CN110395725B - Quick-charging microcrystalline graphite negative electrode material and preparation method thereof - Google Patents
Quick-charging microcrystalline graphite negative electrode material and preparation method thereof Download PDFInfo
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- 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
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The invention discloses a preparation method of a quick-charging type microcrystalline graphite cathode material, which comprises the steps of mixing microcrystalline graphite waste with an additive, transferring the mixed material into granulation equipment, and carrying out composite granulation under the inert atmosphere condition to obtain composite particles; and after cooling the composite particles, carrying out twice classification by a classifier, transferring the twice-classified composite particles into a carbonization furnace for carbonization, and then naturally cooling, scattering, demagnetizing and screening to obtain the quick-charging microcrystalline graphite cathode material. The invention solves the problems that the microcrystalline graphite waste material in the prior art has overhigh specific surface area, low tap density and difficult manufacture of the fast-charging type cathode material.
Description
Technical Field
The invention relates to the technical field of lithium ion battery cathode materials, in particular to a quick-charging microcrystalline graphite cathode material and a preparation method thereof.
Background
With the continuous acceleration of life rhythm and the explosive increase of information circulation, people have stronger and stronger dependence on daily tools at their sides and also put higher requirements on their performances. As the most important portable secondary power source, lithium ions have been widely used in various daily tools, such as mobile phones, I-Watch, notebook computers, electric vehicles, etc., however, the current lithium ion battery generally has a problem of slow charging speed, which greatly affects the comfort of people when using corresponding daily tools. Therefore, the development of fast-charging lithium ion batteries has become a major current direction.
The negative electrode material is one of the keys influencing the quick charge performance of the lithium ion battery, and the most commonly used negative electrode material at present is a graphite material. In order to improve the quick charging performance of the graphite cathode material, researchers make a large number of attempts, and finally confirm that two approaches for solving the quick charging performance of the graphite material are mainly used, namely, coal-series and other square cokes are selected as raw materials of graphite, and the graphite cathode material with the quick charging performance can be obtained by utilizing the isotropy of the equal square cokes; the second approach is post-processing, which improves the rapid lithium intercalation capability of graphite materials by coating or composite granulation.
However, the iso-square coke scheme is difficult to industrialize in a short time, which is mainly limited by the poor quality and the impracticality of the iso-square coke in China, and the iso-square coke in foreign countries cannot be exported to China due to the security limit of the nuclear graphite technology. Therefore, no equiaxed square coke graphite negative electrode material exists at home.
Therefore, post-processing methods have been focused on people. In order to realize the 10C fast charging of the graphite negative electrode, the patents [ JP10294111 ] and [ CN105024043A ] both use natural graphite as a raw material, and improve the fast charging performance of the graphite negative electrode by means of coating and granulating respectively, but the cycle performance of the natural graphite is inferior to that of artificial graphite, so the application range of the natural graphite is small. Patent [ CN106981632A ] uses pitch coke or petroleum coke as raw material, and a fast-charging graphite cathode material is obtained by a way of granulating first and then coating, and the material also avoids the problem of poor circulation of natural graphite, however, the process steps are complicated, the production cost is high, and the process is only suitable for high-end lithium ion batteries.
The microcrystalline graphite has low strength, a large amount of fine powder is easily generated in the machining process, the powder preparation yield is difficult to exceed 40%, and the generated fine powder of about 60% can be treated as waste solids. The invention takes the microcrystalline graphite waste produced by a graphite mining plant as a raw material, utilizes the characteristic that the microcrystalline graphite is similar to an equi-square coke structure, and prepares the high-cost-performance fast-charging microcrystalline graphite cathode material by a composite granulation process.
Disclosure of Invention
The invention provides a quick-charging type microcrystalline graphite negative electrode material and a preparation method thereof, aiming at overcoming the defects of the prior art.
The invention is realized by the following technical scheme:
a fast-charging microcrystalline graphite anode material is characterized by comprising the following components in percentage by weight:
i, the granularity of microcrystalline graphite is 2-6 mu m, the graphitization degree is more than 92%, and the impurity content is lower than 0.1%;
II, forming secondary particles by connecting the microcrystalline graphite through pyrolytic carbon, wherein the particle size of the secondary particles is 12-20 mu m;
III, completely filling the inner pores of the microcrystalline graphite with pyrolytic carbon;
IV, the specific surface area of the microcrystalline graphite secondary particles is less than or equal to 3m2(iv)/g, tap density is more than or equal to 1.0 g/cc;
and V, a loose carbon layer with the thickness of 1-3 nm is arranged on the outermost layer of the microcrystalline graphite.
