CN114430030B - Soft carbon with multi-interface structure, preparation method and energy storage application thereof - Google Patents

Soft carbon with multi-interface structure, preparation method and energy storage application thereof Download PDF

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CN114430030B
CN114430030B CN202210042849.XA CN202210042849A CN114430030B CN 114430030 B CN114430030 B CN 114430030B CN 202210042849 A CN202210042849 A CN 202210042849A CN 114430030 B CN114430030 B CN 114430030B
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soft carbon
asphalt
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dispersion liquid
carbon
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CN114430030A (en
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宋怀河
袁满
陈晓红
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Beijing University of Chemical Technology
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    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M4/36—Selection of substances as active materials, active masses, active liquids
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
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    • C01B32/00—Carbon; Compounds thereof
    • C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
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    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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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
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Abstract

The invention provides soft carbon with a multi-interface structure, a preparation method and energy storage application thereof, and relates to the field of sodium ion battery electrode materials. The specific surface area of the multi-interface soft carbon is 10m 2 About/g, tap density between 0.7 and 1.1g/mL, the added high-conductivity nano material is uniformly embedded and dispersed in the soft carbon, a large number of communicated interface structures exist between the nano material with higher crystallinity and the soft carbon matrix with lower crystallinity, and the surface and the inside of the soft carbon are provided with fold structures. Dripping the high-conductivity nano material dispersion liquid into the asphalt dispersion liquid, and evaporating the solvent; and then carbonizing in nitrogen environment to obtain the final product. When the material is used as a negative electrode material of a sodium ion battery, the material has excellent reversible capacity and rate capability.

