CN110048092B - Lithium battery silicon-carbon composite material and preparation method thereof - Google Patents
Lithium battery silicon-carbon composite material and preparation method thereof Download PDFInfo
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- CN110048092B CN110048092B CN201910155100.4A CN201910155100A CN110048092B CN 110048092 B CN110048092 B CN 110048092B CN 201910155100 A CN201910155100 A CN 201910155100A CN 110048092 B CN110048092 B CN 110048092B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—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
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—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
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of a lithium battery silicon-carbon composite material, which comprises the following steps: sending the coarse silicon powder into a plasma spraying system through a first powder feeder by using inert gas to be evaporated into silicon vapor, sending graphite into a cooling kettle through a second powder feeder by using inert gas, and condensing or depositing the silicon vapor on the graphite in the cooling kettle to form a mixture of nano silicon powder and graphite; and then, conveying the mixture of the nano silicon powder and the graphite into a CVD furnace for vapor deposition carbon coating, conveying the mixture into a fusion machine for fusion with a binder, and then carbonizing the mixture at high temperature through a roller kiln to obtain the silicon-carbon composite material product. According to the invention, the plasma spraying system is adopted to carry out nanocrystallization on the silicon, so that the expansion characteristic of the material is effectively inhibited, and the cycle performance of the material is improved. CVD is adopted to coat the nano silicon and graphite surfaces to form a conductive carbon layer, and the conductive carbon layer is mechanically fused with a binder and carbonized at high temperature in the later period to improve the first efficiency and the cycle performance of the product.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a lithium battery silicon-carbon composite material and a preparation method thereof.
Background
With the rapid development of the demand of the times, the energy density of lithium ion batteries is increased at a rate of 7% -10% per year. In 2016, the hard index of the energy density of the power battery is released in China, and according to the technical route chart of energy-saving and new energy vehicles, the energy density target of the power battery of the pure electric vehicle in 2020 is 350 W.h/kg. The currently commercialized lithium ion battery mainly adopts graphite as a negative electrode material, but the theoretical specific capacity of the graphite is only 372mAh/g, so that the further improvement of the specific energy of the lithium ion battery is limited; because the silicon cathode based on alloying reaction has the theoretical lithium storage capacity as high as 4200mAh/g, the silicon cathode material is always concerned and is one of the most potential next-generation lithium ion battery cathode materials. In order to meet the requirements of new-generation energy, the development of a novel lithium battery cathode technology is imminent. However, silicon suffers from severe volume expansion (about 300%) during charging and discharging, and the huge volume effect and low conductivity limit the commercial application of silicon anode technology.
Disclosure of Invention
In view of the above, the present invention provides a lithium battery silicon-carbon composite material and a preparation method thereof, which can effectively solve the defects of the existing silicon negative electrode material, such as obvious volume effect and poor material cycle stability.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a lithium battery silicon-carbon composite material comprises the following steps: sending the coarse silicon powder into a plasma spraying system through a first powder feeder by using inert gas to be evaporated into silicon vapor, sending graphite into a cooling kettle through a second powder feeder by using inert gas, and condensing or depositing the silicon vapor on the graphite in the cooling kettle to form a mixture of nano silicon powder and graphite; and then, conveying the mixture of the nano silicon powder and the graphite into a CVD furnace for vapor deposition carbon coating, conveying the mixture into a fusion machine for fusion with a binder, and then carbonizing the mixture at high temperature through a roller kiln to obtain the silicon-carbon composite material product.
Preferably, the coarse silicon powder is one or a combination of two of high-purity monocrystalline silicon and polycrystalline silicon, and the particle size d50 in the coarse silicon powder is 10-50 μm.
Preferably, the inert gas is any one of high-purity nitrogen, argon, helium, xenon, neon or krypton or a combination of at least two of the above gases.
As a preferable scheme, the feeding amount of the first powder feeder is 1-10 kg/h.
Preferably, the pressure of the inert gas input into the plasma spraying system is 0.5-0.8mPa, and the pressure of the hydrogen input into the plasma spraying system is 0.05-0.5 mPa.
