CN111697206A - Preparation method of silicon-carbon negative electrode material - Google Patents
Preparation method of silicon-carbon negative electrode material Download PDFInfo
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- CN111697206A CN111697206A CN201910192422.6A CN201910192422A CN111697206A CN 111697206 A CN111697206 A CN 111697206A CN 201910192422 A CN201910192422 A CN 201910192422A CN 111697206 A CN111697206 A CN 111697206A
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- 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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- 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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- 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
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Abstract
The invention provides a preparation method of a silicon-carbon anode material, which comprises the following steps: mixing, high-temperature treatment and carbon coating, wherein in the obtained silicon-carbon negative electrode material, silicon materials are uniformly distributed in graphite particles and are tightly combined with carbon particles, so that the silicon-carbon bonding strength is higher, and the technical defects that the silicon materials are not uniformly dispersed, larger silicon particles are easily pulverized, and a silicon-carbon structure is easily peeled off due to weak silicon-carbon bonding strength in the prior art are overcome; in the obtained silicon-carbon negative electrode material, the content of nano silicon can reach (5-50)%, so that the gram specific capacity, the efficiency and the cycle use frequency of the silicon-carbon negative electrode material are effectively improved; meanwhile, the method provided by the invention has the advantages of simple steps, wide material requirements, high realizable degree in industrial production and stable quality of the obtained product.
Description
Technical Field
The invention relates to the field of preparation of lithium battery cathode materials, in particular to a preparation method of a silicon-carbon cathode material.
Background
With the national regulation of new energy automobile policies and the higher requirements of new energy automobile enterprises on the energy density of batteries, the aim is urgently needed to be achieved by improving the gram specific capacity of the lithium battery negative electrode material. Therefore, research on negative electrode materials for lithium batteries is shifting toward high capacity, high rate, long cycle, and low price. In the negative electrode materials for the lithium ion battery in the current market, the graphite carbon materials still occupy the main position, but the gram specific capacity research of the traditional graphite negative electrode materials is close to the limit, so that the energy density of the lithium battery cannot be greatly improved. Because the silicon element and the carbon element are in the same main group and are the second-order elements in the earth crust, and the theoretical gram specific capacity of silicon reaches 4200mAh/g, the silicon-containing negative electrode material becomes the best substitute of a graphite negative electrode material. However, silicon as a lithium battery negative electrode material has huge expansion and shrinkage in the charging and discharging processes, so that the negative electrode part of the lithium battery is structurally collapsed, demoulding is caused, and finally the lithium battery fails. Therefore, how to prolong the charge and discharge service life of the silicon-containing anode material has been a main subject of research in the field of silicon-based materials for many years.
The realization of the combination of silicon and carbon is the key content of the preparation of the silicon-carbon cathode material. The method of preparing a silicon-carbon negative electrode material by simple mechanical mixing is called a solid phase mixing method, but silicon obtained by this method is not tightly bonded to graphite and a large amount of silicon is exposed to an electrolyte, adversely affecting electrochemical properties. The liquid phase composite method is used for better dispersing raw materials in a mild environment, promotes the combination of silicon and graphite in modes of amorphous carbon and the like, and is the main direction for preparing the silicon-carbon cathode material at present.
Disclosure of Invention
The invention aims to overcome the technical defects and defects of uneven silicon material dispersion, easy pulverization of larger silicon particles, structural peeling caused by weak silicon-carbon bonding strength and the like in the prior art by providing a preparation method of a silicon-carbon negative electrode material.