Description

Soft carbon with multi-interface structure, preparation method and energy storage application thereof
Technical Field
The invention relates to the field of sodium ion battery electrode materials, in particular to soft carbon with a multi-interface structure, a preparation method and energy storage application thereof.
Background
With the continuous development and progress of new energy technology, the trend of replacing the traditional fuel oil vehicles by electric vehicles is more obvious. At present, batteries of electric vehicles mainly comprise lithium ion batteries, but the comprehensive popularization of the electric vehicles is seriously hindered by the limited reserve of lithium resources. As an element of the same main group as lithium, sodium has electrochemical properties similar to lithium and reserves in the crust of earth much higher than lithium, so sodium ion batteries are expected to become a supplement and replacement for lithium ion batteries.
The negative electrode material is a key factor for restricting the trend of the sodium ion battery to practical use. Graphite materials are the most widely used negative electrode materials in lithium ion batteries, but they do not exhibit an effective sodium storage capacity in sodium ion batteries. The hard carbon material shows higher reversible sodium storage capacity by virtue of larger carbon layer spacing, rich pore structure and defect sites, and becomes the sodium ion battery anode material which is most concerned at present. However, such high reversible capacity of hard carbon exhibits a relatively rapid decay at high current densities, resulting in a battery exhibiting a relatively low power density that is detrimental to the power battery's fast charge and fast discharge requirements. As another amorphous carbon material, the reversible capacity of soft carbon decays slowly with increasing current density, showing greater potential in the preparation of high power density sodium ion batteries, however, the lower reversible capacity at small current densities also limits the application of soft carbon.
Asphalt is a byproduct of coal chemical industry and petrochemical industry, is rich in yield and low in price, is rich in polycyclic aromatic hydrocarbon structure, has higher carbonization yield, and is a high-quality carbonaceous precursor. After the asphalt is directly carbonized, a typical soft carbon material is obtained, and when the material is used for a negative electrode of a sodium ion battery, the material only shows low reversible capacity of about 100mA h/g under a small current density of 50mA/g, and the application value is lacked. In order to improve the sodium-storage reversible capacity of the asphalt-based soft carbon, lu et al (Advanced Energy Materials) (8, 2018, 1800108) published an article entitled "Pre-Oxidation-Tuned Microstructures of Carbon Anodes Derived from Pitch for Enhancing Na Storage Performance", a cross-linked structure is constructed by Pre-oxidizing asphalt in a muffle furnace, so that ordered rearrangement of carbon layers in the carbonization process of asphalt is blocked, the disorder degree of carbonized products is improved, and finally the asphalt-based carbon material with high reversible capacity is obtained. In addition, asphalt is compounded with hard carbon precursors such as resin, sucrose, coal and the like and then carbonized, so that the sodium storage reversible capacity of the product is improved. However, the final products obtained by the modification methods are actually converted into hard carbon materials, and the reversible capacity is improved, but the high rate performance of the soft carbon materials is lost. On the basis of maintaining the high rate performance of the soft carbon material, the method for improving the reversible capacity of the soft carbon material under the low current density is still a problem to be solved at present.
Disclosure of Invention
In order to overcome the problems of the prior art, the invention aims to provide soft carbon with a multi-interface structure characteristic, a preparation method and energy storage application thereof, and is characterized in that:
the specific surface area of the multi-interface soft carbon obtained by the invention is 10m 2 About/g, tap density between 0.7 and 1.1g/ml, the added high-conductivity nano material is uniformly embedded and dispersed in the soft carbon, a large number of communicated interface structures exist between the nano material with higher crystallinity and the soft carbon matrix with lower crystallinity, and the surface and the inside of the soft carbon are provided with fold structures.
The preparation method of the multi-interface soft carbon comprises the following steps:
step 1): asphalt is taken as a raw material, dispersed in an organic solvent according to a certain proportion, and stirred for a certain time to form stable asphalt dispersion liquid;
step 2): dispersing a certain amount of high-conductivity nano material in deionized water, and respectively carrying out ultrasonic treatment and stirring treatment to form stable nano material dispersion;
step 3): heating the asphalt dispersion liquid to 100-200 ℃ at a certain stirring rate, then slowly dripping the nano material dispersion liquid into the asphalt dispersion liquid, and keeping the temperature constant until the solvent is completely evaporated;
step 4): carbonizing the product of the step 3) to obtain a final product.
The carbon source is selected from petroleum asphalt, coal asphalt, synthetic asphalt or coal liquefaction residues, and the high-conductivity nanomaterial is selected from one or more of one-dimensional or two-dimensional materials such as carbon nanotubes, graphene oxide, graphene, mxene and the like.
The mass of the high-conductivity nano material accounts for 0.1-10% of the mass of the asphalt. The concentration of the asphalt dispersion liquid is 5-100 mg ml -1 The concentration of the high-conductivity nano material dispersion liquid is 0.1-10 mg ml -1 。
The carbonization temperature is 800-1200 ℃.
The invention obtains a soft carbon material with a multi-interface structure and applies the soft carbon material to a negative electrode material of a sodium ion battery.
Compared with the prior art, the invention has the advantages that the high-conductivity nano material is uniformly embedded into the soft carbon in a three-dimensional network structure, a large number of communicated interface structures exist between the nano material with higher crystallinity and the soft carbon matrix with lower crystallinity, and the interface structures can be used as channels for ions and electrons to enter the soft carbon matrix and diffuse in the soft carbon matrix at high speed, so that the improvement of the rate performance is realized. The embedded three-dimensional network can prevent the carbon layer structure inside the soft carbon from developing towards the long-range ordered structure, and improve the disorder degree of the soft carbon, thereby achieving the purpose of improving the reversible capacity. The charge-discharge curve of the carbonized product has only a slope area and does not have a platform area special to the hard carbon material, which also shows that the disordered degree is improved, but the final product with multiple interfaces still belongs to the soft carbon material.
