CN113526489B - Performance improvement method and application of sodium ion battery carbon-based negative electrode material - Google Patents
Performance improvement method and application of sodium ion battery carbon-based negative electrode material Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
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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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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- 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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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a performance improvement method and application of a sodium ion battery carbon-based negative electrode material, which comprises the following steps: s1, pre-oxidizing the soft carbon precursor; s2, mixing the pre-oxidized soft carbon precursor with the hard carbon precursor to form a mixture material; s3, placing the obtained mixed material into a high-temperature carbonization furnace; and S4, cooling the high-temperature treatment product to room temperature to obtain an amorphous carbon material, namely the sodium ion battery carbon-based negative electrode material. An electrode material comprises the sodium ion battery carbon-based negative electrode material prepared by the performance improvement method. A negative pole piece of a sodium ion battery comprises the sodium ion battery carbon-based negative pole material prepared by the performance improvement method. A sodium ion battery comprises the negative pole piece. The prepared carbon-based cathode material of the sodium ion battery is applied to the sodium ion battery, so that the sodium ion battery has higher capacity and energy density, stable cycle performance and good safety performance.
Description
Technical Field
The invention relates to a performance improvement method and application, in particular to a performance improvement method and application of a sodium ion battery carbon-based negative electrode material, and belongs to the technical field of battery materials.
Background
With the proposition of the goals of carbon peak reaching and carbon neutralization, the environmental protection consciousness of people is further improved, and the demand of developing renewable energy sources to replace the traditional fossil energy sources is more and more urgent. Secondary energy sources such as wind energy, tidal energy and solar energy have the characteristic of unstable power generation quantity and are difficult to be directly incorporated into the existing power grid. Meanwhile, the existing power grid also has the demand of peak clipping and valley filling. In meeting the above requirements, electrochemical secondary energy storage technology plays an important role.
The sodium ion battery has a similar working principle with the lithium ion battery widely applied at present, and the energy density and the cycle life of the sodium ion battery are both close to those of the lithium ion battery. In addition, the sodium source is widely distributed, the cost is low, and the sodium ion battery is good in safety and easy to maintain. In application scenes such as an energy storage power station and the like sensitive to cost and high in safety requirement, the sodium ion battery has great technical advantages. As early as the 80's of the last century, the research on sodium ion batteries began simultaneously with lithium ion batteries. So far, sodium ion battery positive electrode materials such as layered oxides, polyanions and prussian blue have been developed and can meet basic application requirements. However, the performance of the negative electrode material still limits the further improvement of the performance of the sodium-ion battery.
Among the currently common negative electrode materials for sodium ion batteries, amorphous carbon-based materials have high energy density and long cycle life, and are one of the most promising negative electrode materials for sodium ion batteries. Precursors for preparing amorphous carbon are divided into hard carbon precursors and soft carbon precursors. Wherein, the soft carbon precursors such as petroleum asphalt, coal asphalt and the like have low cost, and the prepared carbon material has good electrical conductivity. However, in the carbonization process, the soft carbon precursor is easily subjected to graphitization reaction after high-temperature treatment, and presents a more ordered microstructure, resulting in low sodium storage capacity. The hard carbon precursor is difficult to graphitize at high temperature, and the obtained carbon has higher disorder degree, so the sodium storage capacity of the hard carbon precursor is higher, but the carbon yield is lower, the cost is relatively high, and the large-scale application of the hard carbon precursor is restricted.
Disclosure of Invention
In order to solve the defects of the technology, the invention provides a method for improving the performance of a carbon-based negative electrode material of a sodium-ion battery and application thereof, which effectively solve the problem that the negative electrode material of the carbon-based battery generates graphitization reaction in the carbonization process and can improve the carbon yield. The carbon-based negative electrode material of the sodium ion battery prepared by the invention has better sodium ion de-intercalation capability and high specific capacity, and the preparation method is simple and has low cost.
