CN115108556A - Silicon-carbon composite material and preparation method thereof - Google Patents
Silicon-carbon composite material and preparation method thereof Download PDFInfo
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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
- H01M10/00—Secondary cells; Manufacture thereof
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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- H—ELECTRICITY
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
Abstract
The invention discloses a silicon-carbon composite material and a preparation method thereof, wherein the preparation method of the silicon-carbon composite material comprises the following steps: performing ball-milling reaction on a silicon source and a carbon source to obtain the silicon-carbon composite material, wherein the silicon source is a silicon alloy, and the carbon source is chlorobenzene, bromobenzene or iodobenzene. The industrial ball milling process adopted by the preparation method promotes the reaction to be rapidly carried out, has high efficiency, is easy to realize uniform compounding and can be amplified; meanwhile, through chemical design, theoretically, no tail gas is discharged, tail gas treatment is not needed, the requirements on production environment and environmental protection pressure are low, and industrial popularization is facilitated.
Description
Technical Field
The invention belongs to the technical field of silicon-carbon composite materials, and particularly relates to a silicon-carbon composite material and a preparation method thereof.
Background
The mobile power supply is the basis of the development of industries such as mobile communication, electric vehicles and the like. Lithium batteries are the most widely used mobile power sources at present. The energy storage of lithium batteries is based on a rocking chair type process of lithium ions between positive and negative electrodes. The lithium ion storage capacity, stability and migration rate of the positive and negative electrodes are the key factors for determining the performance of the lithium battery. Therefore, improving the lithium storage capacity and stability of the electrode is one of the keys for improving the performance. The negative electrode material of the lithium battery mainly takes graphite, and the theoretical capacity is 372 mAh/g. Decades of research shows that the practical utilization capacity of the graphite cathode approaches the theoretical ceiling. Therefore, the development of new anode materials is the key point for further improving the energy density of the battery. As a carbon family material, silicon has extremely high lithium storage capacity, and the theoretical specific capacity is up to 4200 mAh/g.
Unlike the energy storage process of intercalation/deintercalation of lithium ion layers of graphite, silicon lithium storage generally has an alloying reaction with lithium to form a silicon lithium alloy, and a serious volume effect can be generated in the lithium storage process, namely, the volume change is large, so that electrodes are pulverized and separated from the electrodes, new interfaces are easily formed, an SEI (solid electrolyte interphase) film is formed, lithium is consumed, and the electrode performance is rapidly attenuated and the cycling stability is poor. And silicon is not conductive by itself, which is also a disadvantage as an electrode material.
Different strategies have been proposed to address the above problems. The main strategy is nanocrystallization, and the volume effect of the silicon material in the charging and discharging process is reduced by nanocrystallization of silicon, so that electrode pulverization and cracking are avoided. Meanwhile, in order to further buffer the volume effect of the silicon cathode material, pore-forming has also proved effective. By designing the silicon material with the porous structure and utilizing the developed pore structure of the silicon material, the volume effect is buffered so as to reduce the influence on the overall structure of the cathode. In order to solve the problem of poor conductivity of silicon, the major technical route for developing silicon cathode materials is to compound carbon.
The silicon-carbon composite is mainly to coat the surface of silicon by a carbon layer. In application, the high-capacity lithium battery cathode is designed and prepared by combining the silicon-carbon cathode material and the graphite cathode through optimizing matching parameters such as content, granularity and the like, and a binder, an electrolyte, an assembly process and the like. At present, only a few reports about the realization of commercial application of the silicon-carbon anode material are reported and are still in the introduction stage. The development of the silicon-carbon composite battery negative electrode material is a hot spot of the application research of the current lithium battery material. At present, silicon-carbon preparation mainly adopts two steps including nano-silicon preparation and carbon coating. The preparation process is complex, the flow is long, the cost is high, and the industrial popularization is not facilitated.
Disclosure of Invention
The invention aims to provide a preparation method of a silicon-carbon composite material, which uses silicon alloy as a silicon source and chlorobenzene, bromobenzene or iodobenzene as a carbon source, and promotes halogen group-X (-Cl, -Br, -I) in the carbon source to react with cations in the silicon alloy by high-temperature ball milling or plasma ball milling to obtain the silicon-carbon composite material and a byproduct Y (salt formed by the cations in the silicon alloy and halogen in the carbon source) so as to obtain the high-performance lithium ion battery silicon-carbon cathode material.
