CN110655073A - Artificial graphite material with spherical structure and preparation method thereof - Google Patents
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Abstract
An artificial graphite material with a spherical structure and a preparation method thereof, the artificial graphite material has regular spherical particle size of 1-10 μm, and the preparation method comprises the following steps: s1, selecting an original material and crushing the original material according to the requirement of the particle size to obtain a precursor; s2, quantitatively adding a catalyst into the precursor; s3, fully and uniformly mixing the precursor and the catalyst to enable the particle size of the mixture to reach a set range; and S4, graphitizing the mixture at high temperature under a protective atmosphere to obtain the artificial graphite material with the spherical structure. The invention has simple catalytic graphitization route, compared with the traditional graphitization which needs a long time, the addition of the catalyst promotes the reaction to a great extent, shortens the graphitization time, is easy to control the graphitization process, and is beneficial to industrial production. When the prepared artificial graphite material is applied to a lithium ion battery cathode material, excellent rate capability and cycle stability performance are shown.
Description
Technical Field
The invention relates to the field of lithium ion battery cathode materials and processing and preparation thereof, in particular to an artificial graphite material with a spherical structure and a preparation method thereof, which meet the structural stability requirement under high rate and have low preparation cost.
Background
With the increasing exhaustion of traditional fuels such as coal, oil and natural gas, the environmental problems are becoming worse, and the search for a new clean energy source becomes a hot issue of interest for researchers. Because the lithium ion battery has higher energy density and output voltage, stable cycle life, lower self-discharge performance and environmental protection, the lithium ion battery becomes a new generation of energy storage device for replacing the traditional fuel. With the improvement of living standard and the development of electronic informatization, the demand for electronic products and electric equipment is continuously increased, and high-performance and low-cost lithium ion batteries are the direction of important attention of people. The cathode material, as an important component of the lithium ion battery, largely determines the practicability and safety of the battery device.
At present, graphite materials are still the medium strength of commercial lithium ion battery negative electrode materials due to the advantages of good stability, low voltage, capability of forming good lithium intercalation compounds with lithium and the like. In recent years, with the increasing difficulty of natural graphite mining and the complexity of post-treatment processes, the cost of graphite negative electrodes is continuously increased, and the capacity of natural graphite is too rapidly attenuated in the charging and discharging processes, so that the development and application of artificial graphite become an important direction for the development of the field of graphite materials.
However, most of the artificial graphite is currently formed by graphitizing needle coke, petroleum coke or cordierite, and is applied after a spheroidizing process, which undoubtedly increases the production cost and makes it difficult to maintain stable cycle performance at high rate. In view of the above problems, the development of a graphite material with low cost, stable structure and excellent performance is not easy.
Disclosure of Invention
The invention aims to solve the problems of poor circulation stability of the artificial graphite material under high multiplying power and high preparation process and raw material cost in the prior art, and provides the artificial graphite material with the spherical structure and the preparation method thereof.
In order to achieve the purpose, the invention has the following technical scheme:
a preparation method of an artificial graphite material with a spherical structure comprises the following steps:
s1, selecting an original material and crushing the original material according to the requirement of the particle size to obtain a precursor;
s2, quantitatively adding a catalyst into the precursor;
s3, fully and uniformly mixing the precursor and the catalyst to enable the particle size of the mixture to reach a set range;
and S4, graphitizing the mixture at high temperature under a protective atmosphere to obtain the artificial graphite material with the spherical structure.
In a preferred embodiment of the preparation method of the present invention, the raw material in step S1 is one or more of semi-coke and anthracite, and the average particle size after pulverization is 1mm to 10 mm.
In one embodiment of the preparation method of the present invention, the catalyst in step S2 is B, Si, Mn, Co, Ca, Ni, B2O3、H3BO3、B4C、Fe2O3、Fe3O4、SiO、SiO2、SiC、Al2O3、MgO、MnO2One or more of them.
In a preferred embodiment of the preparation method of the present invention, the added mass of the catalyst in step S2 is 4-20% of the mass of the precursor.
As a preferable mode, in an embodiment of the preparation method of the present invention, the step S3 is performed by mixing by a ball mill; the ball milling time in the mixing process is 1-10 h, and the ball-material ratio is (1-20): 1, the rotating speed is 100rpm-1000 rpm.
In one embodiment of the preparation method of the present invention, the particle size of the mixture is 1 μm to 20 μm in step S3.
As a preferable scheme, in an embodiment of the preparation method of the present invention, the graphitization temperature in the step S4 is 2000 ℃ to 3000 ℃, the graphitization time is 1h to 10h, and the protective atmosphere is argon.
