CN111017903A - High-performance carbon anode PAN hard carbon material and preparation method thereof - Google Patents
High-performance carbon anode PAN hard carbon material and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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Abstract
The invention discloses a high-performance carbon anode PAN hard carbon material and a preparation method thereof, wherein the preparation method comprises the processes of pre-oxidation and carbonization, polyacrylonitrile powder is sintered at high temperature under inert gas to obtain polyacrylonitrile hard carbon microsphere blocks, and the polyacrylonitrile hard carbon microsphere blocks used for the negative electrode material of a lithium ion battery have the advantages of simple preparation method, low cost, environmental protection, no toxicity and the like.
Description
Technical Field
The invention belongs to the functional material technology, relates to a preparation method of a high-performance carbon anode material, and particularly relates to a high-performance carbon anode PAN hard carbon material and a preparation method thereof.
Background
Lithium ion batteries have excellent energy storage characteristics and are widely applied to the fields of mobile communication, information technology, consumer electronics, mobile automobiles and the like. With the progress and development of human society, advanced lithium ion batteries are required to have higher capacity, better rate performance, and longer service life. Among all the components of a lithium ion battery, the electrode material is a key factor that restricts the performance of the lithium ion battery. The negative electrode material is used as an important component of the lithium ion battery and has important influence on the electrochemical performance of the lithium ion battery. In the anode material of the lithium ion battery, the carbon material has the advantages of low electrode potential, high cycle efficiency, long cycle life, good safety performance and the like, and is the preferred anode material of the lithium ion battery.
At present, graphite is a common carbon anode material, has a good layered structure, is suitable for lithium ion intercalation and deintercalation, has the advantages of high conductivity and high reversible specificity, and becomes a widely used traditional commercial anode material. However, conventional graphite anode materials still have some drawbacks, which severely limit their applications. Firstly, the theoretical capacity of the graphite cathode is only 372mAh mu g-1, which is far from the requirement of a high-performance lithium ion battery; secondly, the layered structure has poor stability and is easy to collapse after a long charge discharge period, so that the specific capacity is seriously reduced, and the energy storage life is greatly shortened; third, electrolyte decomposition produces a large irreversible capacity on first discharge. These defects have largely limited the use of graphite anode materials in high performance lithium ion batteries.
Therefore, we have been working on finding new carbon anode materials with high performance, high capacity, stable layered structure, long cycle life, etc. These research works provide a good idea for developing new high-performance carbon anode materials. However, in the case of the layered graphite anode material, in addition to the above-mentioned disadvantages, the interlayer spacing is small and Li + can be inserted only into the end faces of the material, which tends to increase the diffusion resistance of lithium ions. Thus, the poor rate performance of the layered graphite anode limits its application in high power batteries. Therefore, improving the capacity and rate performance of carbon anode materials is an important issue to be solved at present.
The low-temperature amorphous carbon ball has the advantages of simple preparation method, low cost, small pollution, realization of large-scale production and the like, and simultaneously shows high specific capacity, large specific surface area, relatively stable structure and the like when being used as a negative electrode material of a lithium ion battery, so the low-temperature amorphous carbon ball is considered to be one of negative electrode materials with great development prospects. According to the deintercalation mechanism of lithium ions in the carbon material, the microporous structure in the low-temperature amorphous carbon is more suitable for deintercalation of lithium ions.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a high-performance carbon anode PAN hard carbon material, and the high-performance carbon anode material prepared from the high-performance carbon anode PAN hard carbon material has high stability, good high-rate cycle performance and large discharge capacity.
In order to achieve the above object, the present invention adopts the following technical solutions.
A preparation method of a high-performance carbon anode PAN hard carbon material comprises the following steps:
step 1, paving a ceramic boat with polyacrylonitrile powder;
step 3, carbonization: and (3) heating the pre-oxidized polyacrylonitrile obtained in the step (2) to 500-600 ℃ at a speed of 1-3 ℃/min in an inert gas atmosphere, preserving heat for 0.5h, heating to 700-1500 ℃ at a speed of 3-6 ℃/min, preserving heat for 1h, and cooling to room temperature to obtain the high-performance carbon anode PAN hard carbon material.
Further, in the step 1, the relative molecular mass of the polyacrylonitrile powder is 15W.
