CN114275764A - Preparation method and application of carbon material based on co-carbonization of porous carbon and thermoplastic carbon source - Google Patents
Preparation method and application of carbon material based on co-carbonization of porous carbon and thermoplastic carbon source Download PDFInfo
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Abstract
The invention discloses a preparation method and application of a carbon material based on co-carbonization of porous carbon and a thermoplastic carbon source, wherein the preparation method comprises the following steps: uniformly mixing porous carbon and a thermoplastic carbon source; drying the mixed sample, transferring the dried mixed sample to a high-temperature furnace protected by inert atmosphere, performing low-temperature melting treatment, and performing high-temperature carbonization treatment; and step three, cooling to room temperature to obtain the secondary ion battery cathode carbon material. The invention is based on a porous carbon material which is widely applied and mature in preparation process, realizes the cooperative optimization of a pore structure and a microcrystalline structure of the carbon material by constructing a novel carbon material with a homomorphic heterogeneous composite structure, is applied to the cathode of a secondary ion battery, has the cooperative promotion effect of ion adsorption and embedding behaviors, and improves the coulombic efficiency, capacity, multiplying power and cycle stability of the cathode of the secondary ion battery in the first circle.
Description
Technical Field
The invention relates to a preparation method and application of a carbon-based negative electrode material of a secondary ion battery, in particular to a preparation method of a carbon material based on co-carbonization of porous carbon and a thermoplastic carbon source and application of the carbon material as a negative electrode of the secondary ion battery.
Background
The carbon material is the most common and ideal negative electrode material of the secondary ion battery (lithium/sodium/potassium ion battery) at present, but is limited by the energy storage mechanism of the existing graphite negative electrode system, and the requirement of future development is difficult to meet. The energy storage mechanism of the carbon cathode material of the secondary ion battery mainly comprises two modes of adsorption and embedding. The adsorption energy storage mechanism is mainly related to active sites on the surface of a material pore structure, and energy storage and release are realized through the adsorption/desorption of ions on the active sites; the embedded energy storage mechanism is mainly related to the microcrystalline structure of the material, and the energy storage and release are realized through the embedding and the extraction of ions in the microcrystalline. The regulation and control of the multi-scale structure of the carbon material to strengthen the storage and transportation of the energy-carrying ions is an important direction for the research and development of the carbon-based negative electrode material at present.
Porous carbon is a typical carbon material, and particularly, coal-based and biomass-based porous carbon is widely applied to the fields of liquid/gas phase adsorption, electrochemical energy storage and the like at present. Due to the developed pore structure of the porous carbon, the energy storage mode of the porous carbon mainly based on an adsorption mechanism is determined, so that the porous carbon is mainly applied to a super capacitor in the field of electrochemical energy storage. Due to the developed pore structure and the extremely short-range microcrystalline structure in the porous carbon, the porous carbon has almost no ion intercalation behavior when being used for a secondary ion battery, so that the reversible capacity is low; a large number of defect structures exist on the surface of the pore structure, so that ions have irreversible adsorption behavior, and the coulomb efficiency of the first circle is low. Therefore, the porous carbon is difficult to be directly used as a negative electrode material for a secondary ion battery.
The cooperative optimization of the microcrystalline structure and the pore structure of the carbon-based negative electrode material is the key for improving the ion storage performance. Researchers first try to improve their performance by optimizing the crystallite structure. Relevant studies indicate that the hard carbon material having a short-range disordered microcrystalline structure has more stable and higher ion storage properties than the graphite material having a long-range ordered microcrystalline structure. On this basis, researchers have also begun to focus on the role that the pore structure plays in ion storage. Recent researches show that the extremely microporous and closed pore structure of the carbon material is beneficial to ion storage, and can greatly improve the reversible capacity of a low-voltage area. Because the crystallite and the pore structure of the carbon material are interdependent, the synergistic optimization of the crystallite and the pore structure is difficult to realize. Aiming at the problem, the development of the carbon material with the homomorphic heterogeneous composite structure is expected to realize the cooperative optimization of the pore and microcrystal structures in a cooperative manner, and the performance of the carbon-based negative electrode material is further improved.
