CN112349919A - Surface-coated natural spherical graphite and preparation method and application thereof - Google Patents
Surface-coated natural spherical graphite and preparation method and application thereof Download PDFInfo
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- H01M4/00—Electrodes
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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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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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention relates to a natural spherical graphite with surface coating treatment, a preparation method and application thereof. The natural spherical graphite with the surface coated has high specific surface area and high electrochemical performance, and is suitable for lithium ion battery cathode materials, fuel cell key electrode materials and the like. The natural graphite surface coating method has the characteristics of low cost, simplicity, practicability, no environmental pollution, large-scale industrial production and the like.
Description
Technical Field
The invention belongs to the technical field of fuel cells, and relates to natural spherical graphite with a surface coated and treated, a preparation method and application thereof.
Background
Energy is the most fundamental driving force for development and economic growth throughout the world, and is the basis on which humans rely for survival. Due to exhaustion of traditional fossil energy sources used in large quantities at present such as petroleum and coal and increase of energy requirements of human society, advanced energy conversion and storage technology is a difficult point for establishing a new energy production and supply system, and how to develop a green and sustainable new energy source in the future is a common problem facing the world at present. As more new energy sources, such as solar energy, wind energy, geothermal energy, biomass energy, etc., are developed and utilized, the demand and demand for new energy conversion and storage devices has also increased substantially. Fuel cells and lithium ion batteries are used as new energy conversion and storage devices respectively, so that the use cost is reduced, and the increase of the energy density is the starting point of research.
The cathode oxygen reduction reaction of the fuel cell has higher energy barrier, and needs a high-efficiency catalyst to reduce the reaction activation energy and improve the reaction rate. Currently, noble metal platinum-based catalysts are widely used in oxygen reduction reactions due to their high electrocatalytic activity, however, their high cost and limited reserves limit the commercial application of fuel cell technology. Therefore, it is of great significance to develop a non-platinum catalyst which is low in cost, high in activity and high in stability. For a lithium ion battery, the energy density depends on a negative electrode material to a great extent, natural graphite has the characteristics of high crystallinity, good conductivity, low price and the like, and is a wider negative electrode material in the application of the current lithium ion battery, but the theoretical capacity of the graphite is only 372 mA h/g, the compatibility of the graphite to an electrolyte is not good, and solvent molecules and lithium ions are commonly inserted into a graphite layer in the charge-discharge process to cause the expansion and the peeling of the graphite layer, so that the capacity and the service life of the battery are reduced. Therefore, the performance of the graphite cathode can be effectively improved by modifying and modifying the graphite material.
Chitosan is the only alkaline polysaccharide in the nature, and has the characteristics of wide source, low price and the like. A large number of amino groups and carboxyl groups exist in chitosan molecules, so that the chitosan molecules are relatively active in property, and chemical reactions are easy to occur when the groups act. The chitosan is uniformly coated on the surface of the natural spherical graphite in an acid system, and the natural graphite coated with the chitosan-derived carbon layer is prepared by hydrothermal carbonization and high-temperature ammonia activation. The natural graphite surface coating method has the characteristics of low cost, simplicity, practicability, no environmental pollution, large-scale production and the like. After surface modification treatment, the electrochemical activity of the natural spherical graphite is obviously improved, and the natural spherical graphite is suitable for being used as an electrode material of a fuel cell, a cathode material of a lithium ion battery and the like.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a natural spherical graphite with a surface coating treatment, and a preparation method and application thereof. The coating method has the characteristics of low cost, simple operation process, no environmental pollution, easy industrial production and the like. The electrochemical activity of the natural spherical graphite after surface modification treatment is obviously improved, and the natural spherical graphite is suitable for serving as a cathode catalyst of a fuel cell, a cathode material of a lithium ion battery and the like.
In order to realize the purpose of the invention, the invention adopts the following technical scheme: the surface of the natural spherical graphite is a carbon shell layer formed by chitosan, the inner core of the natural spherical graphite is the natural spherical graphite, and the natural spherical graphite and the inner core are tightly compounded to form a carbon-carbon composite material with a stable structure, so that the natural spherical graphite with the surface being coated is obtained.