As a preferable scheme, the graphite is one or more of secondary particle natural graphite or artificial graphite; the particle size d50 in the graphite is 10-20 μm, and the graphite feeding amount of the second powder feeder is 10-200 kg/h.
As a preferable scheme, the coating gas input by the CVD furnace is a mixed gas composed of any one or combination of at least two of methane, ethane, propane, ethylene, propylene or acetylene and argon, the coating temperature is 800-.
As a preferable scheme, the binder is one or more of petroleum asphalt, coal asphalt and polycondensation resin; the binder accounts for 3 to 30 percent of the mass of the mixture; the petroleum asphalt and/or the coal asphalt are molten petroleum asphalt and/or coal asphalt; the polycondensation resin is one or more of phenolic resin, epoxy resin, acrylic resin, furfural resin and polyester resin; the rotating speed of the fusion machine is 800-; the fusion time of the fusion machine is 0.5-5 h.
As a preferable scheme, the heating rate of the roller kiln is preferably 0.5-20 ℃/min, and the upper limit temperature of the roller kiln is 900-.
A lithium battery silicon-carbon composite material is prepared by the preparation method of the lithium battery silicon-carbon composite material.
Compared with the prior art, the invention has obvious advantages and beneficial effects, and specifically, the technical scheme includes that:
according to the invention, the plasma spraying system is adopted to carry out nanocrystallization on the silicon, so that the expansion characteristic of the material is effectively inhibited, and the cycle performance of the material is improved. CVD is adopted to coat the nano silicon and graphite surfaces to form a conductive carbon layer, and the conductive carbon layer is mechanically fused with a binder and carbonized at high temperature in the later period to improve the first efficiency and the cycle performance of the product. The invention has the greatest characteristic that silicon is nano-sized and uniformly dispersed in graphite, and a stable conductive carbon layer and a coating structure are formed through two coating processes, so that the expansion of the material is effectively inhibited, and the stability of the structure is ensured.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a scanning electron micrograph of a sample obtained according to an embodiment of the present invention;
fig. 3 is a graph of a simulated battery obtained after a sample is manufactured into an electrode according to an embodiment of the present invention.
Detailed Description
The invention discloses a preparation method of a lithium battery silicon-carbon composite material, which comprises the following steps: sending the coarse silicon powder into a plasma spraying system through a first powder feeder by using inert gas to be evaporated into silicon vapor, sending graphite into a cooling kettle through a second powder feeder by using inert gas, and condensing or depositing the silicon vapor on the graphite in the cooling kettle to form a mixture of nano silicon powder and graphite; and then, conveying the mixture of the nano silicon powder and the graphite into a CVD furnace for vapor deposition carbon coating, conveying the mixture into a fusion machine for fusion with a binder, and then carbonizing the mixture at high temperature through a roller kiln to obtain the silicon-carbon composite material product.
The coarse silicon powder is one or the combination of high-purity monocrystalline silicon or polycrystalline silicon, and the particle size d50 in the coarse silicon powder is 10-50 mu m. The inert gas is any one or the combination of at least two of high-purity nitrogen, argon, helium, xenon, neon or krypton. The feeding amount of the first powder feeder is 1-10 kg/h. The pressure of the inert gas input into the plasma spraying system is 0.5-0.8mPa, and the pressure of the hydrogen input into the plasma spraying system is 0.05-0.5 mPa. The graphite is one or more of secondary particle natural graphite or artificial graphite; the particle size d50 in the graphite is 10-20 μm, and the graphite feeding amount of the second powder feeder is 10-200 kg/h. The coating gas input by the CVD furnace is a mixed gas composed of argon and any one or at least two of methane, ethane, propane, ethylene, propylene or acetylene, the coating temperature is 800-1200 ℃, and the coating time is 2-20 h. The binder is one or more of petroleum asphalt, coal asphalt and polycondensation resin; the binder accounts for 3-30% of the mixture by mass percent; the petroleum asphalt and/or the coal asphalt are molten petroleum asphalt and/or coal asphalt; the polycondensation resin is one or more of phenolic resin, epoxy resin, acrylic resin, furfural resin and polyester resin; the rotating speed of the fusion machine is 800-; the fusion time of the fusion machine is 0.5-5 h. The heating rate of the roller kiln is preferably 0.5-20 ℃/min, and the upper limit temperature of the roller kiln is 900-.