The invention also provides an artificial graphite material with a spherical structure, and the particle size of the regular spheres is 1-10 mu m.
The invention also provides a lithium ion battery cathode material prepared from the artificial graphite material with the spherical structure, the theoretical capacity can reach 347.5mA/g at 0.05C, the capacity retention rate is close to 100% after 100 cycles, the initial capacity can reach 313mA/g at 0.5C, and the capacity retention rate is 97.3% after 100 cycles.
Compared with the prior art, the invention has the following beneficial effects: the catalyst is quantitatively added into the precursor, so that the artificial graphite material with the spherical structure can be directly obtained by fully and uniformly mixing the precursor and the catalyst, and the graphite material produced by the traditional method can reach the required spherical structure only by carrying out additional spheroidization treatment, which undoubtedly increases the cost of the artificial graphite material. The invention avoids the subsequent spheroidization treatment, and the catalyst has a special mechanism of dissolution and re-precipitation catalysis, thereby not only accelerating the graphitization, but also having positive influence on the nucleation process of the spherical graphite. The invention has simple catalytic graphitization route, high reaction speed, obviously shortened graphitization time, low catalyst cost and easily controlled graphitization process compared with the traditional graphitization treatment which needs a long time, and is beneficial to industrial production.
Furthermore, the raw material for preparing the precursor is one or more of semi-coke and anthracite, the semi-coke and anthracite are crushed to the average particle size of 1mm-10mm, the selected raw material is an industrial waste product, and compared with the traditional method for producing artificial graphite by using needle coke or petroleum coke or asphalt, the method has the advantages of lower cost, capability of changing waste into valuables and reduction of environmental pollution.
Compared with the prior art, the artificial graphite material prepared by the invention has a regular spherical structure, is uniform in size, has the particle size of about 1-10 mu m, can be directly used as a lithium ion battery cathode material, and avoids the later spheroidization process.
Compared with the prior art, when the artificial graphite material prepared by the invention is applied to a lithium ion battery cathode material, the artificial graphite material shows excellent rate capability and cycle stability performance, the first discharge specific capacity at 0.05C can reach 347.5mA/g, the capacity retention rate is almost 100% after 100 cycles, and the capacity retention rate can still reach 97.7% after 100 cycles at the rate of 0.5C; even when the multiplying power is increased to 3C, the specific capacity is still 160(mA · h)/g, which is incomparable with the common commercial graphite material on the market at present.
Drawings
In order to more clearly illustrate the technical solution of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
FIG. 1 is a graph comparing the cycle performance of the artificial graphite material of the present invention with a commercial graphite material at a current density of 0.5C;
FIG. 2 is a graph comparing the rate capability of the artificial graphite material of the present invention with that of a commercial graphite material at different current densities;
FIG. 3 is an SEM image of the negative electrode material of the lithium ion battery prepared by the invention;
FIG. 4 is a TEM image of the lithium ion battery negative electrode material prepared by the invention;
FIG. 5 is a STEM diagram of the lithium ion battery negative electrode material prepared by the invention;
FIG. 6 is a first charge-discharge curve of the artificial graphite material according to each example of the present invention at a current density of 0.05C;
FIG. 7 is a first charge-discharge curve of the artificial graphite material according to each example of the present invention at a current density of 0.5C;
FIG. 8 is a graph showing the specific cycle at a current density of 0.5C for the artificial graphite material according to the examples of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, also belong to the protection scope of the present invention.
Example 1
The preparation method of the artificial graphite material with the spherical structure comprises the following steps:
raw materials such as semi-coke and the like are crushed to 5mm, Ni is taken as a catalyst, the mass of the catalyst is 4% of that of a precursor, the ball milling time is 5h, the ball-material ratio is 10:1, and the ball milling is carried out at the rotating speed of 100rpm to obtain uniform mixture powder. Then graphitizing to obtain artificial graphite, wherein the protective atmosphere is argon, the graphitizing temperature is 2100 ℃, and the time is 2 hours, and the spherical graphite cathode material is obtained after graphitization.
Example 2
The preparation method of the artificial graphite material with the spherical structure comprises the following steps:
pulverizing raw materials such as semi-coke to 5mm, and collecting B2O3Adding the catalyst as a catalyst, wherein the mass of the added catalyst is 6% of that of the precursor, and performing ball milling for 5h at a ball-to-material ratio of 10:1 and a rotation speed of 450rpm to obtain uniform mixture powder. Then, graphitizing to obtain artificial graphite, wherein the graphitizing temperature is 2300 ℃, the time is 1h, and the spherical graphite cathode material is obtained after graphitization.