The chlorobenzene, the bromobenzene and the iodobenzene have benzene ring structures, so that the pyrolytic carbon has good electrical properties, and is beneficial to obtaining a silicon-carbon composite structure and improving the corresponding battery performance. The heating ball milling reaction and the plasma ball milling reaction can effectively activate reactants, promote the reaction, improve the preparation efficiency of the silicon-carbon composite material and have industrial prospect.
Another object of the present invention is to provide a silicon carbon composite material.
The purpose of the invention is realized by the following technical scheme.
A preparation method of a silicon-carbon composite material comprises the following steps: performing ball milling reaction on a silicon source and a carbon source to obtain the silicon-carbon composite material, wherein the silicon source is a silicon alloy, and the carbon source is chlorobenzene, bromobenzene or iodobenzene.
In the technical scheme, the temperature of the ball milling reaction is 100-600 ℃.
In the technical scheme, the heating rate of heating to 100-600 ℃ is 1-20 ℃/min.
In the technical scheme, the ball milling reaction is a plasma ball milling reaction.
In the technical scheme, the voltage of the plasma in the plasma ball milling reaction is set to be 10-15KV, and the current is set to be 0.5-1.5A.
In the above technical scheme, the ratio of the silicon source to the carbon source is (1.5-3): 1.
in the technical scheme, the ball milling reaction is placed in an inert gas environment.
In the technical scheme, the ball milling reaction time is at least 0.5 h.
In the technical scheme, the cleaning is carried out after the ball milling reaction, and the cleaning is used for washing off by-products in the ball milling reaction process, wherein the by-products are salts formed by cations in the silicon alloy and halogen in a carbon source.
In the above technical scheme, ethanol, methanol or tetrahydrofuran is used for cleaning.
In the above technical solution, the silicon source is calcium silicide, magnesium silicide, iron silicide or aluminum silicide.
The silicon-carbon composite material is of a layered structure and is formed by uniformly compounding silicon elements and carbon elements in parts by weight, and the content of the silicon elements in the silicon-carbon composite material is 35-80 wt% in parts by weight.
The industrial ball milling process adopted by the preparation method promotes the reaction to be rapidly carried out, has high efficiency, is easy to realize uniform compounding and can be amplified; meanwhile, through chemical design, no tail gas is theoretically discharged, tail gas treatment is not needed, the production environment requirement and the environmental protection pressure are low, industrial popularization is facilitated, and contribution can be made to promotion of industrial application of the silicon-carbon material.
The silicon source and the carbon source adopted by the invention are industrial products, and the reaction is promoted through a simple ball milling process, so that the preparation of the silicon-carbon composite material in one step is realized. The realization of the technology has important significance for breaking through the problems that the current silicon-carbon composite material preparation technical route is long in time consumption, multiple in steps and limited in industrial popularization. Meanwhile, the technical process and the preparation of the silicon-carbon composite material can not generate waste gas theoretically, which means that the requirement on production environment is low, the industrial clearance is facilitated, the economic benefit is high, and the environmental protection is facilitated. Different from the early-stage silicon-carbon composite material, the carbon source selected by the invention is beneficial to obtaining high-quality carbon products, thereby laying a foundation for obtaining the high-performance silicon-carbon composite material.
In order to meet the requirements of the industry on different silicon-carbon materials, the invention is based on a high-temperature ball-milling carbon-coating process, the reaction temperature is set to be 100-600 ℃, a solid silicon source and a carbon source are heated to form a liquid phase, and the liquid phase and the prepared silicon material are subjected to impregnation ball-milling compounding to obtain the high-performance silicon-carbon composite material. Compared with the existing carbon coating process, such as conventional carbon source gas phase pyrolysis coating, the ball milling auxiliary carbon coating efficiency is higher and the coating is more uniform.
Drawings
FIG. 1 is a scanning electron microscope image of a silicon-carbon composite material obtained in example 1 of the present invention;
FIG. 2 is a distribution diagram of Si element in the Si-C composite material obtained in example 1 of the present invention;
FIG. 3 is a diagram showing the distribution of carbon in the Si-C composite material obtained in example 1 of the present invention;
FIG. 4 is a scanning electron microscope image of the silicon-carbon composite material obtained in example 2 of the present invention;
FIG. 5 is a scanning electron microscope image of the silicon-carbon composite material obtained in example 3 of the present invention;
FIG. 6 is a scanning electron micrograph of a silicon-carbon composite product obtained in example 8.
Detailed Description
The technical scheme of the invention is further explained by combining specific examples.
The instruments involved in the following examples are as follows: high-temperature vibration ball mill of Hefei Kejing materials Co., Ltd, model HTVB-50, PBMS type plasma ball mill of south China university of science.
