CN116053479A - Graphitization production process of lithium battery cathode material - Google Patents

Graphitization production process of lithium battery cathode material Download PDF

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Publication number
CN116053479A
CN116053479A CN202310155105.3A CN202310155105A CN116053479A CN 116053479 A CN116053479 A CN 116053479A CN 202310155105 A CN202310155105 A CN 202310155105A CN 116053479 A CN116053479 A CN 116053479A
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graphitization
production process
negative electrode
electrode material
lithium battery
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吕军超
刘人杰
郭琴
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Baoxing Yida Photovoltaic Blade Material Co ltd
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Baoxing Yida Photovoltaic Blade Material Co ltd
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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
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/20—Graphite
    • C01B32/205—Preparation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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    • Y02E60/10—Energy storage using batteries

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Abstract

The invention relates to the technical field of negative electrode materials, in particular to a graphitization production process of a lithium battery negative electrode material. Which comprises the following steps: washing the carbon material with water, grinding to obtain particles, and adding asphalt for mixing and coating to obtain a coating material; putting the coating material into a stirring container, putting a forming agent and deionized water into the stirring container, uniformly stirring the coating material, and performing demagnetizing treatment to generate mixed slurry; heating the mixed slurry to remove water and generate material slurry, and placing the material slurry in a crucible to preheat in a nitrogen atmosphere; and transferring the crucible into a graphitizing furnace for heating graphitization to generate a negative electrode material, and cooling to take out the negative electrode material. According to the invention, the three-dimensional highly cross-linked network structure of the resin pyrolytic carbon and the carbon black are matched to form the conductive network, so that the discharge effect of the anode material can be ensured, the disordered carbon structure in the anode material is converted into a crystalline structure similar to graphite after graphitization, and the interlayer spacing is reduced, so that the discharge effect of the anode material is ensured.

Description

Graphitization production process of lithium battery cathode material
Technical Field
The invention relates to the technical field of negative electrode materials, in particular to a graphitization production process of a lithium battery negative electrode material.
Background
In order to ensure the discharge performance of the lithium ion battery, the intercalation oxidation-reduction potential of lithium ions in the negative electrode matrix needs to be as low as possible and close to the potential of metallic lithium, so that the input voltage of the battery is high, and the structure of the negative electrode main body is not or little changed in the intercalation/deintercalation process.
The preparation method adopts a microwave vapor deposition method to prepare the carbon nano tube/graphene composite negative electrode material in situ, does not need a pre-synthesis process to reduce the production cost, adopts microwave heating, is high in efficiency and low in energy consumption, has short production period, reduces the irreversible capacity of first charge and discharge due to the fact that the carbon nano tube/graphene composite negative electrode material is contained, has good safety and high power, and is convenient for the first charge and discharge of lithium ions to be reduced by only containing the carbon nano tube/graphene composite negative electrode material in the preparation method.
In order to enable the lithium battery anode material to have a better discharge effect, a graphitization process of the lithium battery anode material is provided.
Disclosure of Invention
The invention aims to provide a graphitization production process of a lithium battery anode material, which aims to solve the problems in the background technology.
In order to achieve the above object, the present invention provides a graphitization production process of a lithium battery anode material, comprising the following steps:
s1, washing a carbon material with water, grinding the carbon material into particles, and adding asphalt for mixing and coating to generate a coating material;
s2, putting the coating material into a stirring container, putting a forming agent and deionized water into the stirring container, uniformly stirring the coating material, and performing demagnetizing treatment to generate mixed slurry;
s3, heating the mixed slurry to remove water to generate material slurry, and placing the material slurry in a crucible to preheat in a nitrogen atmosphere;
s4, transferring the crucible into a graphitization furnace for heating graphitization to generate a negative electrode material, and cooling to take out the negative electrode material.
As a further improvement of the technical scheme, in the step S1, the carbon material is resin pyrolytic carbon prepared by using phenolic resin as a precursor.
As a further improvement of the present technical solution, in S1, the coating method is a chemical vapor deposition method.