A preparation method of a quick-charging microcrystalline graphite negative electrode material comprises the following steps:
s1, mixing the microcrystalline graphite waste with additives, wherein the additives comprise petroleum asphalt, coal asphalt and biomass asphalt;
s2, transferring the mixed materials into granulation equipment, and carrying out composite granulation under the inert atmosphere condition to obtain composite particles;
and S3, cooling the composite particles, and then carrying out twice classification by using a classifier, wherein the particle size of the twice-classified composite particles is 13-22 mu m, and the PSD is 0.9-1.1.
And S4, transferring the composite particles subjected to twice classification into a carbonization furnace for carbonization, naturally cooling after carbonization, scattering, demagnetizing and screening to obtain the quick-charging microcrystalline graphite cathode material.
Preferably, the preparation method of the fast-charging microcrystalline graphite negative electrode material comprises the following steps:
s1, mixing the microcrystalline graphite waste with an additive according to the mass ratio of 10: 1.5-10: 3, mixing in a VC mechanical mixing mode, wherein the particle size of the additive is 3-5 mu m, the additive comprises petroleum asphalt, coal asphalt and biomass asphalt, and the softening point of the additive is 120-300 ℃;
s2, transferring the mixed materials into a granulation device, and carrying out compound granulation at 400-600 ℃ in an inert atmosphere, wherein the rotation speed of the granulation device is 10-90 rpm, and the granulation time is 2-8 h, so as to obtain compound particles;
s3, after cooling the composite particles, performing two-time classification by a classifier, wherein the first classification uses 2# as a target discharge hole, the second classification uses 2# obtained in the first classification as a second classification, the 1# of the classifier is used as a target discharge hole, the particle size of the composite particles after the two-time classification is 13-22 mu m, the PSD is 0.9-1.1, and the PSD calculation method is (D)90-D10)/D50；
S4, transferring the composite particles after twice classification into a carbonization furnace, rapidly heating to 350-500 ℃ at a speed of 5-10 ℃/min under an inert atmosphere, preserving heat for 4-10 h, then slowly heating to 900-1250 ℃ at a heating speed of 1-3 ℃/min, preserving heat for 1h, naturally cooling, scattering, demagnetizing and screening to obtain the fast-filling microcrystalline graphite cathode material.
Preferably, in step S2, the granulation equipment includes, but is not limited to, a vertical kettle, a roller furnace, a horizontal kettle, and the like.
Preferably, the inert atmosphere includes, but is not limited to, inert gases such as nitrogen, argon, helium, and the like, which do not chemically react with the microcrystalline graphite, the additives, and the pyrolysis products of the additives at high temperatures.
The invention discloses a high-cost-performance fast-charging microcrystalline graphite cathode material and a preparation method thereof, and the method mainly comprises the following steps: the method comprises the following steps of microcrystalline graphite waste material, compound granulation, grading, carbonization, and demagnetizing screening. The innovation points of the invention are mainly as follows:
1. selecting raw materials:
the structural characteristics of the microcrystalline graphite are very beneficial to the rapid intercalation of lithium ions, and particularly the microcrystalline graphite waste with smaller granularity has better quick charging performance.
The invention selects the microcrystalline graphite waste as the raw material for the first time, so that the waste can be recycled, and the fast-charging cathode material with high cost performance can be obtained.
2. Grading process after compounding:
therefore, the microcrystalline graphite waste material is not used for preparing the fast-charging type cathode material of the lithium ion battery by people, and the main reason is that an effective process route is difficult to design for improving the physical properties of the microcrystalline graphite, such as the specific surface area and the tap density, because the physical properties of the microcrystalline graphite waste material are very poor.
The method adopts a composite granulation mode to improve the specific surface area of the microcrystalline graphite waste, and then controls the particle size distribution of the precursor by removing small-particle-size compounds through a grading process, thereby improving the tap density of the precursor. To achieve this, the fractionation process used in the present invention is two steps: in the first step, the material for composite granulation is taken as a feeding material, a grader 2# is taken as a target discharge hole, and the purpose is mainly to remove large particles (1#) and part of small particles (3#) (mainly to remove large particles) in a precursor; and in the second step, the material obtained by grading the No. 2 is used as a feeding material, grading is carried out again, the No. 1 of the grader is used as a target discharge hole, and the main purpose is to completely remove small particles (2#, 3#) in the precursor.
