating uniformity of the graphite is further improved by coating a layer of soft carbon again in a spray drying mode, and solid-phase crosslinking of particles in a carbonization process is avoided by adopting the spray drying mode, so that the surfaces of the particles are smoother, and the compaction density of the graphite is greatly improved.
Detailed Description
Example 1:
the embodiment provides a method for producing a high-compaction and fast-charging type lithium ion battery cathode material, which comprises the following steps:
(1) carrying out coarse crushing and fine crushing on a petroleum coke raw material, and then carrying out spheroidizing, shaping and grading to obtain graphite raw material powder with the D50 particle size value of 6 mu m;
(2) mixing the raw material powder obtained in the step (1) with a petroleum asphalt binder according to the ratio of 95:5 for 2 hours to obtain a mixture 1,
(3) carrying out chemical modification on the mixed powder 1 obtained in the step (2) in a coating kettle under the protection of inert gas nitrogen, wherein the modification temperature is 550 ℃, and the treatment time is 10 hours, so as to obtain secondary particles with the D50 particle size value of 16 mu m;
(4) mixing the secondary particles obtained in the step (3) with phenolic resin according to the ratio of 98:2 for 3 hours to obtain a mixture 2;
(5) curing the mixture 2 obtained in the step (4) in a reaction kettle at a low temperature of 200 ℃ for 4h under the protection of inert gas nitrogen to obtain a hard carbon coated secondary particle precursor;
(6) graphitizing the hard carbon coated secondary particle precursor obtained in the step (5) in a graphitizing furnace, wherein the graphitizing temperature is 3000 ℃, and the graphitizing time is 65 hours to obtain a graphitized product precursor;
(7) mixing the graphitized product precursor obtained in the step (6) with an organic solvent of asphalt according to the ratio of 1:25, wherein
The ratio of the asphalt to the organic solvent is 1:4, and then spray drying is carried out to obtain a precursor, wherein the temperature of the spray drying is 160 ℃.
(8) And (4) carbonizing the spray-dried precursor obtained in the step (7) for 8 hours at 1050 ℃ in a roller kiln under the protection of nitrogen atmosphere to obtain the high-compaction and fast-charging type lithium ion battery cathode material.
Example 2
The embodiment provides a method for producing a high-compaction and fast-charging type lithium ion battery cathode material, which comprises the following steps:
(1) carrying out coarse crushing and fine crushing on needle coke green coke, and then carrying out spheroidizing, shaping and grading to obtain graphite raw material powder with the D50 particle size value of 8 mu m;
(2) mixing the raw material powder obtained in the step (1) with a petroleum asphalt binder according to a ratio of 90:10 for 2 hours to obtain a mixture 1,
(3) carrying out chemical modification on the mixed powder 1 obtained in the step (2) in a coating kettle under the protection of inert gas nitrogen, wherein the modification temperature is 650 ℃, and the treatment time is 8h, so as to obtain secondary particles with the particle size value of D50 being 15 mu m;
(4) mixing the secondary particles obtained in the step (3) with phenolic resin according to the ratio of 97:3 for 4 hours to obtain a mixture 2;
(5) curing the mixture 2 obtained in the step (4) in a reaction kettle at a low temperature of 250 ℃ for 6h under the protection of inert gas nitrogen to obtain a hard carbon coated secondary particle precursor;
(6) graphitizing the hard carbon coated secondary particle precursor obtained in the step (5) in a graphitization furnace, wherein the graphitization temperature is 3100 ℃, and the graphitization time is 70h to obtain a graphitized product precursor;
(7) mixing the graphitized product precursor obtained in the step (6) with an organic solvent of asphalt according to the ratio of 1:25, wherein
The ratio of the asphalt to the organic solvent is 1:3, and then spray drying is carried out to obtain a precursor, wherein the temperature of the spray drying is 180 ℃.