As a further improvement of the technical scheme, in the step S2, the forming agent comprises polyacrylic acid and carbon black, wherein the weight ratio of the polyacrylic acid to the carbon black is 9:1.
As a further improvement of the technical scheme, in the step S2, the stirring rotation speed is 40-60rpm/min.
As a further improvement of the technical scheme, in the step S3, the preheating temperature is 80-180 ℃.
As a further improvement of the technical scheme, in the step S3, the water content of the material slurry is 0.05-0.20%.
As a further improvement of the technical scheme, in the S4, the graphitization temperature is 2450-2850 ℃.
As a further improvement of the technical scheme, in the S4, the graphitization time is 8-15h.
According to the invention, resin pyrolytic carbon prepared by taking phenolic acid resin as a precursor is used as a carbon source of the anode material, a three-dimensional highly crosslinked network structure of the resin pyrolytic carbon is utilized, and high chemical bond energy among carbon atoms in benzene rings is utilized to provide cohesive force among chains of molecules, so that the stability of the structure is enhanced.
Compared with the prior art, the invention has the beneficial effects that:
in the graphitization production process of the lithium battery anode material, the three-dimensional highly crosslinked network structure of the resin pyrolytic carbon is utilized, the high chemical bond energy between carbon atoms in benzene rings is utilized to provide cohesive force between chains of molecules, the stability of the structure is enhanced, the influence of lithium ion insertion/deintercalation on the structure can be reduced, the pulverization amplitude of the structure is reduced, the discharge effect of the anode material can be ensured after the carbon black is matched with the conductive network, the disordered carbon structure in the anode material is converted into a crystalline structure similar to graphite after graphitization, and the layer spacing is reduced, so that the discharge effect of the anode material is ensured.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1, the invention aims to provide a graphitization production process of a lithium battery anode material, which comprises the following steps:
s1, washing a carbon material with water, grinding the carbon material to be granular, adding asphalt, mixing and coating to generate a coating material, wherein the carbon material is resin pyrolytic carbon prepared by taking phenolic resin as a precursor, the phenolic resin belongs to thermosetting resin, a cured structure shows a three-dimensional network high-crosslinking characteristic, the main structure of the carbon material is a benzene ring structure with a large proportion, the chemical bond energy among carbon atoms is high, the cohesive force among chains of molecules is large, the phenolic resin has the characteristics of high carbon residue rate and strong carbon forming capability after pyrolysis, the cyclic discharge efficiency of the anode material is improved, the coating mode is a chemical vapor deposition method, namely, chemical substances in a gaseous state or a vapor state are formed into solid deposits on a gas-solid interface through chemical reaction in a heating, plasma excitation or light radiation mode, and a layer of amorphous asphalt is deposited on the surface of the carbon material to form a shell structure, so that the volume expansion or structural damage of the active center of the anode material is restrained and buffered, and the stability of the anode material is maintained;
s2, putting the coating material into a stirring container, putting a forming agent and deionized water, stirring uniformly at a rotating speed of 40-60rpm/min, and then performing demagnetizing treatment to generate mixed slurry, wherein the forming agent comprises polyacrylic acid and carbon black, the weight ratio of the polyacrylic acid to the carbon black is 9:1, the polyacrylic acid is used as an aqueous binder, the material is polymerized and formed in an electrolyte charge adsorption mode, the specific surface area of carbon black particles is large, a conductive network in a negative electrode material can be formed, and the coating material and the forming agent can be fully contacted in a stirring mode, so that uniformly mixed material slurry is generated;
s3, heating the mixed slurry to remove water and generate material slurry, and placing the material slurry in a crucible to preheat in a nitrogen atmosphere, wherein the preheating temperature is 80-180 ℃, excessive water in the material slurry is removed through preheating by preheating the material slurry, and the material slurry is heated in the nitrogen atmosphere, so that the introduction of impurities can be avoided, the water content of the material slurry is 0.05-0.20%, and the stability of the internal structure of the anode material can be influenced when the water content is too low or too high;
s4, transferring the crucible into a graphitization furnace, heating and graphitizing for 8-15 hours at 2450-2850 ℃ to generate a negative electrode material, cooling and taking out the negative electrode material, wherein the graphitization can change a carbon structure in the negative electrode material from disorder to order, realize solidification of the negative electrode material, improve the electrical conductivity of the negative electrode material, and facilitate complete graphitization of the negative electrode material by long-time high-temperature heating, thereby being beneficial to improving the performance of the negative electrode material.