3. Special carbonisation processes
The microcrystalline graphite has too high specific surface area and low tap density. In order to solve the problems, the invention selects a special carbonization process, and has the innovation points that the temperature rising system of carbonization is as follows: firstly, rapidly heating a precursor to 350-500 ℃ and preserving heat for a period of time (the internal pores of the microcrystalline graphite are completely filled with pyrolytic carbon), then slowly heating to 900-1250 ℃ (the outer layer forms a loose carbon layer with the thickness of 1-3 nm), wherein the 350-500 ℃ heat preservation step can convert an additive into a flowing liquid state and further fill the flowing liquid state into the internal pores and the outer surface of the microcrystalline graphite, and in addition, volatile matters in the additive can escape to the surface of particles in the later heat preservation period and form a loose coated carbon layer in the subsequent heating carbonization process.
4. Structure of microcrystalline graphite cathode material
The particle size of the microcrystalline graphite is 2-6 mu m, the microcrystalline graphite micro powder is bonded and compounded into secondary particles through a layer of compact pyrolytic carbon, and the inner gaps of the microcrystalline graphite are also filled with the pyrolytic carbon; and a loose carbon layer with the thickness of 1-3 nm is arranged on the outermost layer of the secondary particles. This structure is extremely beneficial for the rapid lithium insertion of the material. Firstly, the loose carbon layer at the outermost layer can play a role in increasing the liquid storage amount, and provides a sufficient lithium source for the lithium embedding process. Secondly, the compact pyrolytic carbon is distributed on the surface and inside of the microcrystalline graphiteIt is known that the migration speed of lithium ions in pyrolytic carbon is much faster than that between graphite layers, so that the compact pyrolytic carbon is like a fast ion conductor and directly transports the lithium ions to the surface and the inside of microcrystalline graphite, and the diffusion time of the lithium ions in particles is greatly shortened. The close combination of the pyrolytic carbon and the microcrystalline graphite also effectively reduces the specific surface area (less than or equal to 3 m) of the particles2(g), the tap density of the obtained powder is more than or equal to 1.0 g/cc.
The invention provides a novel process method for preparing a fast-charging type cathode material of a lithium ion battery by adopting microcrystalline graphite waste, which solves the problems that the microcrystalline graphite waste has over-high specific surface area, low tap density and difficult manufacture of the fast-charging type cathode material in the prior art through a process route of microcrystalline graphite waste-composite granulation-grading-carbonization-demagnetization screening. The invention selects the microcrystalline graphite waste as the raw material, not only can the waste be recycled, but also the prepared quick-charging type cathode material has the characteristics of low production cost, small specific surface area, high tap density, excellent quick-charging performance and excellent cycle performance, and the specific performance data are shown in a comparison table in the embodiment.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
Mixing microcrystalline graphite waste with a graphitization degree of 93.2% and petroleum asphalt (granularity of 4.8 mu m) with a softening point of 120 ℃ according to the weight ratio of 10: 3 mechanically mixing with VC.
And (3) transferring the mixed materials into a vertical kettle, and carrying out compound granulation in nitrogen atmosphere at the temperature of 400 ℃, wherein the rotating speed of the materials in granulation equipment is 90rpm, and the granulation time is 3h, so as to obtain the compound particles.
And after the composite particles are cooled, performing two-time classification by using a classifier, wherein the first classification uses 2# as a target discharge port, the second classification is to perform secondary classification on the 2# obtained in the first classification, and uses 1# of the classifier as a target discharge port. The particle size of the composite particles after twice classification is 13-22 mu m, the PSD is 0.9-1.1, and the PSD calculation method is (D)90-D10)/D50。
And finally, transferring the composite particles subjected to twice classification into a carbonization furnace, rapidly heating to 350 ℃ at a speed of 10 ℃/min under the nitrogen atmosphere, preserving heat for 10h, slowly heating to 900 ℃ at a heating speed of 1 ℃/min, preserving heat for 1h, naturally cooling, scattering, demagnetizing and screening to obtain a No. 1 sample.
Example 2
Mixing microcrystalline graphite waste with a graphitization degree of 93.2% and coal tar pitch (granularity of 3.9 mu m) with a softening point of 280 ℃ according to the weight ratio of 10: 1.5 mechanical mixing with VC.