In order to realize the purpose, the following technical scheme is provided:
a preparation method of a silicon-carbon negative electrode material comprises the following steps:
s1, mixing: mixing silicon powder and graphite powder, and mechanically stirring to obtain uniformly mixed powder;
s2, high-temperature treatment: placing the mixed powder in a high-temperature treatment device, carrying out multistage vacuum pumping treatment on the high-temperature treatment device to enable the pressure value in the high-temperature treatment device to reach 50-100 Pa, raising the temperature in the device to 1000-1500 ℃, preserving heat for 1-3 hours, introducing inert gas into the high-temperature treatment device until the air pressure value reaches 0.4-0.8 MPa, continuing preserving heat for 2-4 hours, carrying out pressure impregnation treatment on the mixed powder to enable silicon powder in the mixed powder to be molten to obtain nano silicon, uniformly distributing the nano silicon in graphite powder, and combining the nano silicon powder with the graphite powder to form a silicon-carbon structure to obtain silicon-carbon powder;
s3, carbon coating: mixing the silicon-carbon powder obtained after high-temperature treatment with an organic carbon source in proportion, raising the temperature to 600-800 ℃, and carrying out carbonization treatment for 2-6 hours to form a carbon coating layer on the surface of the silicon-carbon structure, thereby obtaining the required silicon-carbon cathode material.
Preferably, in step S1, the mixing ratio of the silicon powder and the graphite powder is: 5:95-50:50, the rotating speed of a stirring rod for mechanical stirring is as follows: 15-30r/min, and the stirring time is 2-5 hours.
Preferably, the silicon powder in step S1 is monocrystalline silicon powder or polycrystalline silicon powder, and the graphite powder is one or a mixture of two or more of natural graphite powder, artificial graphite powder, and mesophase graphite powder.
Preferably, in the step S2, the multi-stage vacuum-pumping process is performed by using a combination of a rotary vane pump, a slide valve pump and a roots pump to form a multi-stage vacuum-pumping mechanism, so that the pressure value in the high-temperature processing device finally reaches the requirement.
Preferably, the inert gas in step S2 is nitrogen or argon.
Preferably, the organic carbon source in step S3 is one of asphalt, tar or organic polymer.
The invention has the beneficial effects that:
1. in the silicon-carbon negative electrode material obtained by the method, the silicon material is uniformly distributed in the graphite particles and is tightly combined with the carbon particles, so that the silicon-carbon bonding strength is higher, and the technical defects that the silicon material is not uniformly dispersed, larger silicon particles are easily pulverized, and the silicon-carbon structure is easily peeled off due to weak silicon-carbon bonding strength in the prior art are overcome.
2. The content of nano silicon in the silicon-carbon negative electrode material obtained by the method can reach (5-50)%, so that the gram specific capacity, the efficiency and the recycling frequency of the silicon-carbon negative electrode material are effectively improved.
3. The method provided by the invention has the advantages of simple steps, low material requirement, high realizable degree in industrial production and stable quality of the obtained product.
Drawings
1. FIG. 1 is a scanning electron microscope photograph of a negative electrode material obtained in an embodiment of the present invention, in which 1a is a 500-fold real object magnification drawing, 1b is a 1000-fold real object magnification drawing, and 1c and 1d are 2000-fold real object magnification drawings;
2. fig. 2 is a charge-discharge curve diagram of a button lithium battery made of the silicon-carbon negative electrode powder obtained in the embodiment.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and examples.
A preparation method of a silicon-carbon negative electrode material comprises the following steps:
s1, mixing: mixing silicon powder and graphite powder, and mechanically stirring to obtain uniformly mixed powder;
s2, high-temperature treatment: placing the mixed powder in a high-temperature treatment device, carrying out multistage vacuum pumping treatment on the high-temperature treatment device to enable the pressure value in the high-temperature treatment device to reach 50-100 Pa, raising the temperature in the device to 1000-1500 ℃, preserving heat for 1-3 hours, introducing inert gas into the high-temperature treatment device until the air pressure value reaches 0.4-0.8 MPa, continuing preserving heat for 2-4 hours, carrying out pressure impregnation treatment on the mixed powder to enable silicon powder in the mixed powder to be molten to obtain nano silicon, uniformly distributing the nano silicon in graphite powder, and combining the nano silicon powder with the graphite powder to form a silicon-carbon structure to obtain silicon-carbon powder;
s3, carbon coating treatment: mixing the silicon-carbon powder obtained after high-temperature treatment with an organic carbon source in proportion, raising the temperature to 600-800 ℃, and carrying out carbonization treatment for 2-6 hours to form a carbon coating layer on the surface of the silicon-carbon structure, thereby obtaining the required silicon-carbon cathode material.