According to the invention, resin pyrolytic carbon prepared by taking phenolic acid resin as a precursor is used as a carbon source of the anode material, a three-dimensional highly crosslinked network structure of the resin pyrolytic carbon is utilized, and high chemical bond energy among carbon atoms in benzene rings is utilized to provide cohesive force among chains of molecules, so that the stability of the structure is enhanced.
According to the difference of technological parameters in the production process, the graphitization production process of the lithium battery anode material provided by the invention is further described through the following specific examples.
Example 1
S1, washing a carbon material with water, grinding the carbon material to be granular, adding asphalt, mixing and coating to generate a coating material, wherein the carbon material is resin pyrolytic carbon prepared by taking phenolic resin as a precursor, and the coating mode is a chemical vapor deposition method;
s2, putting the coating material into a stirring container, putting a forming agent and deionized water, stirring uniformly at a rotating speed of 40rpm/min, and then performing demagnetizing treatment to generate mixed slurry, wherein the forming agent comprises polyacrylic acid and carbon black, and the weight ratio of the polyacrylic acid to the carbon black is 9:1;
s3, heating the mixed slurry to remove water to generate material slurry, and placing the material slurry in a crucible to preheat in a nitrogen atmosphere, wherein the preheating temperature is 80 ℃, and the water content of the material slurry is 0.05%;
s4, transferring the crucible into a graphitization furnace, heating and graphitizing for 8 hours at 2450 ℃ to generate a negative electrode material, and cooling to take out the negative electrode material.
Example 2
S1, washing a carbon material with water, grinding the carbon material to be granular, adding asphalt, mixing and coating to generate a coating material, wherein the carbon material is resin pyrolytic carbon prepared by taking phenolic resin as a precursor, and the coating mode is a chemical vapor deposition method;
s2, putting the coating material into a stirring container, putting a forming agent and deionized water, stirring uniformly at a rotating speed of 50rpm/min, and then performing demagnetizing treatment to generate mixed slurry, wherein the forming agent comprises polyacrylic acid and carbon black, and the weight ratio of the polyacrylic acid to the carbon black is 9:1;
s3, heating the mixed slurry to remove water to generate material slurry, and placing the material slurry in a crucible to preheat in a nitrogen atmosphere, wherein the preheating temperature is 140 ℃, and the water content of the material slurry is 0.12%;
s4, transferring the crucible into a graphitization furnace, heating and graphitizing for 10 hours at the temperature of 2700 ℃ to generate a negative electrode material, and cooling to take out the negative electrode material.
Example 3
S1, washing a carbon material with water, grinding the carbon material to be granular, adding asphalt, mixing and coating to generate a coating material, wherein the carbon material is resin pyrolytic carbon prepared by taking phenolic resin as a precursor, and the coating mode is a chemical vapor deposition method;
s2, putting the coating material into a stirring container, putting a forming agent and deionized water, stirring uniformly at a rotating speed of 60rpm/min, and then performing demagnetizing treatment to generate mixed slurry, wherein the forming agent comprises polyacrylic acid and carbon black, and the weight ratio of the polyacrylic acid to the carbon black is 9:1;
s3, heating the mixed slurry to remove water to generate material slurry, and placing the material slurry in a crucible to preheat in a nitrogen atmosphere, wherein the preheating temperature is 180 ℃, and the water content of the material slurry is 0.20%;
s4, transferring the crucible into a graphitization furnace, heating and graphitizing for 15 hours at 2850 ℃ to generate a negative electrode material, and cooling to take out the negative electrode material.