In a preferred embodiment of the present invention, the natural spherical graphite has a particle size of 1 to 10 μm.
In a preferred embodiment of the present invention, the thickness of the carbon shell layer is 40 to 100 nm.
The invention also provides a preparation method of the natural spherical graphite with the surface coating treatment, which comprises the steps of taking the natural spherical graphite as a core layer material and chitosan as a shell layer coating substance, uniformly coating the chitosan on the surface of the spherical graphite, carbonizing the chitosan through hydrothermal treatment, and then activating at high temperature under ammonia gas to obtain a carbonized product, thus finally obtaining the natural spherical graphite with the surface modified. The natural graphite material after coating treatment has high electrochemical performance and is suitable for fuel cell key electrode materials and lithium ion battery cathode materials.
In a preferred embodiment of the present invention, chitosan is uniformly coated on the surface of the spherical graphite using a crosslinking agent.
In a preferred embodiment of the invention, the hydrothermal treatment is to perform hydrothermal reaction at 180-210 ℃, keep the temperature for 10-12 hours, take out and naturally cool to room temperature.
In a preferred embodiment of the invention, the high-temperature activation of the ammonia gas is carried out by heating to 800-1100 ℃ at a heating rate of 5 ℃/min in an ammonia gas atmosphere, keeping the temperature for 2-4 hours for activating the ammonia gas, cooling along with a furnace, and taking out.
More specifically, the preparation method comprises the following steps:
(1) preparing 0.2 mol/L acetic acid aqueous solution, adding spherical graphite into the acetic acid aqueous solution, and stirring until the spherical graphite and the acetic acid aqueous solution are uniformly mixed; adding chitosan, stirring to completely dissolve the chitosan, placing the mixture in ice water for continuous stirring, and respectively dropwise adding a cross-linking agent to cross-link the chitosan and the cross-linking agent;
(2) carrying out hydrothermal treatment on the reaction liquid prepared in the step (1) at the temperature of 180-210 ℃, preserving heat for 10-12 hours, taking out and naturally cooling to room temperature;
(3) carrying out suction filtration on the carbonized product obtained in the step (2), washing the carbonized product with deionized water until filtrate turns colorless, and then placing a sample obtained after washing in a vacuum oven to dry for 6-10 h at 70-100 ℃;
(4) and (4) putting the product obtained in the step (3) in a tubular furnace under the atmosphere of ammonia gas, raising the temperature to 800-1100 ℃ at the heating rate of 5 ℃/min, preserving the temperature for 2-4 hours at the temperature for activating the ammonia gas, cooling along with the furnace, and taking out the product to obtain the natural spherical graphite with the surface being coated.
In a preferred embodiment of the present invention, the mass ratio of the spherical graphite to the chitosan is 1: 10 to 20.
In a preferred embodiment of the invention, the crosslinking agent is formaldehyde; the mass-volume ratio of the chitosan to the cross-linking agent is 1000 mg: 1 ml.
The invention also protects the natural spherical graphite with the surface coated for preparing the catalyst material of the fuel cell and the cathode material of the lithium ion battery.
Compared with the prior art, the invention has the following beneficial effects:
1. the coating modified natural spherical graphite is prepared by taking chitosan and spherical graphite as precursors through hydrothermal carbonization and ammonia activation, and has high graphitization degree and high specific surface area.
2. The coated and modified natural spherical graphite has high oxygen reduction electrocatalytic activity and stability, and is obviously superior to commercial platinum carbon; as a negative electrode material of the lithium ion battery, the material has the reversible capacity and the excellent rate capability which are higher than those of untreated natural spherical graphite.
3. The natural spherical graphite with the surface coated is suitable for lithium ion battery cathode materials, fuel cell key electrode materials and the like; the natural spherical graphite and the chitosan have wide sources, low price and environmental protection; the natural graphite surface coating method has the characteristics of low cost, simplicity, practicability, no environmental pollution, large-scale industrial production and the like.
Drawings
The invention will be further described with reference to the accompanying drawings, which are only schematic illustrations and illustrations of the invention, and do not limit the scope of the invention.