In order to solve the technical problems, the invention adopts the technical scheme that: a method for improving the performance of a carbon-based negative electrode material of a sodium-ion battery comprises the following steps:
s1, pre-oxidizing the soft carbon precursor, treating the soft carbon precursor or the soft carbon precursor added with the oxidation catalyst at 200-350 ℃ for 0.5-5 hours in air atmosphere, wherein the soft carbon precursor is subjected to oxidation reaction with the oxidation catalyst and oxygen in the low-temperature treatment process, and the surface of the soft carbon precursor is provided with an oxygen-containing functional group;
s2, mixing the pre-oxidized soft carbon precursor and the hard carbon precursor according to the mass ratio of 1 (1-0.02) to form a mixture material, and in the mixing process, performing a crosslinking reaction on the soft carbon precursor and the hard carbon precursor;
s3, placing the obtained mixed material into a high-temperature carbonization furnace, and carrying out high-temperature treatment for 2-9 hours at 1000-1600 ℃ under inert atmosphere;
and S4, cooling the high-temperature treatment product to room temperature to obtain an amorphous carbon material, namely the sodium ion battery carbon-based negative electrode material.
Preferably, the soft carbon precursor comprises any one of pitch, petroleum coke and needle coke;
the petroleum coke is at least one of green coke and cooked coke;
the needle coke is at least one of coal-based needle coke and petroleum-based needle coke;
the asphalt comprises any one or the combination of at least two of coal asphalt, petroleum asphalt, coal tar, heavy oil in petroleum industry or heavy aromatic hydrocarbon;
the oxidation catalyst is at least one of sulfuric acid, nitric acid and hydrogen peroxide.
Preferably, the heavy aromatic hydrocarbon includes any one of naphthalene, acenaphthene, fluorene, phenanthrene, anthracene, methylnaphthalene, phenylpropafluorene, benzodibenzofuran, triphenylene, thiaphenanthrene, fluoranthene, 1, 2-benzanthracene, or a combination of at least two thereof.
Preferably, the hard carbon precursor comprises one or more of phenolic resin, polyacrylonitrile, lignin and cellulose.
Preferably, the prepared carbon-based negative electrode material of the sodium ion battery is irregular and blocky in macroscopic appearance, has macropores, mesopores or micropores in the interior, and has the microstructure characteristics of short-range order and long-range disorder.
An electrode material comprises a conductive additive, a binder and the sodium ion battery carbon-based negative electrode material prepared by the performance improvement method.
Preferably, the conductive additive comprises one or more of carbon black, acetylene black, vapor deposition carbon fiber, conductive graphite, carbon nanotubes and graphene.
Preferably, the binder comprises one or more of sodium alginate, sodium carboxymethylcellulose, sodium polyacrylate and polyaniline.
A negative pole piece of a sodium-ion battery, the negative pole piece comprising: the sodium ion battery carbon-based negative electrode material is prepared by the current collector, the conductive additive coated on the current collector, the binder and the performance improvement method.
A sodium ion battery comprises the negative pole piece.
According to the invention, soft carbon precursor materials such as asphalt, petroleum coke, needle coke and the like are taken as a main body, hard carbon precursor materials such as phenolic resin, polyacrylonitrile, lignin, cellulose and the like are taken as auxiliary materials, the soft carbon precursor materials are subjected to pre-oxidation treatment, so that the soft carbon precursor materials are provided with oxygen-containing functional groups, and the synergistic effect of the oxygen-containing functional groups on the surface of the pre-oxidized soft carbon precursor materials and the hard carbon precursor materials is further utilized, so that the problem of graphitization in the carbonization process of the soft carbon precursor materials can be solved, the carbon yield is increased, and the electrochemical performance of the soft carbon-based battery materials is improved. The performance improvement method has simple process, and the obtained sodium ion battery carbon-based negative electrode material has the characteristics of high disorder degree, rich sodium storage sites and high reversible capacity.
The prepared carbon-based cathode material of the sodium ion battery is applied to the sodium ion battery, so that the sodium ion battery has higher capacity and energy density, stable cycle performance and good safety performance. The sodium ion battery can meet various application scenes such as intelligent peak regulation of a power grid, renewable energy sources matched energy storage power stations and communication base stations.
Drawings
Fig. 1 is an SEM image of a carbon-based negative electrode material prepared in example 1 of the present invention.
Fig. 2 is an XRD spectrum of the carbon-based negative electrode material prepared in example 1 of the present invention.
Fig. 3 is a constant current charge and discharge curve diagram for the first three weeks of the sodium ion battery prepared in example 1 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments.