CN109742399A discloses a sodium ion battery cathode material and a preparation method thereof, the patent provides a method for coating hard carbon with soft carbon and a method for coating soft carbon with hard carbon to improve the storage and transportation characteristics of sodium ions, various treatment means such as carbonization, activation, ball milling mixing, re-carbonization and the like are adopted, and the process is relatively complex. In addition, since both hard and soft carbons are subjected to a high temperature carbonization process, the coating of the hard/soft carbons is not uniform during a subsequent solid-phase mixing process. CN108874774B discloses a composite carbon material of soft carbon coated hard carbon with a core-shell structure, but the composite carbon material has the problems of poor uniformity among composite structures, complex process and the like.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method and application of a carbon material based on co-carbonization of porous carbon and a thermoplastic carbon source. The invention is based on a porous carbon material which is widely applied and mature in preparation process, realizes the cooperative optimization of a pore structure and a microcrystalline structure of the carbon material by constructing a novel carbon material with a homomorphic heterogeneous composite structure, is applied to the cathode of a secondary ion battery, has the cooperative promotion effect of ion adsorption and embedding behaviors, and improves the coulombic efficiency, capacity, multiplying power and cycle stability of the cathode of the secondary ion battery in the first circle.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a carbon material based on co-carbonization of porous carbon and a thermoplastic carbon source comprises the following steps:
step one, uniformly mixing porous carbon and a thermoplastic carbon source, wherein:
the porous carbon is one or more of coal-based activated coke, wood activated carbon, commercial super-capacity carbon and other biomass porous carbon;
the particle size of the porous carbon is 0.1-100 mu m, and the specific surface area is 100-3000 m2G, pore volume>0.1 cm3/g；
The thermoplastic carbon source is one or more of coal tar, coal pitch, petroleum pitch, heavy oil and thermoplastic resin;
the mixing mode is direct mixing or mixing by dissolving in a solvent, and the solvent is one or more of dichloromethane, trichloromethane, toluene, ethanol, tetrahydrofuran and deionized water;
the mass ratio of the porous carbon to the thermoplastic carbon source is 1: 0.1 to 10;
step two, transferring the dried mixed sample to a high-temperature furnace protected by inert atmosphere, performing low-temperature melting treatment, and performing high-temperature carbonization treatment, wherein:
the inert atmosphere is one or more of nitrogen, argon and helium;
the low-temperature melting treatment temperature is 200-400 ℃, the time is 0-2 h, and the heating rate is 1-10 ℃/min;
the high-temperature carbonization temperature is 800-1800 ℃, the time is 0.5-4 h, and the heating rate is 1-10 ℃/min;
and step three, cooling to room temperature to obtain the secondary ion battery cathode carbon material.
The carbon material prepared by the method can be used as a secondary ion battery cathode, wherein:
the negative electrode of the secondary ion battery is a negative electrode of a sodium ion battery or a negative electrode of a potassium ion battery;
the reversible capacity of the negative electrode of the sodium ion battery is not less than 300 mAh g-1The first turn coulombic efficiency is not lower than 80%;
the reversible capacity of the negative electrode of the potassium ion battery is not less than 300 mAh g-1And the coulomb efficiency of the first circle is not lower than 60%.
Compared with the prior art, the invention has the following advantages:
(1) the preparation method of the carbon material based on the co-carbonization of the porous carbon and the thermoplastic carbon source, which is provided by the invention, takes the porous carbon with wide application and mature preparation process and the thermoplastic carbon source with low cost as raw materials, and can obtain the secondary ion battery cathode material through simple mixing and co-carbonization treatment, so that the preparation method has the advantages of low cost of the raw materials, simple preparation process and amplified application potential.
(2) Compared with the traditional hard carbon or graphite-based negative electrode material, the carbon-based material with the homomorphic heterostructure provided by the invention realizes the coupling reinforcement of two energy storage mechanisms of ion adsorption and intercalation through the cooperative optimization of the pore and microcrystalline structure. The thermoplastic carbon source and the porous carbon after mixing are subjected to low-temperature melting, and the thermoplastic carbon source is fully permeated into pores of the porous carbon to realize full, deep and uniform combination of the thermoplastic carbon source and the porous carbon; after high-temperature carbonization treatment, on one hand, the invalid pores of the porous carbon can be reduced by carbonizing the thermoplastic carbon source, and the irreversible capacity is reduced; on the other hand, the microcrystalline structure formed by carbonizing the thermoplastic carbon source can be used as a place for ion insertion and storage, and the conductivity of the composite structure is improved. Through the process, the cooperative optimization of the microcrystalline structure and the pore structure is realized. In addition, in the process of forming the homomorphic heterostructure, larger pores in the porous carbon can be converted into a very microporous or closed pore structure, so that the ion filling storage capacity in a low-voltage interval is enhanced.
