CN109950495B - Preparation method of high-rate graphite negative electrode material, negative electrode material and lithium ion battery - Google Patents
Preparation method of high-rate graphite negative electrode material, negative electrode material and lithium ion battery Download PDFInfo
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Abstract
The embodiment of the invention relates to a preparation method of a high-rate graphite cathode material, the cathode material and a lithium ion battery, and the preparation method comprises the following steps: mixing a first carbon source material with a powdery oxygen-containing metal compound to obtain a first mixture; graphitizing the first mixture at 2000-3300 ℃ to obtain a graphitized material; uniformly mixing the graphitized material and a second carbon source material at room temperature or under the condition of temperature rise to obtain a second mixture; and carbonizing the second mixture at 700-1300 ℃, cooling and screening to obtain the cathode material. According to the invention, the oxygen-containing metal compound and the carbon material are subjected to oxidation-reduction reaction at high temperature, holes are formed on the surface of the carbon material, and the carbon material is coated with the carbonized metal compound to effectively reduce the specific surface, so that the graphite port exposed outside is coated, the charging rate of the lithium ion battery can be effectively improved, the charging time is shortened, and the high-energy-density quick-charging lithium ion battery is obtained.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a preparation method of a high-rate graphite negative electrode material, the negative electrode material and a lithium ion battery.
Background
With the increasing number of fuel vehicles worldwide, the pressure on the environment and energy sources by the vehicles is more severe. The new energy automobile can solve the problem, so that the new energy automobile is increasingly paid attention to in the global scope, and a plan for completely forbidding first-burning vehicles is made in many countries. Under the dual requirements of policy environment and energy pressure, the Chinese automobile industry will undoubtedly meet the wave of development of new energy. However, new energy automobiles still have many short plates, such as short driving range, slow charging speed and the like, and especially, lithium is easily separated from the surface of a negative electrode material during high-rate charging, so that a serious safety problem is caused. The key point of the development of new energy automobiles lies in the breakthrough of battery technology, and the renewal of the battery technology lies in the innovation of materials. The artificial graphite cathode material has the characteristics of high energy density, long cycle life and the like, and the artificial graphite with various specifications has different charging multiplying powers.
How to improve the charging multiplying power of the lithium ion battery and shorten the charging time, and the invention aims to solve the problem of obtaining the high-energy-density quick-charging lithium ion battery.
Disclosure of Invention
The invention aims to provide a preparation method of a high-rate graphite cathode material, the cathode material and a lithium ion battery aiming at the defects of the prior art, wherein an oxygen-containing metal compound is adopted to perform oxidation-reduction reaction with a carbon material at high temperature, holes are formed on the surface of the carbon material, carbonization coating is adopted to effectively reduce the specific surface, and a graphite port exposed outside is further coated, so that the charging rate of the lithium ion battery can be effectively improved, the charging time is shortened, and the high-energy-density quick-charging lithium ion battery is obtained.
In view of this, in a first aspect, an embodiment of the present invention provides a method for preparing a high-rate graphite anode material, including: mixing a first carbon source material and a powdery oxygen-containing metal compound according to a weight ratio of 100: 1-50 to obtain a first mixture;
graphitizing the first mixture at 2000-3300 ℃ to obtain a graphitized material;
uniformly mixing the graphitized material and a second carbon source material according to the weight ratio of 100: 0-10 at room temperature or at a heating condition to obtain a second mixture; wherein the temperature rise temperature is not more than 700 ℃;
and carbonizing the second mixture at 700-1300 ℃, cooling and screening to obtain the negative electrode material.
Preferably, the particle size of the first carbon source material is 5 μm to 30 μm.
Further preferably, the first carbon source material comprises one or more of mesocarbon microbeads, petroleum coke, pitch coke, needle coke, or coke.
Preferably, the powdery oxygen-containing metal compound comprises one or more of ferroferric oxide, ferric oxide, ferrous oxide, ferric hydroxide, aluminum oxide, copper oxide, basic copper carbonate, zinc oxide, calcium oxide, manganese dioxide, manganese heptaoxide and potassium permanganate.
Preferably, the second carbon source material includes pitch powder and/or resin powder.
Preferably, the resin powder comprises one or more of polyvinylidene fluoride, phenolic resin and polyethylene.
Preferably, the temperature rise condition is constant-speed temperature rise or multi-section variable-speed combined temperature rise, and the temperature rise rate is 1-10 ℃/min.
In a second aspect, an embodiment of the present invention provides a graphite negative electrode material prepared by applying the preparation method described in the first aspect.
In a third aspect, embodiments of the present invention provide a lithium ion battery including the graphite negative electrode material described in the second aspect.