And (3) transferring the mixed materials into a roller furnace, and carrying out compound granulation at 600 ℃ in an argon atmosphere, wherein the rotation speed of the materials in granulation equipment is 15rpm, and the granulation time is 8 h.
After the composite particles were cooled, they were classified twice by a classifier in a similar manner to example 1.
And finally, transferring the composite particles subjected to twice classification into a carbonization furnace, rapidly heating to 500 ℃ at the speed of 5 ℃/min under the argon atmosphere, preserving heat for 4h, slowly heating to 1250 ℃ at the heating speed of 3 ℃/min, preserving heat for 1h, naturally cooling, scattering, demagnetizing and screening to obtain a No. 2 sample.
Example 3
Mixing microcrystalline graphite waste with a graphitization degree of 93.2% and biomass asphalt (granularity of 3.3 mu m) with a softening point of 200 ℃ according to the weight ratio of 10: 2.3 mechanical mixing with VC.
And (3) transferring the mixed materials into a horizontal furnace, and carrying out compound granulation at 500 ℃ in an argon atmosphere, wherein the rotation speed of the materials in granulation equipment is 40rpm, and the granulation time is 5 hours.
After the composite particles were cooled, they were classified twice by classifier F1, in a similar manner to example 1.
And finally, transferring the composite particles subjected to twice classification into a carbonization furnace, rapidly heating to 450 ℃ at the speed of 7 ℃/min under the argon atmosphere, preserving heat for 7h, slowly heating to 1100 ℃ at the heating speed of 2 ℃/min, preserving heat for 1h, naturally cooling, scattering, demagnetizing and screening to obtain a No. 3 sample.
Comparative example
Mixing microcrystalline graphite waste with a graphitization degree of 93.2% and coal tar pitch with a softening point of 280 ℃ according to the weight ratio of 10: 1.5 mixing, graphitizing, scattering, demagnetizing and screening to obtain a comparative sample.
Comparison of the 1-3 # samples with the comparative example data is shown in the following table.
As can be seen from the above table, the product prepared by the invention has the characteristics of low production cost, small specific surface area, high tap density, and excellent quick-charging performance and cycle performance.
The invention adopts a process route of 'microcrystalline graphite waste-composite granulation-grading-carbonization-demagnetizing screening'. The innovative idea is as follows:
(1) the microcrystalline graphite waste has the characteristics of small grain size and strong isotropy, and is suitable to be used as a raw material of a fast-charging type cathode material.
(2) The microcrystalline graphite waste has irregular shape, high specific surface area and low tap density, can not be directly used as a lithium ion battery cathode material, and the defects of the microcrystalline graphite waste are difficult to overcome through simple coating.
(3) After granulation, a classification process is added, by which the particle size distribution of the precursor can be controlled within a narrow range, which can further improve the physical properties of the microcrystalline graphite composite particles.
(4) The final heat treatment mode adopts a carbonization process instead of a high-energy consumption graphitization process, and the whole product processing process is simple, so that the low cost of the product is ensured. In addition, the quick charging performance of the negative electrode material obtained by the carbonization process is superior to that of a graphitized product, so that the preparation process is beneficial to ensuring the quick charging performance of the product.
The invention provides a novel process method for preparing a fast-charging type cathode material of a lithium ion battery by adopting microcrystalline graphite waste, which solves the problems that the microcrystalline graphite waste has over-high specific surface area, low tap density and difficult manufacture of the fast-charging type cathode material in the prior art through a process route of microcrystalline graphite waste-composite granulation-grading-carbonization-demagnetization screening. The invention selects the microcrystalline graphite waste as the raw material, not only can recycle the waste, but also has the characteristics of low production cost, small specific surface area, high tap density, and excellent fast charge performance and cycle performance.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above-described embodiments. It should be noted that modifications and adaptations to those skilled in the art may occur to persons skilled in the art without departing from the spirit and scope of the present invention. All the components not specified in the present embodiment can be realized by the prior art.
Claims (5)
1. A fast-charging microcrystalline graphite anode material is characterized by comprising the following components in percentage by weight:
i, the granularity of microcrystalline graphite is 2-6 mu m, the graphitization degree is more than 92%, and the impurity content is lower than 0.1%;
II, forming secondary particles by connecting the microcrystalline graphite through pyrolytic carbon, wherein the particle size of the secondary particles is 12-20 mu m;
III, completely filling the inner pores of the microcrystalline graphite with pyrolytic carbon;
IV, the specific surface area of the microcrystalline graphite secondary particles is less than or equal to 3m2(iv)/g, tap density is more than or equal to 1.0 g/cc;
and V, a loose carbon layer with the thickness of 1-3 nm is arranged on the outermost layer of the microcrystalline graphite.