(3) The invention obviously improves the performance of the cathode of the secondary ion battery through the cooperative reinforcement of a plurality of ion storage mechanisms. When the obtained carbon-based isomeric material is used as a sodium ion battery cathode, the reversible capacity exceeds 300 mAh/g, the coulombic efficiency of the first circle exceeds 80%, and the capacity retention rate exceeds 90% after 100 cycles under the current density of 1C (1C =300 mA/g). When the obtained carbon-based isomeric material is used as a potassium ion battery cathode, the reversible capacity exceeds 300 mAh/g, and the coulombic efficiency of the first circle exceeds 65%.
Drawings
FIG. 1 is a scanning electron microscope image of a sample obtained in example 1.
FIG. 2 is an X-ray diffraction pattern of the sample obtained in example 1.
FIG. 3 shows Raman spectrum data of the sample obtained in example 1.
Fig. 4 shows nitrogen adsorption and desorption test data of the sample obtained in example 1.
FIG. 5 is the rate capability data for the sample obtained in example 1.
FIG. 6 is the cycle performance data for the sample obtained in example 1.
FIG. 7 shows constant current charge and discharge data of the sample obtained in example 2.
Fig. 8 is a scanning electron microscope image of the sample obtained in comparative example 1.
FIG. 9 is an X-ray diffraction pattern of the sample obtained in comparative example 1.
Fig. 10 is raman spectrum data of the sample obtained in comparative example 1.
Fig. 11 is data of nitrogen adsorption desorption test of the sample obtained in comparative example 1.
Fig. 12 is galvanostatic charge and discharge data for the sample obtained in comparative example 1.
Detailed Description
The technical solutions of the present invention are further described below with reference to the following examples, but the present invention is not limited thereto, and any modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Example 1
Mixing commercial super-capacity carbon and coal tar according to a mass ratio of 1: 1, stirring for 2 hours, and fully drying at 45 ℃ to obtain a mixed gray powder sample; transferring the gray powder into a tube furnace, heating to 1600 ℃ at the heating rate of 2 ℃/min under the argon atmosphere, and keeping the temperature for 2 h; naturally cooling to room temperature, and collecting black powder to obtain the final product. The scanning electron microscope image of the obtained carbon material is shown in fig. 1, the X-ray diffraction spectrum is shown in fig. 2, the Raman spectrum data is shown in fig. 3, and the nitrogen adsorption and desorption curve is shown in fig. 4. When the material is used as a cathode of a sodium-ion battery, the rate performance is shown in figure 5, the cycle performance is shown in figure 6, the reversible capacity of the obtained material can reach 320 mAh/g, the coulombic efficiency of the first cycle can reach 84%, and when the current density is 1C, the capacity retention rate can reach 92% after 100 cycles of circulation.
Example 2
Mixing commercial super-capacity carbon and coal pitch according to a mass ratio of 1: 0.75, mixing uniformly; transferring the mixed sample to a tubular furnace, heating to 400 ℃ at a heating rate of 2 ℃/min under an argon atmosphere, keeping the temperature for 2 hours, and then heating to 1400 ℃ at the same heating rate, keeping the temperature for 2 hours; naturally cooling to room temperature, and collecting black powder to obtain the final product. When the material is used as a cathode of a sodium ion battery, a constant current charge-discharge curve is shown in figure 7, the reversible capacity of the obtained material can reach 341 mAh/g, and the coulombic efficiency of the first circle can reach 80%.