The drugs referred to in the following examples are as follows: calcium silicide, chlorobenzene, bromobenzene and iodobenzene are all commercially available reagents, and the purity is analytical purity.
Example 1
A preparation method of a silicon-carbon composite material comprises the following steps: putting a silicon source and a carbon source into a ball milling tank, heating the temperature from 20-25 ℃ to 200 ℃ at the heating rate of 5 ℃/min under the argon atmosphere, carrying out ball milling reaction for 0.5h, cooling to 20-25 ℃ after the ball milling reaction is finished (the argon atmosphere is continuously kept), washing with ethanol to remove by-products (cations in the silicon source and halogens in the carbon source form salts) in the ball milling reaction process, and obtaining the silicon-carbon composite material, wherein the silicon source is calcium silicide, the carbon source is hexachlorobenzene, and the ratio of the silicon source to the carbon source is 3:1 according to the amount of the substances. The content of silicon element in the silicon-carbon composite material is 70 wt%.
Fig. 1 is a scanning electron microscope image of the silicon-carbon composite material obtained in example 1 of the present invention, which shows that calcium silicide reacts with chlorobenzene to generate layered silicon, and the layered silicon is tightly wrapped by carbon to obtain a silicon-carbon composite structure. And performing energy spectrum analysis, wherein the distribution graphs of the silicon element and the carbon element are respectively shown in fig. 2 and fig. 3, and the distribution graphs of the silicon element and the carbon element are completely superposed, so that the uniform compounding of the carbon and the silicon is realized.
Example 2
A preparation method of a silicon-carbon composite material comprises the following steps: putting a silicon source and a carbon source into a ball milling tank, heating the temperature from 20-25 ℃ to 200 ℃ at the heating rate of 5 ℃/min under the argon environment, carrying out ball milling reaction for 2h, cooling to 20-25 ℃ after the ball milling reaction is finished (the argon environment is continuously kept), cleaning with ethanol to remove by-products (cations in the silicon source and halogens in the carbon source form salts) in the ball milling reaction process, and obtaining the silicon-carbon composite material, wherein the silicon source is calcium silicide, the carbon source is hexabromobenzene, and the ratio of the silicon source to the carbon source is 3:1 by the mass. The content of silicon element in the silicon-carbon composite material is 70 wt%. The silicon-carbon composite material was observed by a scanning electron microscope, which showed that the silicon-carbon composite material was in the form of a layered silicon/carbon composite structure, as shown in fig. 4.
Example 3
A preparation method of a silicon-carbon composite material comprises the following steps: putting a silicon source and a carbon source into a ball milling tank, heating the temperature from 20-25 ℃ to 200 ℃ at the heating rate of 5 ℃/min under the argon atmosphere, carrying out ball milling reaction for 4h, cooling to 20-25 ℃ after the ball milling reaction is finished (the argon atmosphere is continuously kept), cleaning with ethanol to remove by-products (cations in the silicon source and halogens in the carbon source form salts) in the ball milling reaction process, and obtaining the silicon-carbon composite material, wherein the silicon source is calcium silicide, the carbon source is hexaiodobenzene, and the ratio of the silicon source to the carbon source is 3:1 according to the amount of the substances. The content of silicon element in the silicon-carbon composite material is 70 wt%. The silicon-carbon composite material was observed by a scanning electron microscope, which showed that the silicon-carbon composite material was in the form of a layered silicon/carbon composite structure, as shown in fig. 5.
Example 4
A preparation method of a silicon-carbon composite material comprises the following steps: putting a silicon source and a carbon source into a ball milling tank, carrying out plasma ball milling reaction for 1h in an argon environment, setting the voltage of plasma to be 15KV, controlling the current to be 1.5A, cooling to room temperature of 20-25 ℃ after the plasma ball milling reaction is finished (keeping the argon environment continuously), washing by using methanol for washing off byproducts (cations in the silicon source and halogens in the carbon source form salts) in the ball milling reaction process to obtain the silicon-carbon composite material, wherein the silicon source is calcium silicide, the carbon source is hexachlorobenzene, and the ratio of the silicon source to the carbon source is 3:1 according to the amount of substances. The content of silicon element in the silicon-carbon composite material is 70 wt%.