The invention also discloses a lithium battery silicon-carbon composite material which is prepared by the preparation method of the lithium battery silicon-carbon composite material.
The invention is illustrated in more detail below with specific examples:
a preparation method of a lithium battery silicon-carbon composite material comprises the following steps:
(1) 1.0kg of silicon powder (the medium particle size d50 is 20um, the purity is 99.98%) is put into a first powder feeder, the system is vacuumized, argon is started, a plasma spraying system is started, the argon pressure is adjusted to be 0.7mPa, hydrogen is adjusted to be 0.1mPa, and the first powder feeder is started and the feeding amount is adjusted to be 1.0 kg/h.
(2) 19.0kg of secondary particle artificial graphite (the medium particle diameter d50 is 16 +/-2 um) for the lithium ion battery is put into a second powder feeder, the second powder feeder is started, the feeding amount is adjusted to be 19.0kg/h, and the secondary particle artificial graphite is fed into a cooling kettle.
(3) And transferring the precursor collected in the cooling kettle to a CVD furnace, and charging acetylene and argon mixed gas to carbonize for 2 hours at the high temperature of 950 ℃.
(4) Mixing the precursor obtained in the step (3) with medium-temperature coal pitch according to the proportion of 90: the 10-ratio mixture was blended for 2h at 1200rpm in the blender.
(5) And (5) transferring the precursor obtained in the step (4) into a roller kiln, heating to 950 ℃ at a speed of 1 ℃/min under the protection of inert gas, preserving heat for 2 hours, naturally cooling to room temperature, and scattering and sieving to obtain a final product.
And (3) electrochemical performance testing:
the preparation method of the electrode comprises the following steps: and mixing the obtained sample, SP and a PVDF solution (the mass concentration of the solution is 8%) dissolved in NMP according to the weight ratio of Powder: PVDF: SP =92.0:6.0:2.0 to obtain slurry, uniformly coating the slurry on a copper foil cleaned by acetone by using a scraper, drying the copper foil in vacuum at 120 ℃ for 12 hours, and then tabletting and cutting to obtain the research electrode.
Performance testing was performed in CR2032 button cells after study electrode fabrication. The battery assembly method is as follows: lithium sheets were used as a counter electrode, Celgard 2300 was used as a separator, and EC-EMC (3: 7) solution containing 1M LiPF6 was used as an electrolyte. During testing, the temperature is room temperature, constant current charging and discharging are adopted, the current density is 0.05C, and the voltage control range is 0.005-2.0V.
FIG. 1 is a scanning electron microscope image of a sample obtained in the present invention, and it can be seen from FIG. 1 that the microstructure of the prepared sample has obvious structural characteristics of silicon-carbon composite material.
FIG. 2 is a graph showing a simulated battery curve obtained after a sample is manufactured into an electrode in the invention, and it can be known from FIG. 2 that a platform curve of silicon is obvious in a 0.2-1.5V interval, the first capacity of the test is 426.3mAh/g, and the first efficiency is 92.5%; the capacity retention rate after 300 cycles of 0.2C is 86%.
The design of the invention is characterized in that: according to the invention, the plasma spraying system is adopted to carry out nanocrystallization on the silicon, so that the expansion characteristic of the material is effectively inhibited, and the cycle performance of the material is improved. CVD is adopted to coat the nano silicon and graphite surfaces to form a conductive carbon layer, and the conductive carbon layer is mechanically fused with a binder and carbonized at high temperature in the later period to improve the first efficiency and the cycle performance of the product. The invention has the greatest characteristic that silicon is nano-sized and uniformly dispersed in graphite, and a stable conductive carbon layer and a coating structure are formed through two coating processes, so that the expansion of the material is effectively inhibited, and the stability of the structure is ensured.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the technical scope of the present invention, so that any minor modifications, equivalent changes and modifications made to the above embodiment according to the technical spirit of the present invention are within the technical scope of the present invention.
