CN108987719B - Three-dimensional sulfur-doped porous carbon/tin dioxide composite electrode material and preparation method thereof - Google Patents
Three-dimensional sulfur-doped porous carbon/tin dioxide composite electrode material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a three-dimensional sulfur-doped porous carbon/tin dioxide composite electrode material and a preparation method thereof, and relates to the field of batteries, wherein the preparation method comprises the following steps: (1) preparing the three-dimensional sulfur-doped porous carbon. (2) Mixing sulfur-doped porous carbon with tin chloride in a mass ratio of 1: 0.2-5, mixing and dissolving, carrying out ultrasonic assistance for 0.5-2h, transferring the mixed solution into a reaction kettle, and carrying out heat preservation for 1-10 h at 150-220 ℃ by a solvothermal method to obtain the composite electrode material with the mass ratio of tin dioxide of 5-60%. The three-dimensional sulfur-doped porous carbon/tin dioxide composite electrode material prepared by the method has the advantages that the specific capacitance, the power density, the energy density, the rate capability, the cycling stability and other properties are greatly improved and enhanced, compared with the existing electrode material, the method is simple and easy to operate, and can be used as a new energy electric vehicle battery pack electrode material to promote the development of new energy automobiles.
Description
Technical Field
The invention relates to the field of batteries, in particular to a three-dimensional sulfur-doped porous carbon/tin dioxide composite electrode material and a preparation method thereof.
Background
The lithium ion battery as a novel rechargeable power supply has the advantages of high working voltage, high energy density, low self-discharge rate, safety, no pollution and the like, and is widely applied to portable electronic equipment such as mobile phones, notebook computers and the like. At present, the commercial lithium ion battery negative electrode material is mainly a graphite/carbon material and has high conductivity, but the theoretical specific capacity is low, the rate capability is poor, and the application of the lithium ion battery negative electrode material in the next generation of lithium ion batteries is restricted. The metal oxide has higher theoretical specific capacity, but the metal oxide has poor conductivity and is easy to agglomerate in the reaction process, so that the circulation stability is poor, and the capacity retention rate is low.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a three-dimensional sulfur-doped porous carbon/tin dioxide composite electrode material and a preparation method thereof.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
in a first aspect, the invention provides a preparation method of a three-dimensional sulfur-doped porous carbon/tin dioxide composite electrode material, which comprises the following steps:
mixing sulfur-doped porous carbon and tin dichloride in a mass ratio of 1: 0.2-5, mixing and dissolving, and preserving heat for 1-10 hours at 150-220 ℃ by adopting a solvothermal method.
Further, in a preferred embodiment of the present invention, the temperature rising rate is 1-5 ℃/min in the solvothermal process.
Further, in a preferred embodiment of the present invention, the doping amount of the sulfur atom in the sulfur-doped porous carbon is 1 to 30%.
Further, in a preferred embodiment of the present invention, the sulfur-doped porous carbon is prepared by mixing a carbon source and a sulfate, and carbonizing at 450 to 800 ℃ for 0.5 to 3 hours under an inert atmosphere.
Further, in a preferred embodiment of the present invention, the mass ratio of the carbon source to the sulfate is 1: 0.5 to 6.
Further, in a preferred embodiment of the present invention, the carbon source is at least one selected from the group consisting of slurry oil, pitch, sucrose, glucose, cellulose and starch. Further, in a preferred embodiment of the present invention, the sulfur source is at least one selected from the group consisting of magnesium sulfate, sodium sulfate, aluminum sulfate, sodium bisulfate, calcium sulfate and zinc sulfate. Further, in a preferred embodiment of the present invention, the temperature increase rate in the process of preparing the sulfur-doped porous carbon is 2 to 10 ℃/min.
Further, in a preferred embodiment of the present invention, after the carbonization under the condition of heat preservation, the method further comprises the steps of acid washing and water washing of the obtained carbonized product.
In a second aspect, the invention provides the three-dimensional sulfur-doped porous carbon/tin dioxide composite electrode material prepared by the preparation method, wherein the percentage content of sulfur atoms is 1-30%, the lithium ion storage capacity is 1000-3000mAh/g, and the energy density is 150-350 wh/kg. Compared with the prior art, the beneficial effects of the invention comprise:
according to the preparation method of the three-dimensional sulfur-doped porous carbon/tin dioxide composite electrode material, sulfur-doped carbon is used as a carrier, and transition metal tin is introduced into interlayers and pore channels of carbon nano-particles by a solvothermal method so as to be uniformly and tightly combined with the carbon carrier, so that a sulfur-doped carbon/tin dioxide nano-composite body is obtained and can be used as an electrode material. By optimizing each reaction parameter in the preparation method, the shape, size and dispersity of the tin dioxide are effectively regulated and controlled, so that the synergistic effect of the sulfur-doped carbon and the tin dioxide is further exerted.
