CN109503166B - Graphite cathode material for platform type lithium ion battery and preparation method thereof - Google Patents
Graphite cathode material for platform type lithium ion battery and preparation method thereof Download PDFInfo
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- CN109503166B CN109503166B CN201811149763.7A CN201811149763A CN109503166B CN 109503166 B CN109503166 B CN 109503166B CN 201811149763 A CN201811149763 A CN 201811149763A CN 109503166 B CN109503166 B CN 109503166B
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/522—Graphite
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/528—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components
- C04B35/532—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components containing a carbonisable binder
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- 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
- 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a graphite cathode material for a platform-type lithium ion battery and a preparation method thereof, wherein the graphite cathode material is formed by homogenizing, heat treating and centrifugally stirring and extruding geometric petroleum coke particles subjected to surface modification with a forming adhesive, wherein centrifugal extrusion force is formed on a mixed material in the heat treating and stirring processes, so that large planes of the petroleum coke particles with the geometric structure are mutually butted and formed, and the graphite particle cathode material with the micro platform-type structure is obtained. The graphite cathode material has the characteristics of platform model, structural stability, better strength and the like, enhances the volume density of graphite, reduces the secondary damage of the structure of particles in the processing process, can prolong the cycle life of the graphite particle material in a lithium battery application system, reduces surface negative reaction, gas generation, lithium dendrite and the like in the reaction process, and greatly improves the safety performance of the material.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a graphite cathode material for a platform type lithium ion battery and a preparation method thereof.
Background
In recent years, the lithium battery energy industry is rapidly developed, the lithium battery related industry is also rapidly developed synchronously, the worldwide prohibition of fuel automobiles is increased day by day, and the prohibition of fuel automobiles is scheduled to be promoted by a plurality of countries all over the world, so that the demand of graphite cathode materials is increased more and more. One of the important links in the preparation process of the graphite cathode material precursor is the formation of graphite micro-particle structure, which is related to the comprehensive performance of the graphite cathode material, and meanwhile, the reasonability of the design of the graphite micro-structure model is related to the reasonability of the application condition of the graphite material in the fields of power and the like. In the process of forming the precursor structure of the negative electrode material, the development of the graphite negative electrode material needs to be designed by taking key factors used by a lithium battery of a power automobile as guidance, and from the application perspective, the charging time, the cycle life and the safety performance are important consideration indexes.
However, the actual commercial microstructure forming mode of the graphite cathode material is relatively single at present, the artificial control capability of the finished product of the microstructure is not strong, randomness exists mostly, or the structure is subjected to compensation modification through later-stage reprocessing after forming, excessive resources are consumed, and the later-stage structural modification is often accompanied by the introduction of a plurality of side reaction factors, such as active points on the surface of graphite particles, and new uncertain factors are introduced into the safety performance of the material due to functional group denaturation, so that the application and the safety performance of the material cannot be guaranteed.
In view of the above, there is a need to research how to screen and prepare graphite particles with similar geometric microstructures; how to screen a proper graphite particle adhesive to ensure the fluidity required by the forming of the platform-shaped structure; how to make a heat treatment mode through the thermal reaction characteristics of the adhesive and the graphite original particles so that the adhesive and the graphite original particles can be fully contacted to form a platform-type structure; how to formulate suitable former through the binder and graphite primary particle self thermal reaction characteristic and make it form the platform type structure graphite particle that possesses stronger structural strength, and then overcome the shortcoming of current graphite anode material.
Disclosure of Invention
The invention aims to provide a graphite cathode material for a platform type lithium ion battery and a preparation method thereof aiming at the defects of the prior art, wherein graphite microscopic particles have the characteristics of platform models, structural stability, better strength and the like, the volume density of graphite is enhanced, the secondary damage of the structure of the particles in the processing process is reduced, the cycle life of the particles can be prolonged, the surface negative reaction, gas generation in the reaction process, lithium dendrite and the like are reduced, and the safety performance of the material is greatly improved.
The technical scheme adopted by the invention to achieve the aim is as follows:
the graphite cathode material for the platform-type lithium ion battery is formed by homogenizing petroleum coke particles with a surface-modified geometric body and an adhesive, performing heat treatment and performing centrifugal stirring and extrusion at the same time. This kind of platform type structure model graphite negative electrode material structure further strengthens graphite granule stability and shaping structural strength, overcomes the anti-destructiveness of graphite negative electrode material structure in the course of working simultaneously, and then the security performance of reinforcing material avoids graphite granule to take place side reaction in lithium cell module working process.