Drawings
FIG. 1 is a high resolution transmission electron microscope image of the multi-interface soft carbon of example 1 of the present invention;
FIG. 2 is a charge-discharge curve of the multi-interface soft carbon of example 2 of the present invention.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and examples, but the present invention is not limited to the following examples. Conditions for electrode testing when used as a negative electrode material for sodium ion batteries in the following examples: the electrode composition is 80% of the multi-interface soft carbon material, 10% of Super P and 10% of PVDF, and the electrolyte composition is 1mol of NaPF 6 Dissolved in a solvent having a volume ratio of EC to DEC of 1:1.
Example 1
5g of coal tar pitch and 100ml of toluene solution were mixed and stirred for 2 hours to obtain a dispersion of pitch. Dispersing 50mg of graphene oxide in 100ml of deionized water, and performing ultrasonic treatment, stirring and the like to form uniform graphene oxide dispersion; heating the asphalt dispersion liquid in an oil bath at 100 ℃, controlling the stirring speed of 200r/min, slowly dropwise adding the graphene oxide dispersion liquid, and keeping the temperature and the rotating speed constant until the solvent is completely evaporated; and (3) carbonizing the product in a nitrogen atmosphere at 800 ℃ to obtain a final product. Specific surface area of 9.5m 2 g -1 Tap density of 0.9g ml -1 。
As shown in a High Resolution Transmission Electron Microscope (HRTEM) of the attached figure 1, graphene is uniformly embedded in a soft carbon matrix in a three-dimensional network structure, and a large number of interface structures exist between the graphene with higher crystallinity and the soft carbon matrix with lower crystallinity.
As shown in the electrochemical performance test result of figure 2, when the electrode material is used as a negative electrode material of a sodium ion battery, the electrode material shows typical charge and discharge behaviors of a soft carbon material and only has a slope type sodium storage capacity. At 0.05mA g -1 The specific discharge capacity under the current density can reach 252mA h g -1 The method comprises the steps of carrying out a first treatment on the surface of the At 20A g -1 The specific discharge capacity can still be kept at 103mA h g under the condition of ultra-large current density -1 。
Example 2
2g of petroleum asphalt and 100mL of tetrahydrofuran solution were mixed and stirred for 2 hours to obtain a dispersion of asphalt. Dispersing 100mg of MXene in 100ml of deionized water, and performing ultrasonic treatment, stirring and the like to form uniform MXene dispersion; heating the asphalt dispersion liquid in an oil bath at 100 ℃, controlling the stirring speed of 200r/min, slowly dropwise adding the MXene dispersion liquid, keeping the temperature and the rotating speed constant until the solvent is completely evaporated; and (3) carbonizing the product at 1200 ℃ in a nitrogen atmosphere to obtain a final product. Specific surface area of 10.6m 2 g -1 Tap density of 0.8g ml -1 。
The electrochemical performance test result shows that when the electrode material is used as the negative electrode material of the sodium ion battery, the electrode material is 0.05mA g -1 The specific discharge capacity under the current density can reach 265mA h g -1 The method comprises the steps of carrying out a first treatment on the surface of the At 20A g -1 The specific discharge capacity can still be kept at 97mA h g under the ultra-large current density -1 。
Example 3
10g of a coal liquefaction residue and 100ml of a pyridine solution were mixed and stirred for 2 hours to obtain a dispersion of the coal liquefaction residue. Dispersing 50mg of graphene oxide and 100mg of carbon nano tubes in 100ml of deionized water, and performing ultrasonic treatment, stirring and the like to form uniform graphene oxide/carbon nano tube dispersion; heating the dispersion liquid of the coal liquefaction residues in an oil bath at 100 ℃, controlling the stirring speed of 200r/min,slowly dripping graphene oxide/carbon nano tube dispersion liquid, keeping the temperature and the rotating speed constant until the solvent is completely evaporated; and (3) carbonizing the product at 1000 ℃ in a nitrogen atmosphere to obtain a final product. Specific surface area of 7.8m 2 g -1 Tap density of 0.9g ml -1 。
The electrochemical performance test result shows that when the electrode material is used as the negative electrode material of the sodium ion battery, the electrode material is 0.05mA g -1 The specific discharge capacity under the current density can reach 241mA h g -1 The method comprises the steps of carrying out a first treatment on the surface of the At 20A g -1 The specific discharge capacity can still be kept at 89mA h g under the ultra-large current density -1 。
Example 4
7g of synthetic asphalt and 100ml of toluene solution were mixed and stirred for 2 hours to obtain a dispersion of asphalt. Dispersing 10mg of carbon nano tube in 100ml of deionized water, and performing ultrasonic treatment, stirring and the like to form uniform carbon tube dispersion; heating the asphalt dispersion liquid in an oil bath at 100 ℃, controlling the stirring speed of 200r/min, slowly dripping the carbon tube dispersion liquid, and keeping the temperature and the rotating speed constant until the solvent is completely evaporated; and (3) carbonizing the product at 800 ℃ in a nitrogen atmosphere to obtain a final product. Specific surface area of 8.5m 2 g -1 Tap density of 0.8g ml -1 。
The electrochemical performance test result shows that when the electrode material is used as the negative electrode material of the sodium ion battery, the electrode material is 0.05mA g -1 The specific discharge capacity under the current density can reach 229mA h g -1 The method comprises the steps of carrying out a first treatment on the surface of the At 20A g -1 The specific discharge capacity can still be kept at 62mA h g under the current density -1 。
While the preferred embodiments of the present invention have been illustrated and described, the present invention is not limited to the embodiments, and various equivalent modifications and substitutions can be made by one skilled in the art without departing from the spirit of the present invention, and these equivalent modifications and substitutions are intended to be included in the scope of the present invention as defined in the appended claims.