(8) And (4) carbonizing the spray-dried precursor obtained in the step (7) for 8 hours at 1100 ℃ in a roller kiln under the protection of nitrogen atmosphere to obtain the high-compaction and fast-charging type lithium ion battery cathode material.
Example 3
The embodiment provides a method for producing a high-compaction and fast-charging type lithium ion battery cathode material, which comprises the following steps:
(1) carrying out coarse crushing and fine crushing on needle coke calcined coke, and then carrying out spheroidizing, shaping and grading to obtain graphite raw material powder with the D50 particle size value of 8.5 mu m;
(2) mixing the raw material powder obtained in the step (1) with a petroleum asphalt binder according to a ratio of 85:15 for 2 hours to obtain a mixture 1,
(3) carrying out chemical modification on the mixed powder 1 obtained in the step (2) in a coating kettle under the protection of inert gas nitrogen, wherein the modification temperature is 700 ℃, and the treatment time is 8h, so as to obtain secondary particles with the D50 particle size value of 18 mu m;
(4) mixing the secondary particles obtained in the step (3) with phenolic resin according to the ratio of 95:5 for 5 hours to obtain a mixture 2;
(5) curing the mixture 2 obtained in the step (4) in a reaction kettle at a low temperature of 300 ℃ for 5 hours under the protection of inert gas nitrogen to obtain a hard carbon coated secondary particle precursor;
(6) graphitizing the hard carbon coated secondary particle precursor obtained in the step (5) in a graphitizing furnace, wherein the graphitizing temperature is 3200 ℃, and the graphitizing time is 75h to obtain a graphitized product precursor;
(7) mixing the graphitized product precursor obtained in the step (6) with an organic solvent of asphalt according to the ratio of 1:20, wherein
The ratio of the asphalt to the organic solvent is 1:3, and then spray drying is carried out to obtain a precursor, wherein the temperature of the spray drying is 220 ℃.
(8) And (4) carbonizing the spray-dried precursor obtained in the step (7) for 10 hours at 1050 ℃ in a roller kiln under the protection of nitrogen atmosphere to obtain the high-compaction and fast-charging type lithium ion battery cathode material.
Example 4
The embodiment provides a method for producing a high-compaction and fast-charging type lithium ion battery cathode material, which comprises the following steps:
(1) roughly crushing and finely crushing the pitch coke, and then carrying out spheroidizing, shaping and grading to obtain graphite raw material powder with the D50 particle size value of 10 mu m;
(2) mixing the raw material powder obtained in the step (1) with a petroleum asphalt binder according to the ratio of 92:8 for 2 hours to obtain a mixture 1,
(3) carrying out chemical modification on the mixed powder 1 obtained in the step (2) in a coating kettle under the protection of inert gas nitrogen, wherein the modification temperature is 650 ℃, and the treatment time is 10 hours, so as to obtain secondary particles with the particle size value of D50 being 17 microns;
(4) mixing the secondary particles obtained in the step (3) with phenolic resin according to a ratio of 96:4 for 4.5 hours to obtain a mixture 2;
(5) curing the mixture 2 obtained in the step (4) in a reaction kettle at a low temperature of 270 ℃ for 3h under the protection of inert gas nitrogen to obtain a hard carbon coated secondary particle precursor;
(6) graphitizing the hard carbon coated secondary particle precursor obtained in the step (5) in a graphitization furnace, wherein the graphitization temperature is 3100 ℃, and the graphitization time is 68h to obtain a graphitized product precursor;
(7) mixing the graphitized product precursor obtained in the step (6) with an organic solvent of asphalt according to the ratio of 1:20, wherein
The ratio of the asphalt to the organic solvent is 1:4, and then spray drying is carried out to obtain a precursor, wherein the temperature of the spray drying is 210 ℃.
(8) And (4) carbonizing the spray-dried precursor obtained in the step (7) for 6 hours at 1100 ℃ in a roller kiln under the protection of nitrogen atmosphere to obtain the high-compaction and fast-charging type lithium ion battery cathode material.