Further, in the step 2, the temperature is increased to 280 ℃ from the room temperature, and the temperature is kept for 2 hours and then the mixture is cooled to the room temperature.
Further, in the step 3, the temperature is raised to 1100 ℃ for the second time, and the temperature is kept for 1h and then the mixture is cooled to the room temperature.
Further, pre-grinding the PAN hard carbon material obtained in the step 3, sieving the pre-ground PAN hard carbon material with a 100-mesh and 200-mesh sieve, ultrasonically dispersing the obtained powder in an organic solvent at 60 ℃ for 2h, performing suction filtration and drying to obtain pure polyacrylonitrile hard powder, and then grinding the powder with a 270-mesh and 400-mesh sieve to obtain the superfine PAN hard carbon material.
Further, the organic solvent is methanol, ethanol or dimethylformamide.
The invention has the following beneficial effects:
according to the invention, polyacrylonitrile powder is oxidized and carbonized to prepare a product, namely, the polyacrylonitrile powder is sintered at a high temperature under inert gas to obtain polyacrylonitrile hard carbon microsphere blocks, and the polyacrylonitrile is directly sintered to form a carbon material, so that the used raw materials are simple, graphite and other doping materials are not needed, the industrial production cost is low, the raw materials are easy to obtain, and the preparation method has the advantages of simplicity, environmental protection, no toxicity and the like; the carbon material is obtained by directly sintering polyacrylonitrile powder, and the preparation process has low sintering temperature, is easier to realize, is simple to control and is easier for industrial production.
The obtained PAN hard carbon is used as a negative electrode material of a lithium ion battery and is tested to have the initial capacity of 343.5mAhg-1Equal to the graphite electrode (348.6mAh g-1), the initial coulombic efficiency was 87.9% (84.4%) higher than that of the graphite electrode. The charging capacity was 320.1, 219.0, 212.9 and 123.5mAh-1The current was 0.2C, 1C, 2C, and 3C, with efficiencies of 98.1%, 100.6%, 88.1%, and 110.0%, respectively, higher than graphite electrodes (83.8%, 97.6%, 98.8%, and 94.1%), respectively, and PAN hard carbon electrodes had excellent cycling stability and rate performance at different current rates.
In addition, the charging capacity of the PAN hard carbon electrode can be still kept at 336.7mAhg-1(0.2C after 80 cycles), 226.4mAhg-1(1C after 150 cycles), 149.5mAh g-1 (2C after 400 cycles) and 120.0mAh g-1 (3C after 100 cycles), capacity retention rates of 98.8%, 106.7%, 79.7% and 88.6%. The capacity and the volume ratio after circulation are obviously higher than those of a graphite electrode, which shows that the PAN hard carbon electrode has excellent rate performance, and provides a new idea for developing a novel high-performance anode material.
Drawings
FIG. 1 is a graph of the impedance properties of the material prepared in example 3 and graphite
FIG. 2 is a graph of 2C cycle performance of the material prepared in example 3 and graphite
FIG. 3 is the discharge curve of the material prepared in example 3 and graphite
FIG. 4 is a scanning electron micrograph of a material of the present invention in example 3
FIG. 5 is a transmission electron micrograph of the material of example 3 of the present invention
Detailed Description
The present invention will be described in further detail with reference to examples, but the present invention is not limited thereto.
Example 1
Step 1, paving a ceramic boat with polyacrylonitrile powder, wherein the relative molecular mass of the polyacrylonitrile powder is 15W.
Step 3, carbonizing: and (3) heating the pre-oxidized polyacrylonitrile obtained in the step (2) to 600 ℃ from room temperature at a speed of 1 ℃/min in an argon atmosphere, preserving heat for 0.5h, and then heating to 1100 ℃ at a speed of 3 ℃/min, and preserving heat for 1 h. And cooling to room temperature. The high-performance carbon anode PAN hard carbon material prepared by the invention is obtained.
Step 4, impurity cleaning: and (3) grinding the blocks in the step (3), sieving the blocks by a 100-mesh sieve, ultrasonically dispersing the obtained powder in alcohol or dimethylformamide at 60 ℃ for 2h, carrying out suction filtration, drying to obtain pure polyacrylonitrile hard powder, and then grinding the powder by a 400-mesh sieve to obtain the superfine polyacrylonitrile hard carbon material.