The inventor researches and discovers that the sulfur atom doping can significantly influence the chemical environment of the carbon structure, including the surface polarity and the electronic state, compared with undoped carbon, thereby promoting the electrochemical process of carbon base, enhancing the electrochemical performance and improving the storage capacity of lithium ions.
Compared with the existing electrode material, the three-dimensional sulfur-doped porous carbon/tin dioxide composite electrode material prepared by the method has the advantages that the specific capacitance, the power density, the energy density, the rate capability, the cycling stability and other properties are greatly improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
Fig. 1 is a transmission electron micrograph of the three-dimensional sulfur-doped porous carbon provided in example 1.
Fig. 2 is a transmission electron micrograph of the three-dimensional sulfur-doped porous carbon/tin dioxide provided in example 2.
Fig. 3 is a transmission electron micrograph of the three-dimensional sulfur-doped porous carbon/tin dioxide provided in example 3.
Fig. 4 is an X-ray photoelectron spectrum of the three-dimensional sulfur-doped porous carbon/tin dioxide composite material provided in example 3.
Fig. 5 is a transmission electron micrograph of the three-dimensional sulfur-doped porous carbon/tin dioxide provided in example 4.
Fig. 6 is a graph of the rate performance of the three-dimensional sulfur-doped porous carbon/tin dioxide provided in example 4.
Fig. 7 is a charge-discharge curve diagram of the three-dimensional sulfur-doped porous carbon/tin dioxide composite electrode material provided in example 4.
Fig. 8 is a graph of power density versus energy density for the three-dimensional sulfur-doped porous carbon/tin dioxide composite electrode material of example 4.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The embodiment provides a three-dimensional sulfur-doped porous carbon/tin dioxide composite electrode material, and the preparation method comprises the following steps:
mixing sulfur-doped porous carbon and tin dichloride in a mass ratio of 1: 0.2-5, mixing and dissolving, and preserving heat for 1-10 hours at 150-220 ℃ by adopting a solvothermal method.
Further, in the process of adopting the solvothermal method, the temperature rise rate is 1-5 ℃/min, or 1.5-2.5 ℃/min, or 1.8-2.2 ℃/min.
Wherein the doping amount of sulfur atoms in the sulfur-doped porous carbon is 0.1-30%, or 3-22%, or 5-20%, or 7-18%, or 9-16%, or 11-14%.
The preparation method of the sulfur-doped porous carbon comprises the following steps:
mixing a carbon source and sulfate, and carrying out heat preservation and carbonization for 0.5-3 h at 450-800 ℃ under inert gas to obtain the carbon source.
By the method, the sulfur-doped carbon can be controllably prepared, the doping modification of the carbon material is realized, the electron hole of the carbon material is effectively adjusted, the energy gap is widened, and more topological defects are induced to be generated, so that the sulfur-doped carbon has more excellent electrochemical performance on a lower voltage platform.
In the method, the carbon source is oil slurry, asphalt, cane sugar, glucose, cellulose and starch; the sulfate is used as a sulfur source and a template precursor, and includes but is not limited to magnesium sulfate, sodium sulfate, aluminum sulfate, sodium bisulfate, calcium sulfate and zinc sulfate, and preferably, the template is magnesium sulfate.
Preferably, the mass ratio of the carbon source to the sulfate is 1: 0.5-6, or 1: 0.7 to 5; or 1: 0.8 to 4; or 1: 0.9 to 3; or 1: 1.1.
preferably, the preparation method of the sulfur-doped porous carbon further comprises the following steps: and (3) carrying out acid washing and water washing on the obtained carbonized product to remove the template agent so as to obtain pure sulfur-doped porous carbon. More preferably, citric acid solution is used for pickling.
Preferably, the heating rate in the process of preparing the sulfur-doped porous carbon is 2-10 ℃/min, or 3-8 ℃/min, or 5-7 ℃/min. The temperature programming is adopted, and the temperature programming is strictly controlled, so that the carbonized substrate is slowly carbonized in the heating process, and the performance of sulfur-doped carbon is further improved.