Example 5
A preparation method of a silicon-carbon composite material comprises the following steps: putting a silicon source and a carbon source into a ball milling tank, heating the temperature from 20-25 ℃ to 200 ℃ at the heating rate of 5 ℃/min under the argon environment, carrying out ball milling reaction for 1h, cooling to 20-25 ℃ after the ball milling reaction is finished (the argon environment is continuously kept), cleaning by using tetrahydrofuran, and washing off by-products (cations in the silicon source and halogens in the carbon source form salts) in the ball milling reaction process to obtain the silicon-carbon composite material, wherein the silicon source is magnesium silicide, the carbon source is hexachlorobenzene, and the ratio of the silicon source to the carbon source is 3:2 according to the amount of the materials. The content of silicon element in the silicon-carbon composite material is 35 wt%.
Example 6
A preparation method of a silicon-carbon composite material comprises the following steps: putting a silicon source and a carbon source into a ball milling tank, heating the temperature from 20-25 ℃ to 200 ℃ at the heating rate of 5 ℃/min under the argon atmosphere, carrying out ball milling reaction for 1h, cooling to 20-25 ℃ after the ball milling reaction is finished (the argon atmosphere is continuously kept), cleaning with ethanol to remove by-products (cations in the silicon source and halogens in the carbon source form salts) in the ball milling reaction process, and obtaining the silicon-carbon composite material, wherein the silicon source is ferric silicide, the carbon source is hexachlorobenzene, and the ratio of the silicon source to the carbon source is 2:1 by the mass. The content of silicon element in the silicon-carbon composite material is 80 wt%.
Example 7
A preparation method of a silicon-carbon composite material comprises the following steps: putting a silicon source and a carbon source into a ball milling tank, heating the temperature from room temperature 20-25 ℃ to 200 ℃ at a heating rate of 5 ℃/min under an argon environment, carrying out ball milling reaction for 1h, cooling to room temperature 20-25 ℃ after the ball milling reaction is finished (the argon environment is continuously kept), washing with ethanol to remove by-products (cations in the silicon source and halogens in the carbon source form salts) in the ball milling reaction process, and obtaining the silicon-carbon composite material, wherein the silicon source is silicon-aluminum alloy (AlSi), the carbon source is hexachlorobenzene, and the ratio of the silicon source to the carbon source is 2:1 according to the amount of the substances. The content of silicon element in the silicon-carbon composite material is 80 wt%.
Comparative example 1
A preparation method of a silicon-carbon composite material comprises the following steps: the method comprises the steps of manually grinding and mechanically mixing a silicon source and a carbon source, heating the mixture to 200 ℃ from room temperature of 20-25 ℃ at a heating rate of 5 ℃/min under an argon environment for more than 3 hours after mechanically mixing, continuously maintaining the argon environment, cooling the mixture to the room temperature of 20-25 ℃, and cleaning the mixture with ethanol to obtain the silicon-carbon composite material, wherein the silicon source is calcium silicide, the carbon source is hexachlorobenzene, and the ratio of the silicon source to the carbon source is 3:1 by mass.
The preparation efficiency of the silicon carbon composite material in comparative example 1 was significantly lower than that of the reaction process in example 1.
Comparative example 2
A preparation method of a silicon-carbon composite material comprises the following steps: putting a silicon source and a carbon source into a ball milling tank, heating the temperature from 20-25 ℃ to 200 ℃ at the heating rate of 5 ℃/min under the argon atmosphere, carrying out ball milling reaction for 0.5h, cooling to 20-25 ℃ after the ball milling reaction is finished (the argon atmosphere is continuously kept), and cleaning with ethanol to obtain the silicon-carbon composite material, wherein the silicon source is calcium silicide, the carbon source is PVC (k-value 62-60), and the ratio of the silicon source to the carbon source is 8:5 in parts by mass. During the reaction, a large amount of gas is released, often resulting in an overpressure. The main components of the tail gas are hydrocarbon gas and hydrogen gas, and subsequent treatment is needed.
Applying the silicon-carbon composite material to a lithium battery, taking 0.6g of one of the silicon-carbon composite materials in examples 1-7 and comparative example 2, 0.2g of acetylene black as a conductive agent and 0.2g of polyacrylic acid (PAA) as a binder, grinding and mixing uniformly, dripping 10 milliliters of deionized water, grinding to obtain slurry, scraping the slurry on a copper foil by using a scraper, wherein the surface density of the silicon-carbon composite material is 1mg/cm 2 The button cell is dried for 12h at the temperature of 80 ℃ in vacuum, a round electrode with the diameter of 10mm is punched by a tablet press, a 2032 button cell is assembled by taking a lithium sheet as a counter electrode, when the charge-discharge rate is 50mAh/g, the initial discharge capacity of the button cell obtained in the embodiments 1-7 is 1600-mAh/g, the initial charge capacity is 1800mAh/g, the 50-circle circulation stable circulation charge-discharge capacity is 1600-mAh/g, and the button cell has obvious advantages compared with the current theoretical capacity 372mAh/g which takes commercial graphite as an electrode raw material.
