CN110718690B - Preparation method of battery negative electrode material based on needle coke green coke and calcined coke - Google Patents
Preparation method of battery negative electrode material based on needle coke green coke and calcined coke Download PDFInfo
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Abstract
The invention discloses a preparation method of a battery cathode material based on needle coke green coke and calcined coke, which comprises the steps of crushing to obtain needle coke green coke particles with different median diameters and volatile content of 10-30% and needle coke calcined coke particles with the same median diameter, determining the mixing ratio of the two types of coke according to the difference of the volatile content of the needle coke, then carrying out high-temperature carbonization and graphitization, and screening to obtain the required median diameter lithium ion battery cathode material. The invention adopts needle coke green coke containing a certain volatile matter, mixes with needle coke calcined coke in a certain proportion, and obtains a lithium ion battery cathode material with higher coulombic efficiency and higher strength through high-temperature carbonization and graphitization.
Description
Technical Field
The invention relates to the field of coal chemical industry and carbon materials, in particular to a preparation method of a battery negative electrode material based on needle coke green coke and calcined coke.
Background
The needle coke-based lithium ion battery cathode material is widely applied to lithium ion batteries for electric automobiles, notebook computers and the like, and manufacturers of the lithium ion battery cathode material continuously improve the electrochemical performance of the lithium ion battery cathode material in various ways.
With the increasing exhaustion of fossil fuels, the energy crisis has become the focus of global attention, and therefore, the development of new energy is now listed in important strategic industries of various countries to get rid of economic decline and take the lead of future development. In the field of new energy, lithium ion batteries have been widely used in portable electronic appliances such as cameras, mobile phones, notebook computers, and the like due to their excellent characteristics of high energy density, high power density, good cycle performance, environmental friendliness, diversified structures, low price, and the like. In recent decades, due to the rapid development of lithium ion batteries, global industries such as communication and energy have been developed vigorously, and once the energy density and power density of lithium ion batteries are further improved greatly, the lithium ion batteries must become an ideal power supply for high-end energy storage systems such as future pure electric vehicles, hybrid electric vehicles and space technologies.
Carbon-based negative electrode materials that can be used in lithium ion batteries can be broadly classified into graphite, soft carbon, hard carbon, and the like, and their mechanisms are shown in fig. 1a, 1b, and 1 c.
The graphite is divided into natural graphite and artificial graphite, and has a layered structure, wherein carbon atoms are arranged in a hexagonal shape and extend in two-dimensional directions, and the interlayer spacing is 0.335 nm. The disadvantages of natural or artificial graphite as the negative electrode material of lithium ion batteries are:
1) because the edge of the natural or artificial graphite layer has surface functional groups such as carbonyl, carboxyl and the like, under a certain potential, the surface functional groups are easy to generate oxidation reaction with electrolyte and further react with Li + to form lithium salt, namely a so-called SEI (solid electrolyte interface) film, so that the first charge-discharge capacity is reduced, and the coulombic efficiency is reduced;
2) in the repeated lithium intercalation-lithium deintercalation process of natural or artificial graphite, surface chemical functional groups and solvents, such as PC, DME, DMSO and the like, are subjected to solvent co-intercalation to form Li-GIC interlayer compounds, so that graphite layers are expanded, peeled off and even pulverized, and further the lithium intercalation capacity is reduced and the cycle life is shortened;
3) the electrochemical behavior of natural graphite as a negative electrode material at low temperature (for example-20 ℃) is not ideal, mainly caused by slow diffusion of lithium ions in graphite, but not caused by electrolyte and a solid electrolyte interface film (SEI film), which is called the reason for low conductivity of the SEI film for short;
4) for common natural graphite, because the graphitization process in the natural evolution process is not thorough and natural impurities and defect structures exist, the lithium intercalation behavior cannot be compared with high-quality natural graphite or artificial graphite, the capacity is generally lower than 300mAh/g, the charge-discharge efficiency of the first cycle is lower than 80%, and the cycle performance is not ideal;
5) the high-power charging and discharging can not be realized, so that the high-power charging and discharging power supply can not become an ideal power supply of high-end energy storage systems of a pure electric vehicle, a hybrid electric vehicle, a space technology and the like in the future.