The features and properties of the present invention are further described in detail below with reference to examples:
example 1
The embodiment provides a three-dimensional sulfur-doped porous carbon material, and a preparation method thereof comprises the following steps:
mixing the oil slurry with magnesium sulfate in a mass ratio of 1: 3, uniformly mixing and stirring, transferring the mixture into a horizontal tube furnace, introducing argon as protective atmosphere, heating to 700 ℃ at the heating rate of 5 ℃/min, and preserving heat for 1h to obtain the three-dimensional sulfur-doped porous carbon material, wherein a transmission electron microscope photo of the three-dimensional sulfur-doped porous carbon material is shown in figure 1. The method does not need a template precursor, obtains the three-dimensional sulfur-doped porous carbon material containing the porous structure by a one-step method, and is simple.
Example 2
The embodiment provides a three-dimensional sulfur-doped porous carbon/tin dioxide composite electrode material, and the preparation method comprises the following steps:
mixing the sulfur-doped porous carbon prepared in example 1 and tin dichloride in a mass ratio of 1: 1 mixing and dissolving in water, transferring the solution to a high-pressure reaction kettle, putting the high-pressure reaction kettle into an oven, heating the oven to 150 ℃ at the heating rate of 1 ℃/min, and preserving the heat for 10 hours.
And after cooling to room temperature, washing and drying to obtain the three-dimensional sulfur-doped porous carbon/tin dioxide composite material. The three-dimensional sulfur-doped porous carbon/tin dioxide composite material obtained by the method has the particle size of 3-5 nm, the loading amount of 45% and uniform distribution, and a transmission electron microscope image is shown in fig. 2.
Example 3
The embodiment provides a three-dimensional sulfur-doped porous carbon/tin dioxide composite electrode material, and the preparation method comprises the following steps:
A. mixing sucrose and magnesium sulfate, heating to 450 ℃ at a heating rate of 2 ℃/min under inert gas, preserving heat, carbonizing for 0.5h, washing with citric acid solution, and washing with water to obtain the sulfur-doped porous carbon.
B. Mixing sulfur-doped porous carbon and tin dichloride in a mass ratio of 1: 5 mixing and dissolving the mixture in water, transferring the solution to a high-pressure reaction kettle, putting the high-pressure reaction kettle into an oven, heating the oven to 220 ℃ at the heating rate of 5 ℃/min, and keeping the temperature for 1 h.
C. And after cooling to room temperature, washing and drying to obtain the three-dimensional sulfur-doped porous carbon/tin dioxide composite material.
The three-dimensional sulfur-doped porous carbon/carbon alloy provided in this exampleThe transmission electron microscope image of the tin oxide composite electrode material is shown in fig. 3, and it can be clearly seen from the image that tin dioxide nanoparticles are uniformly dispersed on the surface and in the pore channels of the sulfur-doped porous carbon. The mass percentage of the loaded quantity of the tin dioxide is 85 percent. Fig. 4 is a corresponding X-ray photoelectron spectrum, from which it can be seen that the S content is 8.1% and the Sn content is 15.4% by atomic ratio. It was confirmed that S was bonded to the carbon material in the form of a chemical bond, SnO2Successfully compounded into the pore canal and the surface of the porous carbon.
Example 4
The embodiment provides a three-dimensional sulfur-doped porous carbon/tin dioxide composite electrode material, and the preparation method comprises the following steps:
A. mixing sucrose and magnesium sulfate, heating to 600 ℃ at a heating rate of 2 ℃/min under inert gas, preserving heat, carbonizing for 2h, washing with citric acid solution, and washing with water to obtain the sulfur-doped porous carbon.
B. Mixing sulfur-doped porous carbon and tin dichloride in a mass ratio of 1: 2 mixing and dissolving in water, transferring the solution to a high-pressure reaction kettle, putting the high-pressure reaction kettle into an oven, heating the oven to 200 ℃ at the heating rate of 2 ℃/min, and keeping the temperature for 5 hours.
C. And after cooling to room temperature, washing and drying to obtain the three-dimensional sulfur-doped porous carbon/tin dioxide composite material.
A transmission electron microscope image of the three-dimensional sulfur-doped porous carbon/tin dioxide composite electrode material provided in this embodiment is shown in fig. 5, from which it can be clearly seen that tin dioxide nanoparticles are uniformly dispersed on the surface and in the pore channels of the sulfur-doped porous carbon. The mass percentage of the loaded quantity of the tin dioxide is 65 percent.