FIG. 1 is a view illustrating the micro-morphology of the original natural Spheroidal Graphite (SG) in the examples;
FIG. 2 is a graph illustrating the coated spheroidal graphite microstructure prepared in example 1;
FIG. 3 is a SEM image illustrating the coated spheroidal graphite microstructure prepared in example 2;
FIG. 4 is a graph illustrating the coated spheroidal graphite microtopography (TEM image) prepared in example 2;
FIG. 5 is a graph illustrating the coated spheroidal graphite microstructure prepared in example 3;
FIG. 6 is a XRD pattern for coated spheroidal graphites prepared in examples 1-3;
FIG. 7 is a graph illustrating the polarization curves of the coated spheroidal graphite prepared in example 2 and a 20% commercial Pt/C catalyst in an oxygen saturated 1M NaOH solution. Voltage range of 0.1 to-0.8V (vs SCE), scanning speed of 5 mv/s, and electrode rotation speed of 1600 rpm;
FIG. 8 is a graph showing the half-wave potential of the coated spheroidal graphite (C @ C-20) prepared in example 2 and a 20% commercial Pt/C catalyst in an oxygen saturated 1M NaOH solution. Voltage range of 0.1 to-0.8V (vs SCE), scanning speed of 5 mv/s, and electrode rotation speed of 1600 rpm;
FIG. 9 is a graph illustrating the first three charge-discharge curves for the coated spheroidal graphite prepared in example 2, with a current density of 0.1A/g;
FIG. 10 is a graph showing the rate capability of the coated spheroidal graphite prepared in example 2, wherein the current density is 0.1A/g to 10A/g, and the charge and discharge cycles are performed 10 times at each current density.
Detailed Description
The invention will be further described with reference to the following description and examples in conjunction with the accompanying drawings:
example 1
(1) Firstly, preparing 0.2 mol/L acetic acid aqueous solution, and respectively taking 30 ml of the acetic acid aqueous solution and placing the acetic acid aqueous solution in a plurality of beakers; weighing 30 mg of spherical graphite, adding the spherical graphite into an acetic acid solution, and stirring until the spherical graphite and the acetic acid solution are uniformly mixed; adding 300 mg chitosan, stirring for 30 min to completely dissolve chitosan; placing the beaker in ice water for continuous stirring, and respectively dropwise adding 0.3 ml of formaldehyde (AR) and chitosan for crosslinking;
(2) transferring the liquid prepared in the step (1) into a tetrafluoro inner container of a 50ml reaction kettle, carrying out hydrothermal reaction at 180 ℃, keeping the temperature for 12 hours, taking out, and naturally cooling to room temperature;
(3) carrying out suction filtration on the pre-carbonized product obtained in the step (2), washing the pre-carbonized product with deionized water until filtrate turns colorless, and then placing a sample obtained after washing in a vacuum oven to dry for 10 hours at 80 ℃;
(4) and (4) putting the product obtained in the step (3) in a tubular furnace under the atmosphere of ammonia gas, raising the temperature to 900 ℃ at the heating rate of 5 ℃/min, preserving the temperature for 2 hours at the temperature for activating the ammonia gas, cooling along with the furnace, and taking out the product to obtain the carbon material with the C @ C-10 core-shell structure.
Example 2
(1) Firstly, preparing 0.2 mol/L acetic acid aqueous solution, and respectively taking 30 ml of the acetic acid aqueous solution and placing the acetic acid aqueous solution in a plurality of beakers; weighing 30 mg of spherical graphite, adding the spherical graphite into an acetic acid solution, and stirring until the spherical graphite and the acetic acid solution are uniformly mixed; adding 600 mg chitosan, stirring for 30 min to dissolve chitosan completely; placing the beaker in ice water for continuous stirring, and respectively dropwise adding 0.6 ml of formaldehyde (AR) and chitosan for crosslinking;
(2) transferring the liquid prepared in the step (1) into a tetrafluoro inner container of a 50ml reaction kettle, carrying out hydrothermal reaction at 180 ℃, keeping the temperature for 12 hours, taking out, and naturally cooling to room temperature;
(3) carrying out suction filtration on the pre-carbonized product obtained in the step (2), washing the pre-carbonized product with deionized water until filtrate turns colorless, and then placing a sample obtained after washing in a vacuum oven to dry for 10 hours at 80 ℃;
(4) and (4) putting the product obtained in the step (3) in a tubular furnace under the atmosphere of ammonia gas, raising the temperature to 900 ℃ at the heating rate of 5 ℃/min, preserving the temperature for 2 hours at the temperature for activating the ammonia gas, cooling along with the furnace, and taking out the product to obtain the carbon material with the C @ C-20 core-shell structure.