A method for improving the performance of a carbon-based negative electrode material of a sodium-ion battery comprises the following steps:
s1, pre-oxidizing the soft carbon precursor, treating the soft carbon precursor or the soft carbon precursor added with the oxidation catalyst at 200-350 ℃ for 0.5-5 hours in air atmosphere, wherein the soft carbon precursor has oxidation reaction with the oxidation catalyst and oxygen in the low-temperature treatment process, and the surface of the soft carbon precursor is provided with an oxygen-containing functional group;
specifically, the soft carbon precursor comprises any one of asphalt, petroleum coke and needle coke; wherein the petroleum coke is at least one of green coke and cooked coke; the needle coke is at least one of coal-based needle coke and petroleum-based needle coke; the asphalt comprises any one or the combination of at least two of coal asphalt, petroleum asphalt, coal tar, heavy oil in petroleum industry or heavy aromatic hydrocarbon;
specifically, the heavy aromatic hydrocarbon includes any one of naphthalene, acenaphthene, fluorene, phenanthrene, anthracene, methylnaphthalene, phenylpropafluorene, benzodibenzofuran, triphenylene, thiaphenanthrene, fluoranthene, 1, 2-benzanthracene, or a combination of at least two of them.
Specifically, the oxidation catalyst is at least one of sulfuric acid, nitric acid and hydrogen peroxide.
S2, mixing the pre-oxidized soft carbon precursor and the hard carbon precursor according to the mass ratio of 1 (1-0.02) to form a mixture material, and in the mixing process, performing a crosslinking reaction on the soft carbon precursor and the hard carbon precursor;
specifically, the hard carbon precursor comprises one or more of phenolic resin, polyacrylonitrile, lignin and cellulose.
S3, placing the obtained mixed material into a high-temperature carbonization furnace, heating to 1000-1600 ℃ at a heating rate of 3-5 ℃/min, heating the mixed material at a high temperature under an inert atmosphere for 2-9 hours to enable the mixed material to generate cracking and carbonization reactions, and forming disordered stacking of carbon layers in the process, wherein carbon with a large number of nano-scale micropores is arranged inside the carbon;
among them, the inert gas to be introduced is preferably argon gas.
And S4, cooling the high-temperature treatment product to room temperature to obtain an amorphous carbon material, namely the sodium ion battery carbon-based negative electrode material.
Specifically, the cooling may be natural cooling, and the sample is taken out of the tube furnace after the temperature of the sample is reduced to room temperature.
The prepared carbon-based negative electrode material of the sodium ion battery is irregular and blocky in macroscopic appearance, has macropores, mesopores or micropores in the interior, and has the microstructure characteristics of short-range order and long-range disorder.
In specific application, materials with different structures can be obtained by adjusting the proportion of the pre-oxidized soft carbon precursor material to the hard carbon precursor material. The yield of the carbon material can be improved by compounding the carbon material with a hard carbon precursor material; the carbon material with the best electrochemical performance can be obtained according to different requirements by adjusting the carbonization temperature and adjusting the disorder degree of the carbon material to be used as the cathode active material of the sodium-ion battery.
The sodium ion battery carbon-based negative electrode material prepared by the performance improvement method, a conductive additive and a binder are prepared into an electrode material of a battery.
Specifically, the conductive additive comprises one or more of carbon materials such as carbon black, acetylene black, vapor deposition carbon fiber, conductive graphite, carbon nanotubes, graphene, nitrogen-doped carbon and the like. The binder comprises one or more of sodium alginate, sodium carboxymethylcellulose, sodium polyacrylate, polyaniline, etc.
The sodium ion battery carbon-based negative electrode material prepared by the performance improvement method, the conductive additive and the binder are coated on the current collector to prepare the negative electrode plate of the sodium ion battery, and the negative electrode plate is applied to the sodium ion battery, so that the sodium ion battery has higher capacity and energy density, stable cycle performance and good safety performance. The sodium ion battery can meet various application scenes such as intelligent peak regulation of a power grid, renewable energy sources matched energy storage power stations and communication base stations.
In order to better understand the technical scheme provided by the invention, the following specific examples respectively illustrate the specific processes for preparing the sodium ion battery carbon-based negative electrode material based on the pre-oxidized soft carbon precursor and the hard carbon precursor provided by the above examples of the invention, and the method for assembling the sodium ion battery carbon-based negative electrode material in the sodium ion battery as the sodium ion battery negative electrode material and the battery characteristics thereof.