Comparative example 1
(1) Carrying out coarse crushing and fine crushing on needle coke green coke, and then carrying out spheroidizing, shaping and grading to obtain graphite raw material powder with the D50 particle size value of 8 mu m;
(2) mixing the raw material powder obtained in the step (1) with a petroleum asphalt binder according to a ratio of 90:10 for 2 hours to obtain a mixture 1,
(3) carrying out chemical modification on the mixed powder 1 obtained in the step (2) in a coating kettle under the protection of inert gas nitrogen, wherein the modification temperature is 650 ℃, and the treatment time is 8h, so as to obtain secondary particles with the particle size value of D50 being 15 mu m;
(4) graphitizing the secondary particle precursor obtained in the step (3) in a graphitizing furnace, wherein the graphitizing temperature is 3100 ℃, and the graphitizing time is 70h to obtain a graphitized product precursor;
(5) mixing the graphitized product precursor obtained in the step (4) with an organic solvent of asphalt according to the ratio of 1:25, wherein
The ratio of the asphalt to the organic solvent is 1:3, and then spray drying is carried out to obtain a precursor, wherein the temperature of the spray drying is 180 ℃.
(6) And (5) carbonizing the spray-dried precursor obtained in the step (5) for 8 hours at 1100 ℃ in a roller kiln under the protection of nitrogen atmosphere to obtain the high-compaction and fast-charging type lithium ion battery cathode material.
Comparative example 2
(1) Carrying out coarse crushing and fine crushing on needle coke calcined coke, and then carrying out spheroidizing, shaping and grading to obtain graphite raw material powder with the D50 particle size value of 8.5 mu m;
(2) mixing the raw material powder obtained in the step (1) with a petroleum asphalt binder according to a ratio of 85:15 for 2 hours to obtain a mixture 1,
(3) carrying out chemical modification on the mixed powder 1 obtained in the step (2) in a coating kettle under the protection of inert gas nitrogen, wherein the modification temperature is 700 ℃, and the treatment time is 8h, so as to obtain secondary particles with the D50 particle size value of 18 mu m;
(4) mixing the secondary particles obtained in the step (3) with phenolic resin according to the ratio of 95:5 for 5 hours to obtain a mixture 2;
(5) curing the mixture 2 obtained in the step (4) in a reaction kettle at a low temperature of 300 ℃ for 5 hours under the protection of inert gas nitrogen to obtain a hard carbon coated secondary particle precursor;
(6) graphitizing the hard carbon coated secondary particle precursor obtained in the step (5) in a graphitizing furnace, wherein the graphitizing temperature is 3200 ℃, and the graphitizing time is 75h to obtain a graphitized product precursor;
(7) directly mixing the graphitized product precursor obtained in the step (6) with asphalt powder according to the ratio of 98:2 to obtain a mixture 3, wherein the particle size value of the asphalt powder D50 is 2.5 mu m;
(8) and (3) carbonizing the mixture 3 obtained in the step (7) for 10 hours at 1050 ℃ in a roller kiln under the protection of nitrogen atmosphere to obtain the high-compaction fast-charging type lithium ion battery cathode material.
In order to verify the performance of the lithium ion battery cathode material obtained by the invention, the lithium ion battery cathode material is tested according to the conventional indexes and electrochemical performance, and the results are shown in the following table:
results and conclusions:
the lithium ion battery negative electrode materials prepared by the embodiments 1-4 have good effects in the tests of discharge capacity, first efficiency, charge capacity retention rate and pole piece compaction density items; in comparative example 1, the hard carbon coating was not performed, and from the results, the charge capacity retention rate of the obtained negative electrode material was low; in comparison 2, the coating is not carried out in a spray drying mode, but is directly coated by a solid phase, the surface of the prepared negative electrode material is rough, and cross-linking occurs among particles, so that the first efficiency is low, and the compaction density is low.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and those skilled in the art can easily conceive of the modifications or substitutions within the technical scope of the present invention, and the present invention shall be covered thereby. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
1. The high-compaction and fast-charging type lithium ion battery cathode material is characterized in that: the coating agent comprises graphite raw material powder, a hard carbon coating agent and a liquid coating agent, wherein the hard carbon coating agent comprises phenolic resin, and the liquid coating agent comprises a coating agent of asphalt dissolved in an aromatic solvent or a hydrocarbon solvent.