In step S1, the mixing ratio of the silicon powder and the graphite powder is: 5:95-50:50, the rotating speed of a stirring rod for mechanical stirring is as follows: 15-30r/min, and the stirring time is 2-5 hours.
The silicon powder in step S1 is monocrystalline silicon powder or polycrystalline silicon powder, and the graphite powder is one or a mixture of two or more of natural graphite powder, artificial graphite powder, and intermediate phase graphite powder.
In step S2, the multi-stage vacuum process is performed by using a combination of a vane pump, a slide valve pump, and a roots pump, so as to form a multi-stage vacuum mechanism.
Wherein, the inert gas in the step S2 is one of nitrogen or argon.
Wherein, the organic carbon source in step S3 is one of asphalt, tar or organic polymer.
Example one
S1, mixing: mixing monocrystalline silicon powder and natural graphite powder according to a ratio of 5:95, and mechanically stirring for 2 hours at a rotating speed of a stirring rod of 15r/min to obtain uniformly mixed powder;
s2, high-temperature treatment: placing the mixed powder in a high-temperature treatment device, carrying out multistage vacuum pumping treatment on the high-temperature treatment device to enable the pressure value in the high-temperature treatment device to reach 50Pa, raising the temperature in the device to 1000 ℃, keeping the temperature for 1 hour, introducing inert gas into the high-temperature treatment device until the air pressure value reaches 0.4MPa, continuing keeping the temperature for 2 hours, carrying out pressure impregnation treatment on the mixed powder to enable silicon powder in the mixed powder to be molten to obtain nano-silicon, uniformly distributing the nano-silicon in graphite powder, and combining the nano-silicon with the graphite powder to form a silicon-carbon structure to obtain silicon-carbon powder;
s3, carbon coating treatment: and mixing the silicon-carbon powder obtained after the high-temperature treatment with an organic carbon source in proportion, raising the temperature to 600 ℃, and carrying out carbonization treatment for 2 hours to form a carbon coating layer on the surface of the silicon-carbon structure, thereby obtaining the required silicon-carbon cathode material.
Example two
S1, mixing: mixing the monocrystalline silicon powder and the artificial stone ink powder according to the ratio of 20:80, and mechanically stirring for 3 hours at the rotating speed of a stirring rod of 20r/min to obtain uniformly mixed powder;
s2, high-temperature treatment: placing the mixed powder in a high-temperature treatment device, carrying out multistage vacuum pumping treatment on the high-temperature treatment device to enable the pressure value in the high-temperature treatment device to reach 80Pa, raising the temperature in the device to 1300 ℃, preserving heat for 2 hours, introducing argon into the high-temperature treatment device until the air pressure value reaches 0.6MPa, continuing preserving heat for 3 hours, carrying out pressure impregnation treatment on the mixed powder to enable silicon powder in the mixed powder to be molten to obtain nano-silicon, uniformly distributing the nano-silicon in graphite powder, and combining the nano-silicon with the graphite powder to form a silicon-carbon structure to obtain silicon-carbon powder;
s3, carbon coating treatment: and mixing the silicon-carbon powder obtained after the high-temperature treatment with an organic carbon source in proportion, raising the temperature to 700 ℃, and carrying out carbonization treatment for 4 hours to form a carbon coating layer on the surface of the silicon-carbon structure, thereby obtaining the required silicon-carbon cathode material.