Example 4
S1, washing a carbon material with water, grinding the carbon material to be granular, adding asphalt, mixing and coating to generate a coating material, wherein the carbon material is resin pyrolytic carbon prepared by taking phenolic resin as a precursor, and the coating mode is a chemical vapor deposition method;
s2, putting the coating material into a stirring container, putting a forming agent and deionized water, stirring uniformly at a rotating speed of 45rpm/min, and then performing demagnetizing treatment to generate mixed slurry, wherein the forming agent comprises polyacrylic acid and carbon black, and the weight ratio of the polyacrylic acid to the carbon black is 9:1;
s3, heating the mixed slurry to remove water and generate material slurry, and placing the material slurry in a crucible to preheat in a nitrogen atmosphere, wherein the preheating temperature is 150 ℃, and the water content of the material slurry is 0.15%;
s4, transferring the crucible into a graphitization furnace, heating and graphitizing for 12 hours at 2800 ℃ to generate a negative electrode material, and cooling to take out the negative electrode material.
Table 1 comparative process parameters in examples 1-4
Figure BDA0004092047980000061
Comparative example 1
The production process of example 1 was adopted in this comparative example, the stirring rotation speed was set to 30rpm/min, the rest was unchanged, the specific steps were similar to those of example 1, and the description of this comparative example was omitted.
Comparative example 2
The production process of example 2 is adopted in this comparative example, the stirring rotation speed is set to 80rpm/min, the rest is unchanged, the specific steps are similar to those of example 2, and the description of this comparative example is omitted.
Table 2 comparative process parameters comparative examples 1-2
Figure BDA0004092047980000062
Figure BDA0004092047980000071
Comparative example 3
The production process of example 3 is adopted in this comparative example, the preheating temperature is set to 65 ℃, the rest is unchanged, the specific steps are similar to those of example 3, and the description of this comparative example is omitted.
Comparative example 4
The production process of example 4 is adopted in this comparative example, the preheating temperature is set to 200 ℃, the rest is unchanged, the specific steps are similar to those of example 4, and the description of this comparative example is omitted.
Table 3 comparative process parameters comparative examples 3-4
Figure BDA0004092047980000072
Comparative example 5
The production process of example 1 is adopted in this comparative example, the water content of the material slurry is set to be 0.25%, the rest is unchanged, the specific steps are similar to those of example 1, and the description of this comparative example is omitted.
Comparative example 6
The production process of example 2 is adopted in this comparative example, the water content of the material slurry is set to be 0.30%, the rest is unchanged, the specific steps are similar to those of example 2, and the comparative example is not repeated.
Table 4 comparative process parameters comparative examples 5-6
Figure BDA0004092047980000073
Comparative example 7
The production process of example 3 is adopted in this comparative example, the graphitization temperature is set to 2400 ℃, the rest is unchanged, the specific steps are similar to those of example 3, and the description of this comparative example is omitted.
Comparative example 8
The production process of example 4 is adopted in this comparative example, the graphitization temperature is set to 2950 ℃, the rest is unchanged, the specific steps are similar to those of example 4, and the comparative example is not repeated.
Table 5 comparative process parameters comparative examples 7-8
Figure BDA0004092047980000081
Comparative example 9
The production process of example 1 is adopted in this comparative example, the graphitization time is set to 5h, the rest is unchanged, the specific steps are similar to those of example 1, and the comparative example is not repeated.
Comparative example 10
The production process of example 2 is adopted in this comparative example, the graphitization time is set to 15h, the rest is unchanged, the specific steps are similar to those of example 2, and the comparative example is not repeated.
Table 6 comparative process parameters comparative examples 9-10
Figure BDA0004092047980000082
Test examples
The negative electrode materials were produced according to the graphitization production process of a lithium battery negative electrode material provided in examples 1 to 4 and comparative examples 1 to 10, respectively, and the first discharge capacity and the first discharge efficiency of the negative electrode materials were tested according to GB/T24533-2019 lithium ion battery graphite-type negative electrode material and are filled in Table 7 via data.