Example 3
(1) Firstly, preparing 0.2 mol/L acetic acid aqueous solution, and respectively taking 30 ml of the acetic acid aqueous solution and placing the acetic acid aqueous solution in a plurality of beakers; weighing 30 mg of spherical graphite, adding the spherical graphite into an acetic acid solution, and stirring until the spherical graphite and the acetic acid solution are uniformly mixed; adding 900 mg chitosan, stirring for 30 min to dissolve chitosan completely; placing the beaker in ice water for continuous stirring, and respectively dropwise adding 0.9 ml of formaldehyde (AR) and chitosan for crosslinking;
(2) transferring the liquid prepared in the step (1) into a tetrafluoro inner container of a 50ml reaction kettle, carrying out hydrothermal reaction at 180 ℃, keeping the temperature for 12 hours, taking out, and naturally cooling to room temperature;
(3) carrying out suction filtration on the pre-carbonized product obtained in the step (2), washing the pre-carbonized product with deionized water until filtrate turns colorless, and then placing a sample obtained after washing in a vacuum oven to dry for 10 hours at 80 ℃;
(4) and (4) putting the product obtained in the step (3) in a tubular furnace under the atmosphere of ammonia gas, raising the temperature to 900 ℃ at the heating rate of 5 ℃/min, preserving the temperature for 2 hours at the temperature for activating the ammonia gas, cooling along with the furnace, and taking out the product to obtain the C @ C-30 core-shell structure carbon material.
SEM images of the coated spheroidal graphite are shown in fig. 1-4. It can be seen that the surface of the carbon shell formed by chitosan is rough, and the spherical graphite is successfully coated by chitosan. The TEM image (FIG. 5) can obtain C @ C-20 with the particle size of 6-8 um and the shell thickness of 40-100 nm. As can be seen from the XRD pattern (fig. 6), as the mass ratio of chitosan to graphite spherulites increases, the crystallinity of the material decreases. As can be seen from the polarization curve (FIG. 7), the C @ C-20 core-shell structure carbon material has catalytic activity superior to that of commercial platinum carbon. FIG. 8 shows that the half-wave potential of C @ C-20 is 40 mV higher than commercial platinum carbon. The first three-time charge-discharge curve (figure 9) shows that the graphite has the theoretical capacity higher than that of spherical graphite, and the first charge specific capacity is 621.7 mAh/g. From FIG. 10, it is found that when the current returns to 0.1A/g, the capacity is still maintained at 375.9 mAh/g, indicating good rate capability.
It should be understood that although the present description has been described in terms of various embodiments, not every embodiment includes only a single embodiment, and such description is for clarity purposes only, and those skilled in the art will recognize that the embodiments described herein may be combined as suitable to form other embodiments, as will be appreciated by those skilled in the art.
The above list of details is only a concrete description of the feasible examples of the present invention and they are not intended to limit the scope of the present invention, and all equivalent embodiments or modifications such as combinations, divisions or repetitions of the features, which do not depart from the concept and technical solution of the present invention, should be included in the scope of the present invention.
Claims (10)
1. The surface-coated natural spherical graphite is characterized in that the surface of the natural spherical graphite is a carbon shell layer formed by chitosan, the inner core of the natural spherical graphite is natural spherical graphite, and the natural spherical graphite and the inner core are tightly compounded to form a carbon-carbon composite material with a stable structure, so that the surface-coated natural spherical graphite is obtained.
2. The surface-coated natural spherical graphite according to claim 1, wherein the natural spherical graphite has a particle size of 1 to 10 μm.
3. The surface-coated natural spherical graphite according to claim 1, wherein the thickness of the carbon shell layer is 40 to 100 nm.