Example 3
Mixing commercial super-capacity carbon and petroleum asphalt according to the mass ratio of 1: 0.75, mixing uniformly; transferring the mixed sample to a tubular furnace, heating to 400 ℃ at a heating rate of 2 ℃/min under an argon atmosphere, keeping the temperature for 2 hours, and then heating to 1400 ℃ at the same heating rate, keeping the temperature for 2 hours; naturally cooling to room temperature, and collecting black powder to obtain the final product. When the material is used as a cathode of a sodium-ion battery, the reversible capacity of the obtained material can reach 329 mAh/g, and the coulomb efficiency of the first circle can reach 83%.
Example 4
Mixing commercial super-capacity carbon and polystyrene according to a mass ratio of 1: 2, uniformly mixing; transferring the mixed sample to a tubular furnace, heating to 400 ℃ at a heating rate of 2 ℃/min under an argon atmosphere, keeping the temperature for 2 hours, and then heating to 1400 ℃ at the same heating rate, keeping the temperature for 2 hours; naturally cooling to room temperature, and collecting black powder to obtain the final product. When the material is used as a cathode of a sodium ion battery, the reversible capacity of the obtained material can reach 303 mAh/g, and the coulombic efficiency of the first circle can reach 81%.
Example 5
Grinding and crushing commercial granular activated carbon, and mixing the ground commercial granular activated carbon with coal tar according to a mass ratio of 1: 1, stirring for 2 hours, and fully drying at 45 ℃ to obtain a mixed gray powder sample; transferring the mixture powder into a tube furnace, heating to 1400 ℃ at the heating rate of 2 ℃/min under the argon atmosphere, and keeping the temperature for 2 h; naturally cooling to room temperature, and collecting black powder to obtain the final product. When the material is used as a cathode of a sodium ion battery, the reversible capacity of the obtained material can reach 310 mAh/g, and the coulomb efficiency of the first circle can reach 80%.
Example 6
Grinding and crushing the commercial columnar active coke, and mixing the crushed commercial columnar active coke with coal tar according to a mass ratio of 1: 1, stirring for 2 hours, and fully drying at 45 ℃ to obtain a mixed gray powder sample; transferring the mixture powder into a tube furnace, heating to 1400 ℃ at the heating rate of 2 ℃/min under the argon atmosphere, and keeping the temperature for 2 h; naturally cooling to room temperature, and collecting black powder to obtain the final product. When the material is used as a cathode of a sodium-ion battery, the reversible capacity of the obtained material can reach 322 mAh/g, and the coulomb efficiency of the first circle can reach 81%.
Example 7
Mixing commercial super-capacity carbon and coal tar according to a mass ratio of 1: 1, stirring for 2 hours, and fully drying at 45 ℃ to obtain a mixed gray powder sample; transferring the mixture powder into a tube furnace, heating to 1400 ℃ at the heating rate of 2 ℃/min under the argon atmosphere, and keeping the temperature for 2 h; naturally cooling to room temperature, and collecting black powder to obtain the final product. When the material is used as a potassium ion battery cathode, the reversible capacity of the obtained material can reach 308 mAh/g, and the coulomb efficiency of the first circle can reach 65%.
Comparative example 1
Transferring commercial super-capacity carbon into a tube furnace, heating to 1400 ℃ at a heating rate of 2 ℃/min under an argon atmosphere, and keeping the temperature for 2 hours; naturally cooling to room temperature, and collecting black powder to obtain the final product. The scanning electron microscope image of the obtained carbon material is shown in fig. 8, the X-ray diffraction spectrum is shown in fig. 9, the Raman spectrum data is shown in fig. 10, the nitrogen adsorption and desorption curve is shown in fig. 11, and the constant current charge and discharge curve is shown in fig. 12. When the material is used as a negative electrode of a sodium-ion battery, the reversible capacity of the obtained material is only 57.1 mAh/g, and the first-turn coulombic efficiency is only 13.92%.
Compared with the carbon material obtained by direct carbonization, the carbon material prepared by co-carbonizing the porous carbon and the thermoplastic carbon source provided by the invention has obviously improved reversible capacity, first-turn coulombic efficiency, multiplying power and cycle performance when used as the cathode of the secondary ion battery, and the feasibility of the method provided by the invention is proved by comparing the example 1 with the comparative example 1.