The soft carbon, i.e., easily graphitizable carbon, means an amorphous carbon that is graphitizable at a high temperature of 2500 ℃. The soft carbon has low graphitization degree, small crystal grain size, large crystal face spacing (d002) and good compatibility with electrolyte. Common soft carbons include petroleum coke, needle coke, carbon fibers, mesocarbon microbeads, and the like. If the internal structure of the soft carbon material is carefully examined, it may be subdivided into organized regions (organized regions) and unorganized regions (unorganized regions). The organized area is composed of a plurality of parallel graphite layers; the unorganized regions are composed of tetrahedrally bonded carbon and highly warped graphite platelets. The influence of the heat treatment temperature on the material structure and the pre-delithiation performance is large.
The mesocarbon microbeads have good fluidity because the external part is spherical, are easy to be made into excellent high-density electrodes, have high graphitization degree, not only have good lithium intercalation or deintercalation performance to Li +, but also have the defects that the spherical structure can easily form a layer of compact SEI film on the surface to effectively inhibit the exfoliation or pulverization of a graphite layer, but also have the following defects:
1) the irreversible capacity of the first charge and discharge is higher;
2) the output voltage is lower;
3) no obvious charge-discharge platform potential
4) The market price is higher.
Hard carbon, namely amorphous carbon with high graphitization degree is difficult to obtain through high-temperature (>2000 ℃) heat treatment, the graphitization degree of the hard carbon is low, lithium ions can be embedded between carbon layers and also can be embedded in cavities and gaps between the carbon layers, so that the hard carbon has the following advantages as a lithium ion battery negative electrode material:
1) the capacity is much greater than the theoretical capacity of graphite, and j.r.dahn and a.mabuchi et al believe that the higher capacity of such materials may be caused by three aspects: lithium is inserted into nano-pores formed by carbon crystallite dislocations and the like (so-called a pore lithium storage mechanism); and also to the hydrogen content of the carbon material; both sides of the microcrystalline surface in the carbon material can absorb lithium ions;
2) the hard carbon has a wider lithium intercalation potential range and a good lithium ion diffusion coefficient, is convenient for lithium ions to be rapidly intercalated without separating out metallic lithium, and is more suitable for the requirements of HEV on high-power charging characteristics.
However, the hard carbon material as a negative electrode material has the disadvantages of no low and flat charge and discharge platform like graphite and voltage hysteresis, thereby greatly limiting the practical application of the hard carbon material.
In the prior art, asphalt with a softening point of about 260 ℃ is used as a coating material, the addition amount is about 7-10%, the coating material is crushed to about 3 mu m, and the obtained product is fully mixed, carbonized at a low temperature, carbonized at a high temperature and graphitized to obtain the required negative electrode material.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of a battery cathode material based on needle coke green coke and calcined coke, which is characterized in that needle coke green coke containing a certain volatile matter is mixed with needle coke calcined coke in a certain proportion, and a lithium ion battery cathode material with higher coulombic efficiency and higher strength is obtained through high-temperature carbonization and graphitization.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a battery negative electrode material based on needle coke green coke and calcined coke comprises the following steps:
1) crushing to obtain needle coke particles with different median diameters and volatile content of 10-30%;
2) crushing to obtain needle coke calcined coke particles, wherein the median diameter of the calcined coke is the same as that of the raw coke obtained in the step 1);
3) determining the mixing proportion of the green coke particles obtained in the step 1) and the calcined coke particles obtained in the step 2) according to different contents of needle coke green coke volatile matters;
4) carbonizing the mixed particles obtained in the step 3) at a high temperature;
5) then graphitizing;
6) and finally, screening to remove part of small particles to obtain the cathode material with the required median diameter.
In the step 1), the median diameter of the green coke particles is 8-30 μm.
In the step 3), the mixing ratio is 1: 1-5: 8.
In the step 4), the temperature of high-temperature carbonization is 450-1400 ℃.
In the step 6), the required median diameter is 8-30 μm.
In the technical scheme, the preparation method of the battery cathode material based on needle coke green coke and calcined coke provided by the invention also has the following beneficial effects:
1) the preparation method of the invention adopts the needle coke green coke and the calcined coke to be mixed in proportion, and the mixing uniformity is much higher than that of the coating asphalt;
2) compared with the coating asphalt, the preparation method of the invention is easier to control the particle distribution of the cathode material;
3) compared with the coated asphalt, the lithium ion battery cathode material prepared by the preparation method has higher strength, so that the battery has higher safety.