Preferably, the surface modification comprises chamfering, grinding and screening acicular petroleum coke particles; the surface modification can reduce the surface defects of the independent particles, and avoid the generation defects of the platform-type particles and the influence on the structural strength of the formed particles caused by the surface defects of the independent particles in the particle forming process. The graphite cathode material for the platform type lithium ion battery has a platform model, structural stability and graphitized particles with good strength.
Preferably, the acicular petroleum coke particles have a median particle diameter DV50 of 5-30 μm.
Preferably, the mass percentage of the petroleum coke particles and the forming adhesive is 1-30% of the petroleum coke particles and 70-99% of the adhesive.
Preferably, the median particle diameter DV50 of the molding adhesive is 1-20 μm. Preferably, the molding adhesive is a high polymer adhesive, and the high polymer adhesive is one or more of coal, oil-based asphalt or phenolic resin.
The preparation method of the graphite cathode material for the platform-type lithium ion battery comprises the following steps:
s1: modifying the surface of the acicular petroleum coke particles, including removing edges and corners, grinding, screening and distributing materials to obtain modified petroleum coke particles with a similar geometric structure;
s2: mixing petroleum coke particles with a similar geometric structure and a forming adhesive, homogenizing to obtain a mixed material, then carrying out heat treatment on the mixed material, simultaneously stirring the mixed material at a high speed in a fixed heat reaction container, forming centrifugal extrusion force on the mixed material, and carrying out butt joint forming on large planes of the petroleum coke particles with the similar geometric structure by the forming adhesive under the action of strong centrifugal force to obtain the graphite particles with the micro-platform structure.
The optimized forming adhesive has good heating characteristic, after the raw materials are homogenized, a reasonable heat treatment process is set by combining the heating characteristic of the adhesive and the heating characteristic of the graphite particles, the materials move in the fixed thermal reaction container in the heat treatment process, and simultaneously, centrifugal extrusion force with different degrees is generated on the materials in the temperature rising process through the stirring structure and the control of the temperature and the stirring linear speed. The independent graphite granule of geometric structure is at the forming process, owing to accept under stronger external force effect, and two planes that granule surface area is less can't stably dock because of the effect of external force, all are switched to the great plane of granule and granule surface and great plane formation butt joint, and the shaping is docked each other to big plane. Because the bonding area is bigger, so the strength among independent particles also correspondingly reaches the maximization, provide the powerful guarantee for the generation of the microcosmic platform type structure and the strength of the generated structure, simultaneously because of the secondary particles formed under the condition of high linear velocity, the surface of the formed particles is greatly reduced because of bonding the graphite particles with unstable structures, after the forming, the proper linear velocity (3-20m/s) is matched, simultaneously along with the rise of the temperature, the bonding force of the bonding agent is strengthened, the graphite particle structure is further stabilized, thereby the graphitized particles with platform models, good structural stability and strength are obtained, and the safety, the processing and the application performance of the graphite can be greatly improved.
Preferably, the heat treatment process is temperature programmed under a protective atmosphere, the temperature rise rate is 10-15 ℃/min, and the heat treatment temperature range is 500-900 ℃.
Preferably, the ratio of the internal volume of the fixed thermal reaction vessel to the volume of the mixed material is 3-5: 1.
Preferably, the high-speed stirring is 600-1200 r/min.
Compared with the prior art, the invention has the following beneficial effects:
1. the graphite cathode material for the platform-type lithium ion battery and the preparation method thereof are formed by homogenizing, heat treating and centrifugally stirring and extruding geometric petroleum coke particles subjected to surface modification of needle-shaped petroleum coke particles and an adhesive, and the graphitized particles have platform models, structural stability and better strength.
2. Compared with the graphite particles applied at present, the graphite particle micro-structure platform is innovatively flattened, so that the volume density of the graphite can be further enhanced, the energy purpose of graphite application design and the graphitization charging amount of the graphite in the processing process can be improved, and the processing cost is reduced.
3. The graphite particles with the platform-type structures have better structural strength and stability, can effectively reduce the secondary damage of the structures of the particles in the processing process, and can prolong the cycle life of the particles.