According to the preparation method of the high-rate graphite cathode material, the cathode material and the lithium ion battery provided by the embodiment of the invention, the oxygen-containing metal compound and the carbon material are subjected to oxidation-reduction reaction at high temperature, the holes are formed on the surface of the carbon material, carbonization coating is adopted to effectively reduce the specific surface, and the graphite port exposed outside is further coated, so that the charging rate of the lithium ion battery can be effectively improved, the charging time is shortened, and the high-energy-density quick-charging lithium ion battery is obtained.
Drawings
Fig. 1 is a flowchart of a method for preparing a high-rate graphite negative electrode material according to an embodiment of the present invention;
FIG. 2 is a schematic diagram illustrating charging and lithium intercalation of graphite particles after oxidative pore-formation according to an embodiment of the present invention;
FIG. 3 is a schematic representation of lithium intercalation during charging of untreated graphite particles;
fig. 4 is a scanning electron microscope image of the negative electrode material provided in embodiment 1 of the present invention;
fig. 5 is a scanning electron microscope image of the negative electrode material provided in embodiment 2 of the present invention;
fig. 6 is a scanning electron microscope image of the negative electrode material provided in embodiment 3 of the present invention;
fig. 7 is a scanning electron microscope image of the negative electrode material provided in embodiment 4 of the present invention;
FIG. 8 is a scanning electron micrograph of the negative electrode material according to comparative example 1 of the present invention;
FIG. 9 is a scanning electron micrograph of a negative electrode material according to comparative example 2 of the present invention;
FIG. 10 is a scanning electron micrograph of a negative electrode material according to comparative example 3 of the present invention;
fig. 11 is a scanning electron microscope image of the negative electrode material provided by comparative example 4 of the present invention.
Detailed Description
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Fig. 1 is a flowchart of a method for preparing a high-rate graphite negative electrode material, a negative electrode material, and a lithium ion battery, which are provided in an embodiment of the present invention, and as shown in fig. 1, the method includes:
Specifically, the particle size of the first carbon source material is 5-30 μm, and the first carbon source material comprises one or more of mesocarbon microbeads, petroleum coke, pitch coke, needle coke or coke.
The powdery oxygen-containing metal compound comprises one or more of ferroferric oxide, ferric oxide, ferrous oxide, ferric hydroxide, aluminum oxide, copper oxide, basic copper carbonate, zinc oxide, calcium oxide, manganese dioxide, manganic oxide and potassium permanganate.
And 102, graphitizing the first mixture at 2000-3300 ℃ to obtain a graphitized material.
During graphitization, the oxygen-containing metal compound and the first carbon source material generate redox reaction at high temperature, and round holes are formed on the surface of the first carbon source material through oxidation corrosion, and the formed round holes have the function of opening up a plurality of channels for lithium ions to enter graphite, so that the charging rate of the material is increased.
The graphite particles with holes on the surface have more graphite layers exposed outside, and carbon atoms at the end ports of the graphite sheets are easy to collapse or generate side reaction with electrolyte during high-temperature charge and discharge, thereby reducing the performance of the battery. Therefore, the exposed carbon atoms of the graphite sheets need to be coated by the second carbon source material to play a role in protection, so that the cycle performance is improved, and the high-temperature side reaction of the battery is stopped.
Specifically, the second carbon source material comprises asphalt powder and/or resin powder, wherein the resin powder comprises one or more of polyvinylidene fluoride, phenolic resin and polyethylene.
The uniform mixing of the graphitized material and the second carbon source material can be carried out under the conditions of room temperature or temperature rise.
In the first case, the graphitized material obtained in step 102 and the second carbon source material are uniformly mixed in a weight ratio at room temperature, so as to obtain a second mixture.
In the second case, under the condition of temperature rise, the temperature rise temperature does not exceed 700 ℃, and during the temperature rise process, uniform temperature rise or multi-section variable speed combined temperature rise can be selected, the temperature rise rate is 1-10 ℃/min, the graphitized material and the second carbon source material are heated and mixed at the same time, the melting speed of the coating agent is controlled, so that the coating agent can be coated uniformly under the corresponding condition, and if the temperature rise is too fast, the coating agent is carbonized before coating.
The uniform mixing can be achieved by stirring or the like, and the graphitized material sintered or hardened after graphitization can be crushed and sufficiently mixed with the coating agent.
And step 104, carbonizing the second mixture at 700-1300 ℃, cooling and screening to obtain the negative electrode material.
According to the preparation method of the high-rate graphite cathode material provided by the embodiment of the invention, the oxygen-containing metal compound and the carbon material are subjected to oxidation-reduction reaction at high temperature, holes are formed on the surface of the carbon material, and the effective reduction ratio is coated by carbonization, so that the graphite port exposed outside is coated, and the cathode material with high capacity, long cycle life and high charge rate is prepared.