Table 7 comparison of discharge effects of anode materials produced in examples and comparative examples
First discharge capacity/(mA.h)/g First discharge efficiency/%
Example 1 370 94
Example 2 374 96
Example 3 369 93
Example 4 372 95
Comparative example 1 364 89
Comparative example 2 368 92
Comparative example 3 364 89
Comparative example 4 367 91
Comparative example 5 362 88
Comparative example 6 366 90
Comparative example 7 362 88
Comparative example 8 364 89
Comparative example 9 365 90
Comparative example 10 368 92
As can be seen from Table 7, the graphitization process for producing a negative electrode material for a lithium battery according to examples 1 to 4 was compared with the graphitization process for producing a negative electrode material for a lithium battery according to comparative examples 1 to 10, the first discharge capacity and the first discharge efficiency of the negative electrode material produced according to the example process were higher than those of the negative electrode material produced according to the comparative example process, and the first discharge capacity and the first discharge efficiency of the negative electrode material produced according to the example process were higher than 369 (mA.h)/g, and the first discharge efficiency was higher than 93%, and the first discharge capacity and the first discharge efficiency of the negative electrode material produced according to the comparative example process of different process parameters were reduced, so that the graphitization process for producing a negative electrode material for a lithium battery according to the invention can produce a negative electrode material having a good discharge effect.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the above-described embodiments, and that the above-described embodiments and descriptions are only preferred embodiments of the present invention, and are not intended to limit the invention, and that various changes and modifications may be made therein without departing from the spirit and scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (9)

1. The graphitization production process of the lithium battery cathode material is characterized by comprising the following steps of:
s1, washing a carbon material with water, grinding the carbon material into particles, and adding asphalt for mixing and coating to generate a coating material;
s2, putting the coating material into a stirring container, putting a forming agent and deionized water into the stirring container, uniformly stirring the coating material, and performing demagnetizing treatment to generate mixed slurry;
s3, heating the mixed slurry to remove water to generate material slurry, and placing the material slurry in a crucible to preheat in a nitrogen atmosphere;
s4, transferring the crucible into a graphitization furnace for heating graphitization to generate a negative electrode material, and cooling to take out the negative electrode material.
2. The graphitization production process of the negative electrode material of the lithium battery according to claim 1, wherein the graphitization production process is characterized in that: in the step S1, the carbon material is resin pyrolytic carbon prepared by taking phenolic resin as a precursor.
3. The graphitization production process of the negative electrode material of the lithium battery according to claim 1, wherein the graphitization production process is characterized in that: in the step S1, the coating mode is a chemical vapor deposition method.
4. The graphitization production process of the negative electrode material of the lithium battery according to claim 1, wherein the graphitization production process is characterized in that: in the step S2, the forming agent comprises polyacrylic acid and carbon black, wherein the weight ratio of the polyacrylic acid to the carbon black is 9:1.
5. The graphitization production process of the negative electrode material of the lithium battery according to claim 1, wherein the graphitization production process is characterized in that: in the step S2, the stirring rotation speed is 40-60rpm/min.
6. The graphitization production process of the negative electrode material of the lithium battery according to claim 1, wherein the graphitization production process is characterized in that: in the step S3, the preheating temperature is 80-180 ℃.
7. The graphitization production process of the negative electrode material of the lithium battery according to claim 1, wherein the graphitization production process is characterized in that: in the step S3, the water content of the material slurry is 0.05-0.20%.
8. The graphitization production process of the negative electrode material of the lithium battery according to claim 1, wherein the graphitization production process is characterized in that: in the step S4, the graphitization temperature is 2450-2850 ℃.
9. The graphitization production process of the negative electrode material of the lithium battery according to claim 1, wherein the graphitization production process is characterized in that: in the step S4, the graphitization time is 8-15h.
CN202310155105.3A 2023-02-23 2023-02-23 Graphitization production process of lithium battery cathode material Pending CN116053479A (en)

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