Drawings
FIG. 1a is a schematic structural view of a graphite material;
FIG. 1b is a schematic structural view of a soft carbon material;
FIG. 1c is a schematic structural view of a hard carbon material;
FIG. 2 is a flow chart of the preparation process of the present invention.
Detailed Description
The technical scheme of the invention is further explained by combining the drawings and the embodiment.
Referring to fig. 2, the method for preparing a battery negative electrode material based on needle coke green coke and calcined coke provided by the present invention includes the following steps:
1) crushing to obtain needle coke-forming particles with volatile matter content of 10-30% and different median diameters, wherein the median diameter of the obtained coke-forming particles is 8-30 mu m;
2) crushing to obtain needle coke calcined coke particles, wherein the median diameter of the calcined coke is the same as that of the raw coke obtained in the step 1);
3) determining the mixing ratio of the green coke particles obtained in the step 1) and the calcined coke particles obtained in the step 2) according to different needle coke green volatile matter contents, wherein the mixing ratio is 1: 1-5: 8;
4) carbonizing the mixed particles obtained in the step 3) at a high temperature of 450-1400 ℃;
5) then graphitizing;
6) and finally, screening to remove part of small particles to obtain the cathode material with the required median diameter, wherein the median diameter required by the cathode material is 8-30 mu m.
Example one
Needle coke green coke with the median diameter of 15 mu m and the volatile content of 20 percent and needle coke calcined coke with the median diameter of 15 mu m are adopted according to the weight ratio of 3: 7, heating at 450-1400 ℃ according to a specified heating curve, graphitizing, and sieving to obtain the negative electrode material with the negative and middle diameters of 15 mu m, wherein the first coulombic efficiency is 96%, the charge-discharge platform is stable, the charge-discharge potential is 0.2-0.5V, and the lithium intercalation capacity is 363 mAh/g.
Example two
Needle coke green coke with the median diameter of 8 mu m and the volatile matter content of 15 percent and needle coke calcined coke with the median diameter of 8 mu m are adopted according to the weight ratio of 3.5: 6.5, heating at 450-1400 ℃ according to a specified heating curve, graphitizing, and sieving to obtain the negative electrode material with the negative and middle diameters of 8 mu m, wherein the first coulombic efficiency is 95%, the charge-discharge platform is stable, the charge-discharge potential is 0.2-0.5V, and the lithium intercalation capacity is 365 mAh/g.
In conclusion, the preparation method of the invention adopts the volatile matter of the coal-based or oil-based needle coke raw coke as the coating agent of the lithium ion battery cathode material, thereby improving the coulomb efficiency of the needle coke-based lithium ion battery cathode material and the safety of the lithium ion battery.
It should be understood by those skilled in the art that the above embodiments are only for illustrating the present invention and are not to be used as a limitation of the present invention, and that changes and modifications to the above described embodiments are within the scope of the claims of the present invention as long as they are within the spirit and scope of the present invention.
Claims (5)
1. A preparation method of a battery negative electrode material based on needle coke green coke and calcined coke is characterized by comprising the following steps:
1) crushing to obtain needle coke particles with different median diameters and volatile content of 10-30%;
2) crushing to obtain needle coke calcined coke particles, wherein the median diameter of the calcined coke is the same as that of the raw coke obtained in the step 1);
3) determining the mixing proportion of the green coke particles obtained in the step 1) and the calcined coke particles obtained in the step 2) according to different contents of needle coke green coke volatile matters;
4) carbonizing the mixed particles obtained in the step 3) at high temperature;
5) then graphitizing;
6) and finally, screening to remove part of small particles to obtain the cathode material with the required median diameter, wherein the initial coulomb efficiency of the cathode material is as high as 95%.
2. The method for preparing the battery negative electrode material based on needle coke green coke and calcined coke according to claim 1, wherein the method comprises the following steps: in the step 1), the median diameter of the green coke particles is 8-30 μm.
3. The method for preparing the battery negative electrode material based on needle coke green coke and calcined coke according to claim 1, wherein the method comprises the following steps: in the step 3), the mixing ratio is 1: 1-5: 8.
4. The method for preparing the battery negative electrode material based on needle coke green coke and calcined coke according to claim 1, characterized in that: in the step 4), the temperature of high-temperature carbonization is 450-1400 ℃.
5. The method for preparing the battery negative electrode material based on needle coke green coke and calcined coke according to claim 1, characterized in that: in the step 6), the required median diameter is 8-30 μm.
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