Fig. 2 is a schematic diagram of charging and lithium intercalation of graphite particles after oxidative pore formation, fig. 3 is a schematic diagram of charging and lithium intercalation of untreated graphite particles, and it can be known from fig. 2 and fig. 3 that pores are formed on the graphite surface through an oxidation-reduction reaction in the graphite negative electrode material prepared by the preparation method provided by the embodiment of the present invention, and the micropores provide channels for lithium ions to be intercalated into the graphite sheet layer during charging, so as to improve intercalation efficiency. In addition, the carbonization coating is adopted to effectively reduce the ratio table, and further the graphite port exposed outside is coated to play a role of a funnel, so that lithium ions quickly flow to micropores or among graphite sheets, and the charging rate is further improved.
The graphite negative electrode material provided by the embodiment can be used as a negative electrode material of a lithium ion battery or a part of the negative electrode material.
The preparation process of the high-rate graphite negative electrode material provided by the embodiments of the present invention, and the application and performance of the prepared high-rate graphite negative electrode material are further specifically described in the following with some specific examples.
Example 1
Step 1, uniformly mixing petroleum coke with the particle size of 20 microns and powdered iron hydroxide according to the weight ratio of 100:40 to obtain a mixture I;
step 2, graphitizing the mixture I at 3250 ℃ to obtain a graphitized material;
step 3, uniformly mixing the obtained graphitized material and asphalt powder at the room temperature according to the ratio of 100:6 to obtain a mixture II;
and 4, carbonizing the mixture II at 900 ℃, cooling and screening to obtain a finished product.
Scanning electron microscope detection is carried out on the prepared finished product, and the detection result is shown in figure 4.
The obtained negative electrode material was used to prepare a half cell for testing, and the test results are shown in table 1 below.
Example 2
Step 1, uniformly mixing petroleum coke with the particle size of 20 microns and powdered iron hydroxide according to the weight ratio of 100:40 to obtain a mixture I;
step 2, graphitizing the mixture I at 3250 ℃ to obtain a graphitized material;
step 3, uniformly mixing the obtained graphitized material under the condition of not adding a coating agent to obtain a mixture II; the uniformly mixing can crush the sintered graphitized material by stirring and the like, and the graphitized material is uniformly mixed and is convenient to screen;
and 4, screening the mixture II to obtain a finished product.
Scanning electron microscope detection is carried out on the prepared finished product, and the detection result is shown in figure 5.
The obtained negative electrode material was used to prepare a half cell for testing, and the test results are shown in table 1 below.
Example 3
Step 1, uniformly mixing calcined needle coke with the particle size of 7 microns and powdered calcium oxide according to the weight ratio of 100:10 to obtain a mixture I;
step 2, carrying out graphitization treatment on the mixture I at 2000 ℃ to obtain a graphitized material;
step 3, mixing the obtained graphitized material and polyvinylidene fluoride at normal temperature of 100:6 for 30min, heating to 300 ℃ at the speed of 10 ℃/min, heating to 540 ℃ at the speed of 5 ℃/min, preserving heat for 4h, naturally cooling to room temperature, keeping the stirring speed for 15 revolutions per minute in the whole process, and preserving heat to obtain a mixture II;
and 4, carbonizing the mixture II at 1200 ℃, cooling and screening to obtain a finished product.
Scanning electron microscope detection is carried out on the prepared finished product, and the detection result is shown in fig. 6.
The obtained negative electrode material was used to prepare a half cell for testing, and the test results are shown in table 1 below.
Example 4
Step 1, uniformly mixing raw needle coke with the particle size of 12 microns with powdery alumina according to the weight ratio of 100:5 to obtain a mixture I;
step 2, carrying out graphitization treatment on the mixture I at 2600 ℃ to obtain a graphitized material;
step 3, uniformly mixing the obtained graphitized material under the condition of not adding a coating agent to obtain a mixture II;
and 4, screening the mixture II to obtain a finished product.
Scanning electron microscope detection is carried out on the prepared finished product, and the detection result is shown in figure 7.
The obtained negative electrode material was used to prepare a half cell for testing, and the test results are shown in table 1 below.
Comparative example 1
Comparative example 1 is different from example 1 in that powdered iron hydroxide containing an oxygen-containing metal compound is not added, and other steps and parameters are the same as those of example 1.
Scanning electron microscope detection is carried out on the prepared finished product, and the detection result is shown in figure 8.
The obtained negative electrode material was used to prepare a half cell for testing, and the test results are shown in table 1 below.
Comparative example 2
Comparative example 2 is different from example 2 in that powdery basic copper carbonate containing an oxygen-containing metal compound is not added, and other steps and parameters are the same as those of example 2.
Scanning electron microscope detection is carried out on the prepared finished product, and the detection result is shown in fig. 9.
The obtained negative electrode material was used to prepare a half cell for testing, and the test results are shown in table 1 below.
Comparative example 3
Comparative example 3 is different from example 3 in that powdered calcium oxide containing an oxygen-containing metal compound is not added, and other steps and parameters are the same as those of example 3.