2. A method for producing a high-compaction and fast-charging type lithium ion battery cathode material is characterized by comprising the following specific production processes:
s1: carrying out coarse crushing and fine crushing on an artificial graphite raw material, and then carrying out spheroidizing, shaping and grading to obtain graphite raw material powder;
s2: mixing the raw material powder obtained in the step S1 with a binder according to a certain ratio to obtain a mixture 1;
s3: carrying out chemical modification treatment on the mixture 1 obtained in the step S2 under the protection of inert gas to obtain secondary particles;
s4: mixing the secondary particles obtained in the step S3 with a hard carbon coating agent to obtain a mixture 2;
s5: carrying out low-temperature curing treatment on the mixture 2 obtained in the step S4 under the protection of inert gas to obtain a hard carbon coated secondary particle precursor;
s6: performing high-temperature graphitization treatment on the hard carbon-coated secondary particle precursor obtained in the step S5 to obtain a graphitized product precursor;
s7: mixing the graphitized product precursor obtained in the step S6 with a liquid coating agent, and then carrying out spray drying to obtain a spray-dried precursor;
s8: and (5) carbonizing the spray-dried precursor obtained in the step (S7) under the protection of inert gas to obtain the lithium ion battery cathode material.
3. The method for producing the negative electrode material of the high-compaction and fast-charging lithium ion battery as claimed in claim 1, wherein the method comprises the following steps: in step S1, the artificial graphite raw material is raw coke or calcined coke, the raw coke is one or a combination of more of petroleum coke, pitch coke or needle coke, and the particle size value of the graphite raw material powder D50 is 6-10 μm.
4. The method for producing the negative electrode material of the high-compaction and fast-charging lithium ion battery as claimed in claim 1, wherein the method comprises the following steps: in step S2, the ratio of the raw material powder to the binder is 85:15-99:1, the binder is petroleum asphalt or coal asphalt, and the D50 particle size of the binder is 2-6 μm.
5. The method for producing the negative electrode material of the high-compaction and fast-charging lithium ion battery as claimed in claim 1, wherein the method comprises the following steps: in step S3, the temperature of the chemical modification treatment is 500-700 ℃, the treatment time is 8-15h, and the particle size D50 of the secondary particles is 12-20 μm.
6. The method for producing the negative electrode material of the high-compaction and fast-charging lithium ion battery as claimed in claim 1, wherein the method comprises the following steps: in step S4, the hard carbon coating agent is phenolic resin, and the ratio of the secondary particles to the hard carbon coating agent is 92:8-99: 1.
7. The method for producing the negative electrode material of the high-compaction and fast-charging lithium ion battery as claimed in claim 1, wherein the method comprises the following steps: in step S5, the low-temperature curing temperature is 90-300 ℃, and the curing time is 3-6 h.
8. The method for producing the negative electrode material of the high-compaction and fast-charging lithium ion battery as claimed in claim 1, wherein the method comprises the following steps: in step S6, the graphitization temperature is 3000-3200 ℃, and the graphitization treatment time is 60-75 h.
9. The method for producing the negative electrode material of the high-compaction and fast-charging lithium ion battery as claimed in claim 1, wherein the method comprises the following steps: in step S7, the liquid coating agent is a coating agent in which asphalt is dissolved in an aromatic solvent or a hydrocarbon solvent, and the temperature of the spray drying is 90 to 180 ℃.
10. The method for producing the negative electrode material of the high-compaction and fast-charging lithium ion battery as claimed in claim 1, wherein the method comprises the following steps: in step S8, the carbonization temperature is 1050-1250 ℃, and the constant temperature time is 6-10 h.
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