Example 2
Step 1, paving a ceramic boat with polyacrylonitrile powder.
Step 3, carbonizing: and (3) heating the pre-oxidized polyacrylonitrile obtained in the step (2) to 500 ℃ from room temperature at a speed of 3 ℃/min in an argon atmosphere, preserving heat for 0.5h, and then heating to 1050 ℃ at a speed of 4 ℃/min, and preserving heat for 1 h. And cooling to room temperature. The high-performance carbon anode PAN hard carbon material prepared by the invention is obtained.
Step 4, impurity cleaning: and (3) grinding the blocks in the step (3), sieving with a 200-mesh sieve, ultrasonically dispersing the obtained powder in methanol at 60 ℃ for 2h, carrying out suction filtration, drying to obtain pure polyacrylonitrile hard powder, and grinding and sieving with a 300-mesh sieve to obtain the superfine polyacrylonitrile hard carbon material.
Example 3
Step 1, paving a ceramic boat with polyacrylonitrile powder.
And 2, placing the porcelain boat into a tube furnace for pre-oxidation treatment. And then heating polyacrylonitrile from room temperature to 300 ℃ at the speed of 3 ℃/min in the oxygen atmosphere, preserving the heat for 2h, and cooling to the room temperature.
Step 3, carbonizing: and (3) heating the pre-oxidized polyacrylonitrile obtained in the step (2) to 550 ℃ from room temperature at the speed of 2 ℃/min in an argon atmosphere, preserving heat for 0.5h, and then heating to 1000 ℃ at the speed of 6 ℃/min, and preserving heat for 1 h. And cooling to room temperature. The high-performance carbon anode PAN hard carbon material prepared by the invention is obtained.
As shown in fig. 1, the impedance diagram of the lithium ion battery negative electrode material prepared by the present invention shows EIS spectra of the PAN hard carbon and graphite electrodes, and in the high frequency region, the semicircular area of the PAN hard carbon electrode is larger than that of the graphite negative electrode, indicating that the impedance of the PAN hard carbon electrode is larger than that of the graphite negative electrode. The PAN hard carbon electrode has a large impedance value, mainly due to the following reasons. First, PAN hard carbon has a larger particle size, resulting in slower transport and migration of charges within the electrode material. Secondly, the C content in PAN hard carbon materials is only around 74%, significantly lower than the carbon content in graphite materials, which is also the reason for its poor electrical conductivity. The PAN hard carbon electrode has good initial charge and discharge properties, although the conductivity is not excellent.
As shown in fig. 2, the initial capacity of the PAN hard carbon electrode is much higher than that of the graphite electrode, as can be clearly seen at 2C rate current of the anode material prepared by the present invention. Also, PAN hard carbon electrodes exhibit more stable cycling performance than graphite electrodes. The charging capacity of 2C was 187.5 and 142.3mAh g-1And is suitable for PAN hard carbon electrode and graphite electrode. After 400 cycles, the capacity retention rates of the PAN hard carbon electrode and the graphite electrode are respectively 79.7% and 73.2%, and the excellent rate capability of the PAN hard carbon material is shown.
As shown in fig. 3, the rate performance of the lithium ion negative electrode material prepared by the invention is compared with that of the PAN material under the current rate of 0.2C, 1C, 2C, 3C and 5C, and the PAN material has similar performance to the graphite at low rate, but has excellent rate performance at medium and high rate. The PAN hard carbon electrode material has potential application prospect, and provides a new idea for designing a high-performance novel carbon cathode material.
As shown in fig. 4 and 5, the lithium ion negative electrode material prepared by the invention has uniform morphology and smooth surface of formed carbon particles by scanning electron microscope pictures and transmission electron microscope pictures.
Example 4
Step 1, paving a ceramic boat with polyacrylonitrile powder.
Step 3, carbonizing: and (3) heating the pre-oxidized polyacrylonitrile obtained in the step (2) to 600 ℃ from room temperature at a speed of 1 ℃/min in an argon atmosphere, preserving heat for 0.5h, and then heating to 950 ℃ at a speed of 3 ℃/min, and preserving heat for 1 h. And cooling to room temperature. The high-performance carbon anode PAN hard carbon material prepared by the invention is obtained.