Example 1
A sodium ion battery carbon-based negative electrode material comprises the following specific preparation steps: firstly, pitch is pre-oxidized, 2.0g of pitch is placed in an alumina crucible, a sample is heated to 290 ℃ at the speed of 5 ℃/min in a tubular furnace continuously filled with high-purity air, the sample is kept warm for 3h, then heating is stopped, and the sample is naturally cooled to room temperature. And then, mixing the pitch subjected to the pre-oxidation treatment with lignin according to the weight ratio of 7: 3 in a 50mL agate ball milling tank with agate ball milling beads, wherein the ball material ratio is 2: 1, 10mL of water was added to the jar mill. The ball milling was suspended for 15min at a speed of 400rpm for 30min in a ball mill for a total of 4 h. After the ball milling was completed, the ball milling beads were separated by a sieve, and the resulting mixture was dried in an oven at 80 ℃. And (3) placing the dried mixture into a graphite crucible, and heating to 350 ℃ in a tubular furnace in an argon atmosphere at a heating rate of 5 ℃/min to ensure that the pre-oxidized asphalt and the lignin fully interact. And after the heat preservation is carried out for 2h, the temperature is continuously raised to 1400 ℃ at the temperature rising speed of 5 ℃/min, and the heat preservation is carried out for 2h, so that the carbon-based negative electrode material of the sodium-ion battery is obtained. The prepared sodium ion battery carbon-based negative electrode material is used as an active substance of a battery negative electrode material for preparing a sodium ion battery, and an electrochemical test is carried out.
Mixing the prepared carbon-based negative electrode material of the sodium-ion battery with acetylene black and sodium carboxymethyl cellulose as a binder according to the proportion of 90: 5: 5, adding a proper amount of water, grinding to form slurry, uniformly coating the uniformly ground slurry on a current collector copper foil, drying, and cutting into a circular pole piece with the diameter of 10 mm. And drying the negative pole piece at 120 ℃ for 10 hours under vacuum condition, and transferring the negative pole piece into a glove box for later use.
The cell assembly was carried out in a glove box under argon atmosphere, with sodium metal as the counter and reference electrode, and 1mol of NaPF6Volume ratio dissolved in 1L 48.5: 48.5: 3 ethylene carbonate, propylene carbonate and fluoroethylene carbonate solution are used as electrolyte to assemble the CR2032 button cell. The charge and discharge test was performed at a current density of C/10 using constant current charge and discharge conditions. The test was carried out under the conditions of a discharge cut-off voltage of 0V and a charge cut-off voltage of 2V.
The carbon-based negative electrode material of the sodium ion battery prepared in example 1 was detected, and the results are shown in fig. 1 to 3.
Fig. 1 is an SEM electron micrograph of the carbon-based negative electrode material of example 1, and it can be seen from fig. 1 that the prepared carbon-based negative electrode material exhibits a granular morphology, and the particle size of the carbon-based negative electrode material is between 1 μm and 3 μm.
FIG. 2 is a comparison of XRD curve of carbon-based anode material in example 1 and XRD curve of untreated directly high-temperature carbonized asphalt, and it can be seen from FIG. 2 that the method of the present invention can effectively inhibit graphitization during high-temperature treatment, so that the prepared carbon-based anode material presents an amorphous structure, d002＝0.378nm。
FIG. 3 is the charge-discharge curve of the button cell assembled by the carbon-based negative electrode material of example 1 in three weeks, and it can be seen from FIG. 3 that the reversible capacity of the negative electrode material of the sodium-ion battery is 324mAh g-1The first week coulombic efficiency was 89%.
Example 2
A carbon-based negative electrode material of a sodium-ion battery comprises: the electrochemical properties of lignin were shown in Table 1, except that the lignin was replaced with a phenolic resin, as in example 1.
Example 3
A carbon-based negative electrode material of a sodium-ion battery comprises: the electrochemical properties of lignin were shown in Table 1, with cellulose being replaced by lignin, otherwise as in example 1.
Example 4
A carbon-based negative electrode material of a sodium-ion battery comprises: the electrochemical properties of the asphalt were shown in Table 1, except that petroleum coke was used instead of the asphalt in example 1.
Example 5
A carbon-based negative electrode material of a sodium-ion battery comprises: the pitch was replaced with needle coke, otherwise the same as in example 1, and its electrochemical properties are shown in Table 1.
Example 6
A carbon-based negative electrode material of a sodium-ion battery comprises: the pre-oxidation step of 3h incubation at 290 ℃ in air was replaced by 9h incubation at 290 ℃ in air, otherwise the same as in example 1, with electrochemical properties as shown in Table 1.
Example 7
A sodium ion battery carbon-based negative electrode material: the carbonization process of maintaining the temperature at 1400 ℃ for 2h was replaced by maintaining the temperature at 1600 ℃ for 2h, and the electrochemical properties are shown in Table 1 in the same manner as in example 1.