2. A preparation method of a quick-charging microcrystalline graphite negative electrode material is characterized by comprising the following steps:
s1, mixing the microcrystalline graphite waste with an additive, wherein the additive is one of petroleum asphalt, coal asphalt and biomass asphalt;
s2, transferring the mixed materials into a granulation device, and carrying out compound granulation at 400-600 ℃ in an inert atmosphere, wherein the rotation speed of the granulation device is 10-90 rpm, and the granulation time is 2-8 h, so as to obtain compound particles;
s3, cooling the composite particles, and then carrying out twice classification by a classifier, wherein the particle size of the composite particles after twice classification is 13-22 μm, the PSD is 0.9-1.1, and the PSD calculation method is (D)90-D10)/D50；
S4, transferring the composite particles after twice classification into a carbonization furnace, rapidly heating to 350-500 ℃ at a speed of 5-10 ℃/min under an inert atmosphere, preserving heat for 4-10 h to enable internal pores of the microcrystalline graphite to be completely filled with pyrolytic carbon, slowly heating to 900-1250 ℃ at a heating speed of 1-3 ℃/min, preserving heat for 1h to form a loose carbon layer with the thickness of 1-3 nm on the outer layer of the microcrystalline graphite, naturally cooling after carbonization, scattering, demagnetizing and screening to obtain the fast-charging microcrystalline graphite cathode material.
3. The preparation method of the quick-charging microcrystalline graphite anode material as claimed in claim 2, characterized by comprising the following steps:
s1, mixing the microcrystalline graphite waste with an additive according to the mass ratio of 10: 1.5-10: 3, mixing in a VC mechanical mixing mode, wherein the particle size of the additive is 3-5 mu m, the additive is one of petroleum asphalt, coal asphalt and biomass asphalt, and the softening point of the additive is 120-300 ℃;
s2, transferring the mixed materials into a granulation device, and carrying out compound granulation at 400-600 ℃ in an inert atmosphere, wherein the rotation speed of the granulation device is 10-90 rpm, and the granulation time is 2-8 h, so as to obtain compound particles;
s3, after cooling the composite particles, performing two-time classification through a classifier, wherein the first classification uses a No. 2 as a target discharge hole to remove large particles and partial small particles in the composite particles, the second classification is to classify the No. 2 obtained in the first time again, and uses a No. 1 of the classifier as a target discharge hole to completely remove the small particles in the composite particles, the particle size of the composite particles after two-time classification is 13-22 mu m, and the PSD is 0.9-1.1;
s4, transferring the composite particles after twice classification into a carbonization furnace, rapidly heating to 350-500 ℃ at a speed of 5-10 ℃/min under an inert atmosphere, preserving heat for 4-10 h to enable internal pores of the microcrystalline graphite to be completely filled with pyrolytic carbon, slowly heating to 900-1250 ℃ at a heating speed of 1-3 ℃/min, preserving heat for 1h to form a loose carbon layer with the thickness of 1-3 nm on the outer layer of the microcrystalline graphite, naturally cooling, scattering, demagnetizing and screening to obtain the fast-charging microcrystalline graphite cathode material.
4. The preparation method of the rapid-charging microcrystalline graphite anode material as claimed in claim 2, wherein the preparation method comprises the following steps: in step S2, the granulation apparatus used is a vertical kettle, a roller furnace or a horizontal kettle.
5. The preparation method of the rapid-charging microcrystalline graphite anode material as claimed in claim 2, wherein the preparation method comprises the following steps: in steps S2 and S4, the inert gas in the inert atmosphere is nitrogen, argon, or helium.
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| CN111628145B (en) * | 2020-04-23 | 2022-02-01 | 湖南中科星城石墨有限公司 | Preparation method of microcrystalline graphite cathode material easy to prepare slurry |
| CN112694087A (en) * | 2020-12-23 | 2021-04-23 | 东莞市和鸿升新材料科技有限公司 | Method for preparing low-cost negative electrode material by recycling resistance material |
| CN114804095B (en) * | 2022-04-27 | 2023-12-12 | 中南大学 | Graphite negative electrode active material prepared from spheroidized graphite micropowder waste, and preparation method and application thereof |
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