Step 4, impurity cleaning: and (3) grinding the blocks in the step (3), sieving the blocks by a 100-mesh sieve, ultrasonically dispersing the obtained powder in alcohol or dimethylformamide at 60 ℃ for 2h, carrying out suction filtration, drying to obtain pure polyacrylonitrile hard powder, and then grinding the powder by a 400-mesh sieve to obtain the superfine polyacrylonitrile hard carbon material.
Example 5
Step 1, paving a ceramic boat with polyacrylonitrile powder.
Step 3, carbonizing: and (3) heating the pre-oxidized polyacrylonitrile obtained in the step (2) to 600 ℃ from room temperature at a speed of 1 ℃/min in an argon atmosphere, preserving heat for 0.5h, and then heating to 900 ℃ at a speed of 3 ℃/min, and preserving heat for 1 h. And cooling to room temperature. The high-performance carbon anode PAN hard carbon material prepared by the invention is obtained.
Step 4, impurity cleaning: and (3) grinding the blocks in the step (3), sieving the blocks by a 100-mesh sieve, ultrasonically dispersing the obtained powder in alcohol or dimethylformamide at 60 ℃ for 2h, carrying out suction filtration, drying to obtain pure polyacrylonitrile hard powder, and then grinding the powder by a 400-mesh sieve to obtain the superfine polyacrylonitrile hard carbon material.
The method for testing the half cell comprises the following steps: and (2) uniformly mixing 85% of a negative electrode sample, N-methyl pyrrolidone containing 5% of polyvinylidene fluoride and 10% of conductive carbon black, coating the mixture on a copper foil, weighing the coated pole piece stamped sheet, and putting the stamped sheet into a vacuum drying oven at the temperature of 100 ℃ for vacuum drying for 12 hours for later use. Half-cells were assembled in a German Braun glove box filled with argon, the electrolyte was 1M, LiPF6+ EC: DEC: DMC was 1: 1 (volume ratio), a metallic lithium plate was used as a counter electrode, electrochemical performance tests were performed on an American ArbinBT2000 type cell tester, the charge-discharge voltage ranged from 0.005 to 1.0V, the charge-discharge rate was 0.2C, and high-rate cycle tests were also performed, and the cycle performance of the polyacrylonitrile hard carbon material prepared in examples 1-5 was shown in Table 1.
TABLE 1
| Examples of the invention | 0.2C |
1000℃ | Specific charging capacity |
| 1-1100℃ | 291 | 0.2C | 339 |
| 2-1050℃ | 303 | 1C | 235 |
| 3-1000℃ | 342 | 2C | 187 |
| 4-950℃ | 322 | 3C | 124 |
| 5-900℃ | 309 | 5C | 84 |
The full cell testing method used by the invention comprises the following steps: the polyacrylonitrile hard carbon material (1000 ℃) prepared in the embodiment 3 of the invention is used as a negative electrode, the nickel-cobalt-aluminum ternary positive electrode material is used as a positive electrode, a solution with the volume ratio of 1M-LiPF6EC, DMC, EMC being 1: 1 is used as an electrolyte to assemble a full battery, the discharge specific capacity of the test embodiment 3 is 182 under the multiplying power of 0.2C, and the coulombic efficiency is 87%.
Example 6
Step 1, paving a ceramic boat with polyacrylonitrile powder.
Step 3, carbonizing: and (3) heating the pre-oxidized polyacrylonitrile obtained in the step (2) to 600 ℃ from room temperature at a speed of 1 ℃/min in an argon atmosphere, preserving heat for 0.5h, and then heating to 700 ℃ at a speed of 3 ℃/min, and preserving heat for 1 h. And cooling to room temperature. The high-performance carbon anode PAN hard carbon material prepared by the invention is obtained.
Step 4, impurity cleaning: and (3) grinding the blocks in the step (3), sieving the blocks by a 100-mesh sieve, ultrasonically dispersing the obtained powder in alcohol or dimethylformamide at 60 ℃ for 2h, carrying out suction filtration, drying to obtain pure polyacrylonitrile hard powder, and then grinding the powder by a 400-mesh sieve to obtain the superfine polyacrylonitrile hard carbon material.
Example 7
Step 1, paving a ceramic boat with polyacrylonitrile powder.