4. The graphite particles with the platform-shaped structure are reasonably stacked, so that the damage degree of rolled particles after film coating can be reduced, the generation of new end faces due to damage is reduced, the cycle life of the material is prolonged, the surface negative reaction is reduced, the conditions of gas generation, lithium dendrite formation and the like in the reaction process are reduced, and the safety performance of the material is greatly improved.
The above is an overview of the technical solutions of the present invention, and the present invention is further described below with reference to the accompanying drawings and the detailed description thereof.
Drawings
Fig. 1 is an electron microscope picture of the graphite anode material for the platform-type lithium ion battery in example 1;
fig. 2 is another electron microscope picture of the graphite anode material for the platform-type lithium ion battery in this example 1;
FIG. 3 is a schematic representation of the microstructure of a prior art conventional graphite particle after coating with a film;
FIG. 4 is a schematic view of the microstructure of a conventional graphite particle coated film of the prior art after rolling;
FIG. 5 is a schematic view of the microstructure of the modified petroleum coke particles of the present embodiment;
FIG. 6 is a schematic view showing the microstructure of the flat-bed shaped graphite particles in this example;
fig. 7 is a schematic view of the microstructure of the flat-bed shaped graphite particles of this example after rolling.
The specific implementation mode is as follows:
in order to make the objects, technical solutions and advantages of the present invention more apparent, the following detailed description is made with reference to the accompanying drawings and examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the accompanying fig. 3-7, the black part represents graphite particles, and the schematic microstructure of the conventional graphite particles after coating film in fig. 3 shows that there are many internal voids between the formed graphite particles, which affects the volume density of graphite. The microstructure schematic diagram of the rolled conventional graphite particle coating film in fig. 4 shows that the particles are destroyed and shifted after the rolling of the pole piece, and a new active end face with strong side reaction is generated. The individual graphite particles screened after modification can be seen in fig. 5 to have a geometry-like structure. Fig. 6 shows that the flat-bed formed graphite particles have small internal void defects and high bulk density. It can be seen in fig. 7 that the platform-shaped formed graphite particles have a large bonding area, good stability, and high structural strength, and are not easily damaged.
Example 1: the preparation method of the graphite cathode material for the platform-type lithium ion battery and the graphite cathode material thereof comprise the following steps: firstly, modifying the surface of acicular petroleum coke particles, including edge angle removal, grinding, screening and material distribution, to obtain modified petroleum coke particles with a geometric structure; wherein the median diameter DV50 of needle petroleum coke particles is 5-30 μm. The geometric structure can be a cuboid-like structure or a cube-like structure.
Then mixing the petroleum coke particles with the geometric structure with a forming adhesive and homogenizing to obtain a mixed material, wherein the median particle diameter DV50 of the forming adhesive is 1-20 μm. The forming adhesive is high polymer adhesive oil asphalt; the mass percentage of the petroleum coke particles and the forming adhesive is 30 percent of the petroleum coke particles and 70 percent of the adhesive.
And then carrying out heat treatment on the mixed material, wherein the heat treatment process is temperature programming under a protective atmosphere, the temperature rise rate is 10 ℃/min, and the heat treatment temperature range is 900 ℃. And simultaneously stirring the mixed materials in a fixed thermal reaction container at a high speed, wherein the ratio of the internal volume of the fixed thermal reaction container to the volume of the mixed materials is 3:1, and the high-speed stirring speed is 1000 r/min. The temperature and the linear speed in the stirring process are controlled to form centrifugal extrusion force on the mixed material, and the forming adhesive enables large planes of petroleum coke particles with similar geometric structures to be mutually butted and formed under the action of strong centrifugal force, so that the graphite particles with the micro-platform structure are obtained, and the graphite particles are graphitized particles with platform models, structural stability and better strength.
Example 2: the preparation method of the graphite cathode material for the platform-type lithium ion battery and the graphite cathode material thereof comprise the following steps: firstly, modifying the surface of acicular petroleum coke particles, including edge angle removal, grinding, screening and material distribution, to obtain modified petroleum coke particles with a geometric structure; wherein the median diameter DV50 of needle petroleum coke particles is 5-30 μm.