The sulfur-doped porous carbon/tin dioxide composite electrode material prepared by the method has high lithium storage capacity, and a multiplying power performance diagram is shown in fig. 6. The capacity of the sulfur-doped porous carbon/tin dioxide composite electrode material is 1490mAh/g when the current density is 200mA/g, and the capacity can still be maintained to be 800mAh/g when the current density is 1600 mA/g. The lithium storage capacity of the sulfur-doped porous carbon is 1305mAh/g when the current density is 200mA/g, and the capacity can still be maintained to be 580mAh/g when the current density is 1600 mA/g. As can be seen from fig. 6, the sulfur-doped porous carbon/tin dioxide composite electrode material has a higher lithium storage capacity and excellent electrochemical properties.
The charge-discharge curve chart of the sulfur-doped porous carbon/tin dioxide composite electrode material is shown in fig. 7, and the graph shows that the material has better cycle performance.
The power density-energy density curve diagram of the sulfur-doped porous carbon/tin dioxide composite electrode material is shown in fig. 8, and it can be known from the graph that the energy density can reach 341Wh/Kg at a current density of 0.2C, and the sulfur-doped porous carbon/tin dioxide composite electrode material has higher energy density and power density. The novel energy battery can be applied to new energy electric vehicles, and a road is developed for the development of new energy power batteries.
While particular embodiments of the present invention have been illustrated and described, it would be obvious that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.
Claims (7)
1. A preparation method of a three-dimensional sulfur-doped porous carbon/tin dioxide composite electrode material is characterized by comprising the following steps:
mixing sulfur-doped porous carbon and tin dichloride in a mass ratio of 1: 0.2-5, mixing and dissolving, and preserving heat for 1-10 hours at 150-220 ℃ by adopting a solvothermal method;
in the process of adopting the solvothermal method, the heating rate is 1-5 ℃/min, and the mass fraction of sulfur atoms in the sulfur-doped porous carbon is 1-30%;
the sulfur-doped porous carbon is prepared by mixing a carbon source and a sulfur source, and carrying out heat preservation and carbonization for 0.5-3 h at 450-800 ℃ under inert gas.
2. The preparation method of the three-dimensional sulfur-doped porous carbon/tin dioxide composite electrode material according to claim 1, wherein the mass ratio of the carbon source to the sulfur source is 1: 0.5 to 6.
3. The method for preparing the three-dimensional sulfur-doped porous carbon/tin dioxide composite electrode material according to claim 2, wherein the carbon source is at least one selected from oil slurry, asphalt, sucrose, glucose, cellulose and starch.
4. The method for preparing the three-dimensional sulfur-doped porous carbon/tin dioxide composite electrode material according to claim 2, wherein the sulfur source is selected from at least one of magnesium sulfate, sodium sulfate, aluminum sulfate, sodium bisulfate, calcium sulfate and zinc sulfate.
5. The preparation method of the three-dimensional sulfur-doped porous carbon/tin dioxide composite electrode material according to claim 1, wherein the temperature rise rate in the process of preparing the sulfur-doped porous carbon is 2-10 ℃/min.
6. The preparation method of the three-dimensional sulfur-doped porous carbon/tin dioxide composite electrode material according to claim 1, further comprising the steps of acid washing and water washing of the obtained carbonized product after the heat preservation carbonization.
7. The three-dimensional sulfur-doped porous carbon/tin dioxide composite electrode material prepared by the preparation method disclosed by any one of claims 1-6 is characterized in that the mass fraction of sulfur atoms is 1-30%, the lithium ion storage capacity is 1000-3000mAh/g, and the energy density is 150-350 wh/kg.
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| CN103730638A (en) * | 2013-10-12 | 2014-04-16 | 吉林大学 | Preparation method of nitrogen-doped carbon material |
| CN107887586A (en) * | 2017-11-06 | 2018-04-06 | 陈少华 | A kind of preparation method of ion cathode material lithium |
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| CN103730638A (en) * | 2013-10-12 | 2014-04-16 | 吉林大学 | Preparation method of nitrogen-doped carbon material |
| CN107887586A (en) * | 2017-11-06 | 2018-04-06 | 陈少华 | A kind of preparation method of ion cathode material lithium |
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Effective date of registration: 20220325 Address after: 224007 No. 2, South hope Avenue, Yancheng Economic and Technological Development Zone, Jiangsu Province Patentee after: YANCHENG TEACHERS University Address before: 1 / F and 2 / F, R & D building 2, new energy vehicles and auto parts Industrial Park, No. 69, East Ring Road, Yancheng Economic and Technological Development Zone, Yancheng City, Jiangsu Province, 224000 Patentee before: YANCHENG RESEARCH CENTER OF NEW ENERGY ON CHEMICAL STORAGE & POWER SOURCES |