Step 3, carbonizing: and (3) heating the pre-oxidized polyacrylonitrile obtained in the step (2) to 600 ℃ from room temperature at a speed of 1 ℃/min in an argon atmosphere, preserving heat for 0.5h, and then heating to 1500 ℃ at a speed of 3 ℃/min, and preserving heat for 1 h. And cooling to room temperature. The high-performance carbon anode PAN hard carbon material prepared by the invention is obtained.
Step 4, impurity cleaning: and (3) grinding the blocks in the step (3), sieving the blocks by a 100-mesh sieve, ultrasonically dispersing the obtained powder in alcohol or dimethylformamide at 60 ℃ for 2h, carrying out suction filtration, drying to obtain pure polyacrylonitrile hard powder, and then grinding the powder by a 270-mesh sieve to obtain the superfine polyacrylonitrile hard carbon material.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the above embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the embodiments of the invention without departing from the spirit and scope of the invention, which is to be covered by the claims.
Claims (7)
1. A preparation method of a high-performance carbon anode PAN hard carbon material is characterized by comprising the following steps:
step 1, paving a ceramic boat with polyacrylonitrile powder;
step 2, pre-oxidation: placing the porcelain boat in an oxygen atmosphere, heating the porcelain boat from room temperature to 250-300 ℃ at the speed of 1-5 ℃/min, preserving heat for 2h, and cooling the porcelain boat to room temperature;
step 3, carbonization: and (3) heating the pre-oxidized polyacrylonitrile obtained in the step (2) to 500-600 ℃ at a speed of 1-3 ℃/min in an inert gas atmosphere, preserving heat for 0.5h, heating to 700-1500 ℃ at a speed of 3-6 ℃/min, preserving heat for 1h, and cooling to room temperature to obtain the high-performance carbon anode PAN hard carbon material.
2. The method for preparing the high-performance carbon anode PAN hard carbon material according to claim 1, wherein the method comprises the following steps: in the step 1, the relative molecular mass of the polyacrylonitrile powder is 15W.
3. The method for preparing the high-performance carbon anode PAN hard carbon material according to claim 1, wherein the method comprises the following steps: and in the step 2, the temperature is increased from room temperature to 280 ℃, and the temperature is kept for 2 hours and then the mixture is cooled to room temperature.
4. The method for preparing the high-performance carbon anode PAN hard carbon material according to claim 1, wherein the method comprises the following steps: and in the step 3, the temperature is raised to 1100 ℃ for the second time, and the temperature is kept for 1h and then the mixture is cooled to the room temperature.
5. The method for preparing the high-performance carbon anode PAN hard carbon material according to claim 1, wherein the method comprises the following steps: pre-grinding the PAN hard carbon material obtained in the step 3, sieving the PAN hard carbon material with a 100-mesh and 200-mesh sieve, ultrasonically dispersing the obtained powder in an organic solvent at 60 ℃ for 2h, performing suction filtration and drying to obtain pure polyacrylonitrile hard powder, and then grinding the polyacrylonitrile hard carbon material with a 270-mesh and 400-mesh sieve to obtain the superfine polyacrylonitrile hard carbon material.
6. The method for preparing the high-performance carbon anode PAN hard carbon material according to claim 5, wherein the method comprises the following steps: the organic solvent is methanol, ethanol or dimethylformamide.
7. A high performance carbon anode PAN hard carbon material made according to the method of claims 1-6.
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| CN112225194A (en) * | 2020-09-24 | 2021-01-15 | 中国科学院化学研究所 | Hard carbon material and preparation method and application thereof |
| CN113224292A (en) * | 2021-02-02 | 2021-08-06 | 江西理工大学 | High-performance lithium ion battery polyacrylonitrile carbon fiber negative electrode material and preparation method thereof |
| CN114436237A (en) * | 2021-12-21 | 2022-05-06 | 华中科技大学 | Hard carbon material and preparation method and application thereof |
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| CN112225194A (en) * | 2020-09-24 | 2021-01-15 | 中国科学院化学研究所 | Hard carbon material and preparation method and application thereof |
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| CN114436237A (en) * | 2021-12-21 | 2022-05-06 | 华中科技大学 | Hard carbon material and preparation method and application thereof |
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