Example 3
The preparation method of the artificial graphite material with the spherical structure comprises the following steps:
raw materials such as semi-coke and the like are crushed to 5mm, B is taken as a catalyst, the mass of the catalyst is 6 percent of that of the precursor, the ball milling time is 5h, the ball-to-material ratio is 10:1, and the rotating speed is 450rpm, so that uniform mixture powder is obtained. Then, graphitizing to obtain artificial graphite, wherein the graphitizing temperature is 2300 ℃, the time is 1h, and the spherical graphite cathode material is obtained after graphitization.
Example 4
The preparation method of the artificial graphite material with the spherical structure comprises the following steps:
pulverizing raw materials such as semi-coke to 5mm, and collecting B2O3And Si in a mass ratio of 1: 1 as a catalyst, adding 8% of the catalyst by mass of the precursor, and performing ball milling for 5h at a ball-to-material ratio of 10:1 and a rotation speed of 720rpm to obtain uniform mixture powder. Then, graphitizing to obtain artificial graphite, wherein the graphitizing temperature is 2300 ℃, the time is 2 hours, and the spherical graphite cathode material is obtained after graphitization.
Example 5
The preparation method of the artificial graphite material with the spherical structure comprises the following steps:
raw materials such as semi-coke and the like are crushed to 5mm, SiC is taken as a catalyst, the mass of the added catalyst is 12 percent of that of the precursor, the ball milling time is 5h, the ball-to-material ratio is 10:1, and the ball milling is carried out at the rotating speed of 720rpm, so as to obtain uniform mixture powder. Then graphitizing to obtain artificial graphite, wherein the graphitization temperature is 2700 ℃ and the time is 1h, and the spherical graphite cathode material is obtained after graphitization.
Example 6
The preparation method of the artificial graphite material with the spherical structure comprises the following steps:
raw materials such as semi-coke and the like are crushed to 5mm, Si is taken as a catalyst, the mass of the added catalyst is 15% of that of the precursor, the ball milling time is 5h, the ball-to-material ratio is 10:1, and the rotating speed is 450rpm, so that uniform mixture powder is obtained. Then, graphitizing to obtain artificial graphite, wherein the graphitizing temperature is 2300 ℃, the time is 1h, and the spherical graphite cathode material is obtained after graphitization.
Example 7
The preparation method of the artificial graphite material with the spherical structure comprises the following steps:
raw materials such as semi-coke and the like are crushed to 7mm, SiO is taken as a catalyst, the mass of the added catalyst is 15% of that of a precursor, the ball milling time is 1h, the ball-to-material ratio is 20:1, and the rotating speed is 450rpm, so that uniform mixture powder is obtained. Then graphitizing to obtain artificial graphite, wherein the graphitization temperature is 2700 ℃ and the time is 1h, and the spherical graphite cathode material is obtained after graphitization.
Example 8
The preparation method of the artificial graphite material with the spherical structure comprises the following steps:
pulverizing raw materials such as semi-coke to 1mm, and collecting SiO2Adding the catalyst as a catalyst, wherein the mass of the catalyst is 10% of that of the precursor, and performing ball milling for 7h at a ball-to-material ratio of 15:1 and a rotation speed of 720rpm to obtain uniform mixture powder. Then graphitizing to obtain artificial graphite, wherein the graphitization temperature is 2700 ℃ and the time is 1h, and the spherical graphite cathode material is obtained after graphitization.
Table 1 lithium ion battery performance test results
Example 9
The preparation method of the artificial graphite material with the spherical structure comprises the following steps:
pulverizing anthracite into 10mm, and taking H3BO3Adding the catalyst as a catalyst, wherein the mass of the catalyst is 15% of that of the precursor, and performing ball milling for 3h at a ball-to-material ratio of 7:1 and a rotation speed of 570rpm to obtain uniform mixture powder. And then graphitizing to obtain artificial graphite, wherein the graphitizing temperature is 2800 ℃ and the time is 3 hours, and the spherical graphite cathode material is obtained after graphitization.
Example 10
The preparation method of the artificial graphite material with the spherical structure comprises the following steps:
pulverizing anthracite into powder6mm, taking Fe2O3Adding the catalyst as a catalyst, wherein the mass of the catalyst is 8% of that of the precursor, performing ball milling for 7h, the ball-to-material ratio is 3:1, and the rotating speed is 320rpm to obtain uniform mixture powder. Then, graphitizing to obtain artificial graphite, wherein the graphitizing temperature is 2100 ℃, the time is 8 hours, and the spherical graphite cathode material is obtained after graphitization.