Comparative example 2
Grinding and crushing the commercial columnar active coke; transferring the mixture into a tube furnace, heating the mixture to 1400 ℃ at the heating rate of 2 ℃/min under the argon atmosphere, and keeping the temperature for 2 hours; naturally cooling to room temperature, and collecting black powder to obtain the final product. When the material is used as a negative electrode of a sodium-ion battery, the reversible capacity of the obtained material is only 161mAh/g, and the coulombic efficiency of the first circle is only 63%.
Claims (9)
1. A method for preparing a carbon material based on the co-carbonization of porous carbon and a thermoplastic carbon source is characterized by comprising the following steps:
step one, uniformly mixing porous carbon and a thermoplastic carbon source, wherein: the mass ratio of the porous carbon to the thermoplastic carbon source is 1: 0.1 to 10;
step two, transferring the dried mixed sample to a high-temperature furnace protected by inert atmosphere, performing low-temperature melting treatment, and performing high-temperature carbonization treatment, wherein: the low-temperature melting treatment temperature is 200-400 ℃, the time is 0-2 h, and the heating rate is 1-10 ℃/min; the high-temperature carbonization temperature is 800-1800 ℃, the time is 0.5-4 h, and the heating rate is 1-10 ℃/min;
and step three, cooling to room temperature to obtain the secondary ion battery cathode carbon material.
2. The method for preparing a carbon material based on the co-carbonization of porous carbon and a thermoplastic carbon source according to claim 1, characterized in that the porous carbon is one or more of coal-based activated coke, wood activated carbon, commercial super-capacity carbon, and other biomass porous carbon.
3. The method for preparing a carbon material based on co-carbonization of porous carbon and a thermoplastic carbon source according to claim 1, characterized in that the particle size of the porous carbon is 0.1 to 100 μm and the specific surface area is 100 to 3000 m2G, pore volume>0.1 cm3/g。
4. The method for preparing a carbon material based on the co-carbonization of porous carbon and a thermoplastic carbon source according to claim 1, characterized in that the thermoplastic carbon source is one or more of coal tar, coal pitch, petroleum pitch, heavy oil, and thermoplastic resin.
5. Method for the preparation of a carbon material based on the co-carbonization of porous carbon with a thermoplastic carbon source according to claim 1, characterized in that the mixing is direct mixing or solvent mixing.
6. The method for preparing a carbon material based on the co-carbonization of porous carbon and a thermoplastic carbon source according to claim 5, wherein the solvent is one or more of dichloromethane, chloroform, toluene, ethanol, tetrahydrofuran, and deionized water.
7. The method for preparing a carbon material based on the co-carbonization of porous carbon and a thermoplastic carbon source according to claim 1, characterized in that the inert atmosphere is one or several of nitrogen, argon, helium.
8. Use of a carbon material based on the co-carbonization of porous carbon with a thermoplastic carbon source, prepared by the method according to any one of claims 1 to 7, in a negative electrode for a secondary ion battery.
9. Use of a carbon material based on the co-carbonization of porous carbon with a thermoplastic carbon source in a negative electrode of a secondary ion battery according to claim 8, characterized in that the negative electrode of a secondary ion battery is a negative electrode of a sodium ion battery or a negative electrode of a potassium ion battery.
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| CN109148838A (en) * | 2017-09-29 | 2019-01-04 | 中国科学院物理研究所 | Anode material of lithium-ion battery and its preparation method and application based on Carbon Materials and pitch |
| CN110330016A (en) * | 2019-08-10 | 2019-10-15 | 哈尔滨工业大学 | An a kind of step cooperative development method of anthracite-base porous carbon graphite microcrystal and hole |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2003346803A (en) * | 2002-05-27 | 2003-12-05 | Asahi Kasei Corp | Negative electrode material, method for manufacturing the same, and battery element |
| US20080025906A1 (en) * | 2004-12-27 | 2008-01-31 | Jiin-Huey Chern Lin | Method for Preparing a Carbon/Carbon Composite |
| CN109148838A (en) * | 2017-09-29 | 2019-01-04 | 中国科学院物理研究所 | Anode material of lithium-ion battery and its preparation method and application based on Carbon Materials and pitch |
| WO2019062495A1 (en) * | 2017-09-29 | 2019-04-04 | 中国科学院物理研究所 | Carbon material and asphalt-based negative electrode material for sodium-ion battery, and preparation method therefor and applications thereof |
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