Then mixing the petroleum coke particles with the geometric structure with a forming adhesive and homogenizing to obtain a mixed material, wherein the median particle diameter DV50 of the forming adhesive is 1-20 μm. The forming adhesive is high polymer coal pitch; the mass percentage of the petroleum coke particles and the forming adhesive is 20 percent of the petroleum coke particles and 80 percent of the adhesive.
And then carrying out heat treatment on the mixed material, wherein the heat treatment process is temperature programming under a protective atmosphere, the temperature rise rate is 12 ℃/min, and the heat treatment temperature range is 500 ℃. And simultaneously stirring the mixed materials in a fixed thermal reaction container at a high speed, wherein the ratio of the internal volume of the fixed thermal reaction container to the volume of the mixed materials is 5:1, and the high-speed stirring speed is 600r/min, so that the graphite particles with the micro-platform structure are obtained, and the graphite particles are graphitized particles with platform models, structural stability and better strength.
Example 3: the preparation method of the graphite cathode material for the platform-type lithium ion battery and the graphite cathode material thereof comprise the following steps: firstly, modifying the surface of acicular petroleum coke particles, including edge angle removal, grinding, screening and material distribution, to obtain modified petroleum coke particles with a geometric structure; wherein the median diameter DV50 of needle petroleum coke particles is 5-30 μm.
Then mixing the petroleum coke particles with the geometric structure with a forming adhesive and homogenizing to obtain a mixed material, wherein the median particle diameter DV50 of the forming adhesive is 1-20 μm. The forming adhesive is one or more of high polymer adhesive phenolic resin; the mass percentage of the petroleum coke particles and the forming adhesive is 10 percent of the petroleum coke particles and 90 percent of the adhesive.
And then carrying out heat treatment on the mixed material, wherein the heat treatment process is temperature programming under a protective atmosphere, the temperature rise rate is 13 ℃/min, and the heat treatment temperature range is 800 ℃. And simultaneously stirring the mixed materials in a fixed thermal reaction container at a high speed, wherein the ratio of the internal volume of the fixed thermal reaction container to the volume of the mixed materials is 4:1, and the high-speed stirring speed is 900 r/min. The graphite particles with the microscopic platform type structure are obtained, and are graphitized particles with platform models, structural stability and better strength.
Variations and modifications to the above-described embodiments may occur to those skilled in the art, which fall within the scope and spirit of the above description. Therefore, the above description is not intended to limit the invention, and the invention is not limited to the above disclosed and described embodiments, and modifications and variations of the invention, such as equivalent substitutions of each raw material and addition of auxiliary components, selection of specific modes, etc., made by those skilled in the art within the spirit of the embodiments, should also fall within the scope of the claims of the present invention.
Claims (2)
1. A method for preparing a graphite cathode material for a platform type lithium ion battery is characterized by comprising the following steps:
s1: modifying the surface of the acicular petroleum coke particles, including removing edges and corners, grinding, screening and distributing materials to obtain modified petroleum coke particles with a similar geometric structure; the quasi-geometric structure is a quasi-cuboid structure or a quasi-cube structure; the median diameter DV50 of the acicular petroleum coke particles is 5-30 μm;
s2: mixing petroleum coke particles with a similar geometric structure and a forming adhesive, homogenizing to obtain a mixed material, then carrying out heat treatment on the mixed material, simultaneously stirring the mixed material at a high speed in a fixed heat reaction container to form centrifugal extrusion force on the mixed material, and mutually butting and forming large planes of the petroleum coke particles with the similar geometric structure by the forming adhesive under the action of strong centrifugal force to obtain graphite particles with a micro-platform structure; the median particle diameter DV50 of the forming adhesive is 1-20 μm; the mass percentage of the similar geometric petroleum coke particles and the forming adhesive is 10-30% of the similar geometric petroleum coke particles and 70-90% of the adhesive; the heat treatment process is temperature programmed under protective atmosphere, the temperature rise rate is 10-15 ℃/min, and the heat treatment temperature range is 500-900 ℃; the ratio of the internal volume of the fixed thermal reaction container to the volume of the mixed material is 3-5: 1; the high-speed stirring is 600-1200 r/min.
2. The graphite negative electrode material for the platform-type lithium ion battery is characterized by being obtained by the preparation method of the graphite negative electrode material for the platform-type lithium ion battery according to claim 1, wherein the forming adhesive is a high polymer adhesive, and the high polymer adhesive is one or more of coal, oil-based asphalt or phenolic resin.
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