Example 11
The preparation method of the artificial graphite material with the spherical structure comprises the following steps:
pulverizing anthracite powder to 4mm, and taking Al2O3Adding the catalyst as a catalyst, wherein the mass of the catalyst is 8% of that of the precursor, and performing ball milling for 9h at a ball-to-material ratio of 13:1 and a rotating speed of 480rpm to obtain uniform mixture powder. Then graphitizing to obtain artificial graphite, wherein the graphitizing temperature is 2450 ℃ and the time is 6h, and the spherical graphite cathode material is obtained after graphitization.
Example 12
The preparation method of the artificial graphite material with the spherical structure comprises the following steps:
crushing anthracite powder to 6mm, taking Co and SiC according to the mass ratio of 1: 1 as a catalyst, adding 13% of the catalyst by mass of the precursor, performing ball milling for 7.5h at a ball-to-material ratio of 19:1 and a rotation speed of 1000rpm to obtain uniform mixture powder. Then graphitizing to obtain artificial graphite, wherein the graphitizing temperature is 3000 ℃, the time is 7h, and the spherical graphite cathode material is obtained after graphitization.
Example 13
The preparation method of the artificial graphite material with the spherical structure comprises the following steps:
pulverizing anthracite into 8mm, and taking B, Al2O3And SiC in a mass ratio of 1: 1: 1 as a catalyst, adding the catalyst with the mass of 20% of the mass of the precursor, and performing ball milling for 10h at the ball-to-material ratio of 20:1 and the rotation speed of 100rpm to obtain uniform mixture powder. Then obtaining the artificial graphite through graphitization, wherein the graphitization temperature is 200 DEGAnd (3) graphitizing at 0 ℃ for 10h to obtain the spherical graphite cathode material.
Referring to fig. 1, it can be clearly seen from the figure that the artificial graphite material of the present invention is better than conventional graphite in terms of both cycle and rate, compared to three kinds of commonly used commercial artificial graphite. At 0.5C, the graphite material of the present invention exhibited almost no capacity fade after 100 cycles, whereas commercial graphite exhibited a tendency to fade. Referring to FIG. 2, when the current density reached 3C, the commercial graphite had decayed to about 60(mA · h)/g, while the artificial graphite of the present invention could still reach 160(mA · h)/g.
In order to prove the effect of the invention, the preparation method of the spherical artificial graphite adopts a planetary ball mill and a high-temperature graphitization furnace for synthesizing and preparing materials. The successful preparation of the spherical artificial graphite is verified by observing the shape and structure of the material by using a field emission transmission electron microscope (JEOL JEM-F200 (HR)). The electrochemical performance of the cell was tested using a newware cell test system.
Referring to fig. 3, it can be clearly seen that, after the technical scheme is adopted, the prepared artificial graphite material presents a regular spherical structure, and has uniform size with the particle size of about 3 μm. Can be directly used as the cathode material of the lithium ion battery, and avoids the process of the later spheroidization treatment.
Referring to fig. 4-5, the lattice fringes and the corresponding (002) interplanar spacing of graphite can be clearly seen from TEM and STEM images of the lithium ion battery cathode material, which indicates that the prepared material is a graphite material.
Referring to fig. 6-7, it can be seen that graphite materials with good performance can be prepared by different conditions of the preparation method of the present invention. Referring to fig. 8, it can be seen from the cyclic specific volume at 0.5C graph that the stability of the material remained better after 100 cycles, and it is also proved that the preparation of the high-rate long-cycle artificial graphite material of the present invention is achieved by this method.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the technical solution of the present invention, and it should be understood by those skilled in the art that the technical solution can be modified and replaced by a plurality of simple modifications and replacements without departing from the spirit and principle of the present invention, and the modifications and replacements also fall within the protection scope defined by the claims.
Claims (9)
1. A preparation method of an artificial graphite material with a spherical structure is characterized by comprising the following steps:
s1, selecting an original material and crushing the original material according to the requirement of the particle size to obtain a precursor;
s2, quantitatively adding a catalyst into the precursor;
s3, fully and uniformly mixing the precursor and the catalyst to enable the particle size of the mixture to reach a set range;
and S4, graphitizing the mixture at high temperature under a protective atmosphere to obtain the artificial graphite material with the spherical structure.