Claims (10)
1. A preparation method of a lithium battery silicon-carbon composite material is characterized by comprising the following steps: the method comprises the following steps: sending the coarse silicon powder into a plasma spraying system through a first powder feeder by using inert gas to be evaporated into silicon vapor, sending graphite into a cooling kettle through a second powder feeder by using inert gas, and condensing or depositing the silicon vapor on the graphite in the cooling kettle to form a mixture of nano silicon powder and graphite; and then, conveying the mixture of the nano silicon powder and the graphite into a CVD furnace for vapor deposition carbon coating, conveying the mixture into a fusion machine for fusion with a binder, and then carbonizing the mixture at high temperature through a roller kiln to obtain the silicon-carbon composite material product.
2. The method for preparing a silicon-carbon composite material for a lithium battery according to claim 1, wherein the method comprises the following steps: the coarse silicon powder is one or the combination of high-purity monocrystalline silicon or polycrystalline silicon, and the particle size d50 in the coarse silicon powder is 10-50 mu m.
3. The method for preparing a silicon-carbon composite material for a lithium battery according to claim 1, wherein the method comprises the following steps: the inert gas is any one or the combination of at least two of high-purity nitrogen, argon, helium, xenon, neon or krypton.
4. The method for preparing a silicon-carbon composite material for a lithium battery according to claim 1, wherein the method comprises the following steps: the feeding amount of the first powder feeder is 1-10 kg/h.
5. The method for preparing a silicon-carbon composite material for a lithium battery according to claim 1, wherein the method comprises the following steps: the pressure of the inert gas input into the plasma spraying system is 0.5-0.8mPa, and the pressure of the hydrogen input into the plasma spraying system is 0.05-0.5 mPa.
6. The method for preparing a silicon-carbon composite material for a lithium battery according to claim 1, wherein the method comprises the following steps: the graphite is one or more of secondary particle natural graphite or artificial graphite; the particle size d50 of the graphite is 10-20 μm, and the graphite feeding amount of the second powder feeder is 10-200 kg/h.
7. The method for preparing a silicon-carbon composite material for a lithium battery as claimed in claim 1, wherein the method comprises the steps of: the coating gas input by the CVD furnace is a mixed gas composed of argon and any one or at least two of methane, ethane, propane, ethylene, propylene or acetylene, the coating temperature is 800-1200 ℃, and the coating time is 2-20 h.
8. The method for preparing a silicon-carbon composite material for a lithium battery according to claim 1, wherein the method comprises the following steps: the binder is one or more of petroleum asphalt, coal asphalt and polycondensation resin; the binder accounts for 3-30% of the mixture by mass percent; the petroleum asphalt and/or the coal asphalt are molten petroleum asphalt and/or coal asphalt; the polycondensation resin is one or more of phenolic resin, epoxy resin, acrylic resin, furfural resin and polyester resin; the rotating speed of the fusion machine is 800-; the fusion time of the fusion machine is 0.5-5 h.
9. The method for preparing a silicon-carbon composite material for a lithium battery according to claim 1, wherein the method comprises the following steps: the heating rate of the roller kiln is preferably 0.5-20 ℃/min, and the upper limit temperature of the roller kiln is 900-.
10. A lithium battery silicon-carbon composite material is characterized in that: the silicon-carbon composite material for the lithium battery, which is prepared by the method for preparing the silicon-carbon composite material for the lithium battery as claimed in any one of claims 1 to 9.
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| CN112259740B (en) * | 2020-10-28 | 2021-08-17 | 惠州市竤泰科技有限公司 | Dendritic silicon-carbon composite negative electrode material of lithium battery and preparation method |
| CN112520741A (en) * | 2020-11-26 | 2021-03-19 | 宁波广新纳米材料有限公司 | Production method of carbon-coated silicon powder for lithium battery negative electrode material |
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| CN102850087B (en) * | 2012-09-29 | 2014-10-29 | 西安超码科技有限公司 | Method for preparing silicon carbide coating on graphite surface |
| CN102910630B (en) * | 2012-10-15 | 2014-07-02 | 江苏博迁新材料有限公司 | Production method of nano silicon powder |
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