Scanning electron microscope detection is carried out on the prepared finished product, and the detection result is shown in figure 10.
The obtained negative electrode material was used to prepare a half cell for testing, and the test results are shown in table 1 below.
Comparative example 4
Comparative example 4 is different from example 4 in that powdered alumina of an oxygen-containing metal compound is not added and other steps and parameters are the same as those of example 4.
Scanning electron microscope detection is carried out on the prepared finished product, and the detection result is shown in fig. 11.
The obtained negative electrode material was used to prepare a half cell for testing, and the test results are shown in table 1 below.
TABLE 1 half-cell Performance test results of negative electrode materials of examples 1 to 4 and comparative examples 1 to 4
As shown in table 1, the raw materials of examples 1 and 2 are consistent with those of comparative examples 1 and 2, the treatment process is different, the ratio of the finished product is increased due to the oxidative pore-forming in comparative example 2 and comparative example 2, the ratio of the coating can be effectively reduced in comparative example 1 and example 2, which is consistent with the SEM image, and it can be seen that the pores of example 1 are filled with the coating agent, so the ratio is reduced.
The 0.2C reversible capacity of example 1 is slightly lower than that of example 2 due to the soft carbon coating sacrificing some of the capacity, but at 10C rate, the lithium intercalation capacity of example 1 and DCIR at 50% SOC are better than that of example 2 because the soft carbon acts as a funnel during high rate intercalation, directing lithium ions into the pores or graphite sheets, buffering, and thus the high rate charge condition coated carbon product has a high intercalation capacity. Comparing examples 1, 2 with comparative examples 1, 2, it can be seen that the capacity of examples 1, 2 with the pore forming treatment is higher at 0.2C rate and 10C rate, which is mainly due to the fact that pores provide deintercalation channels for lithium ions during charging and discharging, as shown in fig. 1 again, and thus the DCIR is smaller at 50% SOC.
The same rule is kept in examples 3 and 4 and comparative examples 3 and 4, and the rate capability of the product subjected to the oxidized pore-forming treatment is better.
In addition, the introduction of the oxidant does not cause the trace elements of the product to be abnormally increased, which is mainly benefited from the disappearance of the impurity atoms in the graphitization process through gasification escape at high temperature. In addition, all products are made into soft packages and subjected to full electric test, the NCM is matched with the positive electrode, and the result shows that the cycle life of the products is not shortened due to oxidation pore-forming.
The above-mentioned embodiments, objects, technical solutions and advantages of the present invention are further described in detail, it should be understood that the above-mentioned embodiments are only examples of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (5)
1. A preparation method of a high-rate graphite negative electrode material is characterized by comprising the following steps:
mixing a first carbon source material and a powdery oxygen-containing metal compound according to a weight ratio of 100: 1-50 to obtain a first mixture;
graphitizing the first mixture at 2000-3300 ℃ to obtain a graphitized material; in the graphitization treatment process, the powdery oxygen-containing metal compound oxidizes and corrodes a circular hole on the surface of the first carbon source material;
uniformly mixing the graphitized material and a second carbon source material according to the weight ratio of 100: 6-10 at room temperature or at a heating condition to obtain a second mixture; wherein the temperature rise temperature is not more than 700 ℃;
carbonizing the second mixture at 700-1300 ℃, cooling and screening to obtain a high-rate graphite negative electrode material;
the powdery oxygen-containing metal compound comprises one or more of aluminum hydroxide, aluminum oxide, copper oxide, basic copper carbonate, zinc oxide, calcium oxide, manganese dioxide and potassium permanganate;
the first carbon source material comprises one or more of mesocarbon microbeads, petroleum coke, pitch coke, needle coke, or coke; the second carbon source material comprises pitch powder and/or resin powder; the resin powder comprises one or more of polyvinylidene fluoride, phenolic resin and polyethylene.
2. The preparation method of the high-rate graphite anode material according to claim 1, wherein the particle size of the first carbon source material is 5-30 μm.
3. The preparation method of the high-rate graphite negative electrode material according to claim 1, wherein the temperature rise condition is constant-speed temperature rise or multi-stage variable-speed combined temperature rise, and the temperature rise rate is 1-10 ℃/min.
4. A high-rate graphite negative electrode material prepared by the preparation method of any one of claims 1 to 3.
5. A lithium ion battery comprising the high-rate graphite negative electrode material of claim 4.
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| CN112952070A (en) * | 2021-04-08 | 2021-06-11 | 黑龙江省宝泉岭农垦溢祥新能源材料有限公司 | Graphite lithium battery negative electrode material and preparation method thereof |
| CN114400324B (en) * | 2022-01-20 | 2023-09-19 | 深圳市金润能源材料有限公司 | Preparation method of anode material, anode material and lithium ion battery |
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