EXAMPLE III
S1, mixing: mixing polycrystalline silicon powder with mixed graphite powder of natural graphite powder, artificial stone ink powder and mesophase stone ink powder according to a ratio of 50:50, and mechanically stirring for 5 hours at a stirring rod rotating speed of 30r/min to obtain uniformly mixed powder;
s2, high-temperature treatment: placing the mixed powder in a high-temperature treatment device, carrying out multi-stage vacuum-pumping treatment on the high-temperature treatment device to enable the pressure value in the high-temperature treatment device to reach 100Pa, raising the temperature in the device to 1500 ℃, keeping the temperature for 3 hours, introducing nitrogen into the high-temperature treatment device to enable the air pressure value to reach 0.8MPa, continuing keeping the temperature for 4 hours, carrying out pressurization dipping treatment on the mixed powder to enable silicon powder in the mixed powder to be molten to obtain nano-silicon, uniformly distributing the nano-silicon in graphite powder, and combining the nano-silicon with the graphite powder to form a silicon-carbon structure to obtain silicon-carbon powder;
s3, carbon coating treatment: and mixing the silicon-carbon powder obtained after the high-temperature treatment with an organic carbon source in proportion, raising the temperature to 800 ℃, and carrying out carbonization treatment for 4 hours to form a carbon coating layer on the surface of the silicon-carbon structure, thereby obtaining the required silicon-carbon cathode material.
As shown in the attached figure 1, the content of nano-silicon in the obtained silicon-carbon negative electrode material is high by using the method provided by the invention, and the nano-silicon is uniformly dispersed in graphite particles and is tightly combined with the graphite.
The theoretical gram specific capacity of the traditional graphite negative electrode material is 272/mAh, the highest gram specific capacity which can be realized in practical production is 365/mAh, and as shown in the attached figure 2, the charge capacity of the button lithium battery prepared from the silicon-carbon negative electrode material obtained by the method reaches (525+12.4)/mAh, the discharge capacity reaches 491.3/mAh, and compared with the negative electrode capacity of the lithium battery in the prior art, the negative electrode capacity is respectively improved by 47.2% and 34.6%.
In summary, the disclosure of the present invention is not limited to the above-mentioned embodiments, and persons skilled in the art can easily suggest other embodiments within the technical teaching of the present invention, but such embodiments are included in the scope of the present invention.
Claims (6)
1. The preparation method of the silicon-carbon negative electrode material is characterized by comprising the following steps of:
s1, mixing: mixing silicon powder and graphite powder, and mechanically stirring to obtain uniformly mixed powder;
s2, high-temperature treatment: placing the mixed powder in a high-temperature treatment device, carrying out multistage vacuum pumping treatment on the high-temperature treatment device to enable the pressure value in the high-temperature treatment device to reach 50-100 Pa, raising the temperature in the device to 1000-1500 ℃, preserving heat for 1-3 hours, introducing inert gas into the high-temperature treatment device until the air pressure value reaches 0.4-0.8 MPa, continuing preserving heat for 2-4 hours, carrying out pressure impregnation treatment on the mixed powder to enable silicon powder in the mixed powder to be molten to obtain nano silicon, uniformly distributing the nano silicon in graphite powder, and combining the nano silicon powder with the graphite powder to form a silicon-carbon structure to obtain silicon-carbon powder;
s3, carbon coating: mixing the silicon-carbon powder obtained after high-temperature treatment with an organic carbon source in proportion, raising the temperature to 600-800 ℃, and carrying out carbonization treatment for 2-6 hours to form a carbon coating layer on the surface of the silicon-carbon structure, thereby obtaining the required silicon-carbon cathode material.
2. The method for preparing a silicon-carbon anode material according to claim 1, wherein in the step S1, the mixing ratio of the silicon powder and the graphite powder is as follows: 5:95-50:50, the rotating speed of a stirring rod for mechanical stirring is as follows: 15-30r/min, and the stirring time is 2-5 hours.
3. The method according to claim 1, wherein the silicon powder in step S1 is monocrystalline silicon powder or polycrystalline silicon powder, and the graphite powder is one or a mixture of two or more of natural graphite powder, artificial graphite powder, and mesolite powder.
4. The method as claimed in claim 1, wherein in step S2, the multi-stage vacuum-pumping process is performed by using a combination of a vane pump, a slide valve pump and a roots pump to form a multi-stage vacuum-pumping mechanism, so as to finally achieve the required pressure in the high-temperature processing apparatus.
5. The method of claim 1, wherein the inert gas in step S2 is nitrogen or argon.
6. The method of claim 1, wherein the organic carbon source in step S3 is one of pitch, tar, or organic polymer.
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2019
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Application publication date: 20200922 |