TABLE 1 electrochemical Properties of examples 1-7
| Examples | Carbon yield (%) | First week coulombic efficiency (%) | Reversible specific capacity (mAhg)-1) |
| 1 | 66 | 86 | 254 |
| 2 | 64 | 87 | 246 |
| 3 | 60 | 86 | 236 |
| 4 | 76 | 85 | 224 |
| 5 | 74 | 84 | 235 |
| 6 | 56 | 82 | 261 |
| 7 | 59 | 92 | 239 |
As can be seen from table 1, the carbon-based anode material prepared in example 1 has more excellent electrochemical properties, and the carbon yield is relatively high.
The above embodiments are not intended to limit the present invention, and the present invention is not limited to the above examples, and those skilled in the art may make variations, modifications, additions or substitutions within the technical scope of the present invention.
Claims (10)
1. A performance improvement method of a sodium ion battery carbon-based negative electrode material is characterized by comprising the following steps: the performance improvement method comprises the following steps:
s1, pre-oxidizing the soft carbon precursor, and treating the soft carbon precursor or the soft carbon precursor added with the oxidation catalyst at 200-350 ℃ for 0.5-5 hours in air atmosphere;
s2, mixing the pre-oxidized soft carbon precursor and the hard carbon precursor according to the mass ratio of 1 (1-0.02) to form a mixture material, and in the mixing process, performing a cross-linking reaction on the soft carbon precursor and the hard carbon precursor;
s3, placing the obtained mixed material into a high-temperature carbonization furnace, and carrying out high-temperature treatment for 2-9 hours at 1000-1600 ℃ under inert atmosphere;
and S4, cooling the high-temperature treatment product to room temperature to obtain an amorphous carbon material, namely the sodium ion battery carbon-based negative electrode material.
2. The method for improving the performance of the carbon-based anode material of the sodium-ion battery as claimed in claim 1, wherein: the soft carbon precursor comprises any one of asphalt, petroleum coke and needle coke; the petroleum coke is at least one of green coke and cooked coke; the needle coke is at least one of coal-series needle coke and petroleum-series needle coke; the asphalt comprises any one or the combination of at least two of coal asphalt, petroleum asphalt, coal tar, petroleum industry heavy oil or heavy aromatic hydrocarbon; the oxidation catalyst is at least one of sulfuric acid, nitric acid and hydrogen peroxide.
3. The method for improving the performance of the carbon-based negative electrode material of the sodium-ion battery as claimed in claim 2, wherein: the heavy aromatic hydrocarbon comprises any one of naphthalene, acenaphthene, fluorene, phenanthrene, anthracene, methylnaphthalene, phenylfluorene, benzodibenzofuran, triphenylene, thiaphenanthrene, fluoranthene and 1, 2-benzanthracene or the combination of at least two of the above.
4. The method for improving the performance of the carbon-based anode material of the sodium-ion battery as claimed in claim 1, wherein: the hard carbon precursor comprises one or more of phenolic resin, polyacrylonitrile, lignin and cellulose.
5. The method for improving the performance of the carbon-based anode material of the sodium-ion battery as claimed in claim 1, wherein: the prepared carbon-based negative electrode material of the sodium ion battery is irregular and blocky in macroscopic appearance, has macropores, mesopores or micropores in the interior, and has the microstructure characteristics of short-range order and long-range disorder.
6. An electrode material, characterized in that: the electrode material comprises a conductive additive, a binder and the sodium ion battery carbon-based negative electrode material prepared by the performance improvement method of any one of claims 1 to 5.
7. The battery electrode material according to claim 6, characterized in that: the conductive additive comprises one or more of carbon black, acetylene black, vapor deposition carbon fiber, conductive graphite, carbon nano tube and graphene.
8. The battery electrode material according to claim 7, characterized in that: the binder comprises one or more of sodium alginate, sodium carboxymethylcellulose, sodium polyacrylate and polyaniline.
9. The negative pole piece of the sodium ion battery is characterized in that: the negative pole piece includes: a current collector, a conductive additive coated on the current collector, a binder and a sodium ion battery carbon-based negative electrode material prepared by the performance improvement method of any one of the claims 1 to 5.
10. A sodium ion battery, characterized by: the sodium ion battery comprises the negative electrode sheet of claim 9.
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| 锂离子电池硬碳负极材料的研究进展;李玉龙等;《材料导报》;20170525;第236-241页 * |
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