2. The method for preparing artificial graphite material having spherical structure according to claim 1, wherein: the raw material in the step S1 is one or more of semi-coke and anthracite, and the average particle size after crushing is 1mm-10 mm.
3. The method for preparing artificial graphite material having spherical structure according to claim 1, wherein: the catalyst in the step S2 is B, Si, Co, Ni, B2O3、H3BO3、B4C、Fe2O3、SiO、SiO2、SiC、Al2O3、、MnO2One or more of them.
4. The method for preparing artificial graphite material having spherical structure according to claim 1, wherein: the adding mass of the catalyst in the step S2 is 4-20% of the mass of the precursor.
5. The method for preparing artificial graphite material having spherical structure according to claim 1, wherein: the step S3 is carried out mixing by a ball mill;
the ball milling time in the mixing process is 1-10 h, and the ball-material ratio is (1-20): 1, the rotating speed is 100rpm-1000 rpm.
6. The method for preparing artificial graphite material having a spherical structure according to claim 1 or 5, wherein: in step S3, the particle size of the mixture is 1-20 μm.
7. The method for preparing artificial graphite material having spherical structure according to claim 1, wherein: in the step S4, the graphitization temperature is 2000-3000 ℃, the graphitization time is 1-10 h, and the protective atmosphere is argon.
8. An artificial graphite material having a spherical structure produced based on the production method according to any one of claims 1 to 7, characterized in that: the particle size of the regular sphere is 1-10 μm.
9. A lithium ion battery negative electrode material produced using the artificial graphite material having a spherical structure according to claim 8, characterized in that: the initial discharge specific capacity at 0.05C can reach 347.5mA/g, the capacity retention rate after 100 cycles is close to 100%, the initial discharge capacity at 0.5C can reach 313mA/g, and the capacity retention rate after 100 cycles is 97.3%.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080193764A1 (en) * | 2004-05-24 | 2008-08-14 | National Institute For Materials Science | Cladophora-Form Carbon, Process for Producing the Same and Production Apparatus |
| CN102633251A (en) * | 2012-04-13 | 2012-08-15 | 西安交通大学 | Lithium ion battery cathode material prepared by blue carbon solid waste, and preparation method of lithium ion battery cathode material |
| KR20150141015A (en) * | 2014-06-09 | 2015-12-17 | 이성균 | Sugar-synthetic diamond (Manufacturing Method I) |
| CN105819430A (en) * | 2016-03-16 | 2016-08-03 | 中国科学院山西煤炭化学研究所 | Preparation method of coal base graphene |
| CN109321211A (en) * | 2018-10-19 | 2019-02-12 | 福州大学 | A kind of graphitization graded porous carbon composite phase-change energy storage material and preparation method thereof |
| CN110085863A (en) * | 2019-04-26 | 2019-08-02 | 桑顿新能源科技有限公司 | Graphite cathode material and preparation method thereof, battery |
-
2019
- 2019-09-17 CN CN201910877431.9A patent/CN110655073A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080193764A1 (en) * | 2004-05-24 | 2008-08-14 | National Institute For Materials Science | Cladophora-Form Carbon, Process for Producing the Same and Production Apparatus |
| CN102633251A (en) * | 2012-04-13 | 2012-08-15 | 西安交通大学 | Lithium ion battery cathode material prepared by blue carbon solid waste, and preparation method of lithium ion battery cathode material |
| KR20150141015A (en) * | 2014-06-09 | 2015-12-17 | 이성균 | Sugar-synthetic diamond (Manufacturing Method I) |
| CN105819430A (en) * | 2016-03-16 | 2016-08-03 | 中国科学院山西煤炭化学研究所 | Preparation method of coal base graphene |
| CN109321211A (en) * | 2018-10-19 | 2019-02-12 | 福州大学 | A kind of graphitization graded porous carbon composite phase-change energy storage material and preparation method thereof |
| CN110085863A (en) * | 2019-04-26 | 2019-08-02 | 桑顿新能源科技有限公司 | Graphite cathode material and preparation method thereof, battery |
Non-Patent Citations (2)
| Title |
|---|
| MING SHI, ET AL.: "Spherical graphite produced from waste semi-coke with enhanced properties as an anode material for Li-ion batteries", 《SUSTAINABLE ENERGY FUELS》 * |
| 江行国等: "采用固体废弃物兰炭末制备锂离子电池负极材料 ", 《新型炭材料》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113636546A (en) * | 2021-07-19 | 2021-11-12 | 西安交通大学 | Composite graphite material and preparation method and application thereof |
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