4. The method for preparing surface-coated natural spherical graphite according to any one of claims 1 to 3, wherein the surface-modified natural spherical graphite is obtained by uniformly coating the surface of the spherical graphite with the natural spherical graphite as a core material and chitosan as a shell-coated substance, then carbonizing the chitosan through hydrothermal treatment, and then activating at high temperature under ammonia gas to obtain a carbonized product.
5. The method according to claim 4, wherein the surface of the spherical graphite is uniformly coated with chitosan using a crosslinking agent.
6. The preparation method according to claim 4, wherein the hydrothermal treatment is a hydrothermal reaction at 180-210 ℃, and the hydrothermal reaction is carried out after heat preservation for 10-12 hours, and then the mixture is taken out and naturally cooled to room temperature.
7. The preparation method according to claim 4, characterized in that the high-temperature activation under ammonia gas is carried out by heating to 800-1100 ℃ at a heating rate of 5 ℃/min under an ammonia gas atmosphere, keeping the temperature for 2-4 hours for ammonia gas activation, cooling along with a furnace, and taking out.
8. The method according to any one of claims 4 to 7, characterized by the following steps:
(1) preparing 0.2 mol/L acetic acid aqueous solution, adding spherical graphite into the acetic acid aqueous solution, and stirring until the spherical graphite and the acetic acid aqueous solution are uniformly mixed; adding chitosan, stirring to completely dissolve the chitosan, placing the mixture in ice water for continuous stirring, and respectively dropwise adding a cross-linking agent to cross-link the chitosan and the cross-linking agent;
(2) carrying out hydrothermal treatment on the reaction liquid prepared in the step (1) at the temperature of 180-210 ℃, preserving heat for 10-12 hours, taking out and naturally cooling to room temperature;
(3) carrying out suction filtration on the carbonized product obtained in the step (2), washing the carbonized product with deionized water until filtrate turns colorless, and then placing a sample obtained after washing in a vacuum oven to dry for 6-10 h at 70-100 ℃;
(4) and (4) putting the product obtained in the step (3) in a tubular furnace under the atmosphere of ammonia gas, raising the temperature to 800-1100 ℃ at the heating rate of 5 ℃/min, preserving the temperature for 2-4 hours at the temperature for activating the ammonia gas, cooling along with the furnace, and taking out the product to obtain the natural spherical graphite with the surface being coated.
9. The preparation method according to claim 8, wherein the mass ratio of the spherical graphite to the chitosan is 1: 10-20; the cross-linking agent is formaldehyde; the mass-volume ratio of the chitosan to the cross-linking agent is 1000 mg: 1 ml.
10. The surface-coated natural spherical graphite according to any one of claims 1 to 3 and the surface-coated natural spherical graphite prepared by the preparation method according to claims 4 to 9 are used for preparing fuel cell catalyst materials and anode materials of lithium ion batteries.
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| CN114538569A (en) * | 2022-02-25 | 2022-05-27 | 中国科学技术大学 | Fe coated with chitosan-derived carbon shell0/FeOxGranular electro-Fenton cathode and preparation and application thereof |
| CN117199249A (en) * | 2023-11-08 | 2023-12-08 | 深圳海辰储能科技有限公司 | Negative plate, energy storage device and electric equipment |
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| CN1567617A (en) * | 2003-06-20 | 2005-01-19 | 比亚迪股份有限公司 | Method for preparing a carbon cathode material of lithium ion battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114538569A (en) * | 2022-02-25 | 2022-05-27 | 中国科学技术大学 | Fe coated with chitosan-derived carbon shell0/FeOxGranular electro-Fenton cathode and preparation and application thereof |
| CN114538569B (en) * | 2022-02-25 | 2023-03-10 | 中国科学技术大学 | Fe coated with chitosan-derived carbon shell 0 /FeO X Granular electro-Fenton cathode and preparation and application thereof |
| CN117199249A (en) * | 2023-11-08 | 2023-12-08 | 深圳海辰储能科技有限公司 | Negative plate, energy storage device and electric equipment |
| CN117199249B (en) * | 2023-11-08 | 2024-03-08 | 深圳海辰储能科技有限公司 | Negative plate, energy storage device and electric equipment |
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