Claims (5)

1. The preparation method of the soft carbon with the multi-interface structure is characterized by comprising the following steps:
step 1): asphalt is taken as a raw material, dispersed in an organic solvent according to a certain proportion, and stirred for a certain time to form stable asphalt dispersion liquid;
step 2): dispersing a certain amount of high-conductivity nano material in deionized water, and respectively carrying out ultrasonic treatment and stirring treatment to form stable nano material dispersion;
step 3): heating the asphalt dispersion liquid to 100-200 ℃ at a certain stirring rate, then slowly dripping the nano material dispersion liquid into the asphalt dispersion liquid, and keeping the temperature constant until the solvent is completely evaporated;
step 4): carbonizing the product of the step 3) to obtain a final product;
the specific surface area of the obtained soft carbon with the multi-interface structure is 10m 2 About/g, tap density between 0.7 and 1.1g/ml, the added high-conductivity nano material is uniformly embedded and dispersed in the soft carbon, a large number of communicated interface structures exist between the nano material with higher crystallinity and the soft carbon matrix with lower crystallinity, and the surface and the inside of the soft carbon are provided with fold structures.
2. A method according to claim 1, characterized in that: the carbon source is selected from petroleum asphalt, coal asphalt, synthetic asphalt and the like, and the high-conductivity nano material is selected from one or more of carbon nano tubes, graphene oxide, graphene, MXene and the like.
3. A method according to claim 1, characterized in that: the mass of the high-conductivity nano material accounts for 0.1-10% of the mass of asphalt, and the concentration of the asphalt dispersion liquid is 5-100 mg mL -1 The concentration of the high-conductivity nano material dispersion liquid is 0.1-10 mg mL -1 。
4. A method according to claim 1, characterized in that: when asphalt is dispersed, one of toluene, pyridine, tetrahydrofuran, DMF and other organic solvents is selected.
5. A soft carbon material having a multi-interface structure obtained by the method of claims 1 to 4, characterized by being used as a negative electrode material for sodium ion batteries.
CN202210042849.XA 2022-01-14 2022-01-14 Soft carbon with multi-interface structure, preparation method and energy storage application thereof Active CN114430030B (en)

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CN114906834A (en) * 2022-05-09 2022-08-16 北京化工大学 Preparation method and energy storage application of silicon carbon/graphene composite material
CN115275190B (en) * 2022-09-22 2023-05-16 中国科学院山西煤炭化学研究所 Self-supporting soft/hard carbon film for negative electrode of sodium ion battery and preparation and application thereof
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