The performance of the 2032 coin cell obtained in examples 1 to 7 and comparative example 2 was as follows:
example 8
The silicon-carbon composite material obtained in example 1 was carbon-coated using mesophase pitch (zhangwei. mesophase pitch and research on the preparation of carbon foam thereof [ D ]. tianjin university, 2007.) as a raw material, and the specific operation method was: mixing the silicon-carbon composite material obtained in the example 1 and the mesophase pitch according to the mass ratio of 5: 1, heating and ball milling, ball milling for 1h at 500 ℃, and then pyrolyzing for 2h at 800 ℃ in argon atmosphere to realize further carbon coating, thereby obtaining the silicon-carbon composite product. Scanning electron microscopy showed that the layered silicon was completely encapsulated by carbon, reaching the expected carbon encapsulation assumption, with the SEM shown in fig. 6.
The lithium storage test of the obtained product is performed in the same manner as the performance test process of the negative electrode of the lithium ion battery made of silicon-carbon material obtained in the above examples 1 to 7. The test shows that 1540mAh/g is discharged for the first time, 1420mAh/g is charged for the first time, and 1360mAh/g is discharged for 50 times. By coating carbon, the cycling stability of lithium storage of silicon carbon products is improved.
The invention being thus described by way of example, it should be understood that any simple alterations, modifications or other equivalent alterations as would be within the skill of the art without the exercise of inventive faculty, are within the scope of the invention.
Claims (10)
1. A preparation method of a silicon-carbon composite material is characterized by comprising the following steps: performing ball milling reaction on a silicon source and a carbon source to obtain the silicon-carbon composite material, wherein the silicon source is a silicon alloy, and the carbon source is chlorobenzene, bromobenzene or iodobenzene.
2. The method of claim 1, wherein the silicon source is calcium silicide, magnesium silicide, iron silicide, or aluminum silicide.
3. The preparation method according to claim 2, wherein the temperature of the ball milling reaction is 100 to 600 ℃.
4. The method according to claim 3, wherein the heating rate of the temperature to 100 to 600 ℃ is 1 to 20 ℃/min.
5. The method of claim 1, wherein the ball milling reaction is a plasma ball milling reaction.
6. The preparation method according to claim 5, wherein the voltage of the plasma in the plasma ball milling reaction is set to 10-15KV, and the current is set to 0.5-1.5A.
7. The method according to claim 1, wherein the ratio of the silicon source to the carbon source is (1.5-3): 1.
8. the method of claim 1, wherein the ball milling reaction is conducted in an inert gas environment.
9. The preparation method of claim 1, wherein the time of the ball milling reaction is at least 0.5h, and after the ball milling reaction, the cleaning is performed to wash away by-products generated in the process of the ball milling reaction, wherein the by-products are salts formed by cations in the silicon alloy and halogens in a carbon source, and ethanol, methanol or tetrahydrofuran is used for cleaning.
10. The silicon-carbon composite material is characterized by having a layered structure, and being formed by uniformly compounding silicon elements and carbon elements according to the parts by weight of substances, wherein the content of the silicon elements in the silicon-carbon composite material is 35-80 wt% according to the parts by weight of the substances.
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| US20170256793A1 (en) * | 2014-08-27 | 2017-09-07 | Kabushiki Kaisha Toyota Jidoshokki | Production process for carbon-coated silicon material |
| CN108539156A (en) * | 2018-03-30 | 2018-09-14 | 北京国能电池科技股份有限公司 | Lithium ion battery negative material, lithium ion battery and its device of driving and preparation method |
| CN110767881A (en) * | 2018-07-26 | 2020-02-07 | 纳诺思能源有限公司 | High-silicon-content carbon-silicon sandwich material, preparation method thereof and application thereof in lithium ion battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170256793A1 (en) * | 2014-08-27 | 2017-09-07 | Kabushiki Kaisha Toyota Jidoshokki | Production process for carbon-coated silicon material |
| CN108539156A (en) * | 2018-03-30 | 2018-09-14 | 北京国能电池科技股份有限公司 | Lithium ion battery negative material, lithium ion battery and its device of driving and preparation method |
| CN110767881A (en) * | 2018-07-26 | 2020-02-07 | 纳诺思能源有限公司 | High-silicon-content carbon-silicon sandwich material, preparation method thereof and application thereof in lithium ion battery |
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