CN112164779B - Carbon-coated silicon-based negative electrode material and preparation method thereof - Google Patents
Carbon-coated silicon-based negative electrode material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a carbon-coated silicon-based negative electrode material and a preparation method thereof. The preparation method comprises the following steps: and uniformly mixing a lithium source and a silicon source, heating the mixture under an inert atmosphere to perform a pre-lithiation reaction, adding an organic carbon source, continuously heating the mixture to perform high-temperature calcination, and not cooling the mixture in the process from the pre-lithiation reaction to the high-temperature calcination to obtain the carbon-coated silicon-based negative electrode material. The preparation method of the invention effectively relieves the expansion of silicon, and subsequently improves the conductivity of lithium silicate by coating the carbon layer on the surface of the lithium silicate, and simultaneously can avoid potential safety hazard caused by the contact of lithium or lithium alloy and water. The carbon-coated silicon-based negative electrode material prepared by the method has the characteristics of high capacity, high first charge-discharge efficiency, high energy density and excellent cycle performance.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a carbon-coated silicon-based negative electrode material and a preparation method thereof.
Background
With the increasing global resource crisis and the environmental pollution problem, the utilization of renewable energy is more and more emphasized. Clean and efficient energy storage technology is a necessary way to realize renewable energy utilization. Lithium ion batteries are currently widely used in portable electronic devices and electric vehicles as an advanced energy storage device.
The current research on lithium ion batteries mainly focuses on the improvement of energy density, and silicon negative electrode materials are concerned due to the higher theoretical specific capacity (4200 mAh/g). However, the abrupt change in volume (300%) during electrochemical cycling can cause gradual pulverization of the silicon negative electrode material during cycling, resulting in structural collapse, eventually leading to detachment of the active species from the current collector, and significant degradation of cycling capacity.
Compared with a silicon negative electrode, the silicon oxide (SiOx) can effectively buffer the volume expansion in the circulation process due to the generation of lithium oxide and lithium silicate in the lithium intercalation process, and meanwhile, the silicon oxide has lower cost and is a very competitive negative electrode material. The volume expansion of the silicon monoxide still has about 200% in a fully lithiated state, and the cycle performance of the silicon monoxide can be effectively improved by reducing the particle size or increasing a carbon coating layer; however, the first charge-discharge efficiency of the improved silica by the above method is still low due to the formation of irreversible products during the first lithium intercalation. The pre-lithiation treatment of the silicon protoxide material can effectively compensate lithium loss in the material and improve the first charge-discharge efficiency of the material, but the metal lithium or lithium alloy generated after the conventional pre-lithiation treatment can generate potential safety hazard when contacting with water in the battery preparation process.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and shortcomings in the background art and provide a carbon-coated silicon-based negative electrode material and a preparation method thereof.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a preparation method of a carbon-coated silicon-based negative electrode material comprises the following steps:
and uniformly mixing a lithium source and a silicon source, heating the mixture under an inert atmosphere to perform a pre-lithiation reaction, adding an organic carbon source, continuously heating the mixture to perform high-temperature calcination, and not cooling the mixture in the process from the pre-lithiation reaction to the high-temperature calcination to obtain the carbon-coated silicon-based negative electrode material.
In the preparation method, preferably, the temperature of the prelithiation reaction is 700-; the high-temperature calcination temperature is 800-1200 ℃, and the time is 1.5-2.5 h; the heating rate is 3-10 deg.C/min.
In the above preparation method, preferably, the silicon source is silicon monoxide with a chemical formula of SiOxWherein x is more than or equal to 0.5 and less than or equal to 1.7.
In the above preparation method, preferably, the silicon source further includes a simple substance of silicon and/or a silicon metal alloy.
In the above preparation method, preferably, the lithium source is Li powder, LiOH, Li2O、Li2CO3、LiF、Li2SO4、LiH、Li3N、LiBH4At least one of (1).
In the above preparation method, preferably, the mass of the lithium source accounts for 1-30wt% of the total mass of the lithium source and the silicon source.
In the above preparation method, preferably, the average particle size D50 of the lithium source is 1 to 20 μm, and the average particle size D50 of the silicon source is 1 to 20 μm.
In the above preparation method, preferably, the organic carbon source is at least one of methane, ethane, propane, butane, pentane, isobutane, hexane, ethylene, propylene, butene, acetylene, benzene, toluene and biphenyl.
In the above preparation method, the molar ratio of the organic carbon source to the silicon source is preferably 0.1 to 3. More preferably, the molar ratio of the organic carbon source to the silicon source is 0.1 to 1.
In the above preparation method, preferably, the inert atmosphere is nitrogen and/or argon.
The invention also provides the carbon-coated silicon-based negative electrode material prepared by the preparation method.
Compared with the prior art, the invention has the advantages that:
the preparation method of the invention generates lithium silicate on the surface of the silicon-containing material in situ in advance through the prelithiation reaction, and then takes the silicon oxide/lithium silicate composite material as the core and coats the surface with the carbon layer to improve the conductivity of the lithium silicate. The invention uses stable and cheap lithium compound to complete the pre-lithiation and carbon coating processes in the same reactor, does not need to be heated and cooled repeatedly in the preparation process, effectively controls the disproportionation degree of the silicon monoxide by controlling the reaction temperature and the reaction time of each heating stage in the primary temperature-rising process (the temperature is not required to be reduced after the pre-lithiation), forms a structure that silicon crystal grains (2.5-3.5nm) are embedded into silicon dioxide in the disproportionation process, and ensures that the peripheral silicon dioxide generated by the disproportionation can fully react with a lithium source to generate lithium silicate, thereby effectively relieving the expansion of silicon, and subsequently coats a carbon layer on the surface of the lithium silicate, thereby improving the conductivity of the lithium silicate and avoiding the potential safety hazard generated by the contact of the lithium or lithium alloy and water.
The preparation method of the invention has the advantages of greatly shortened working hours, saved energy consumption, low process cost, strong operability and suitability for large-scale production. The carbon-coated silicon-based negative electrode material prepared by the method has the characteristics of high capacity, high first charge-discharge efficiency, high energy density and excellent cycle performance.
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 introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
Fig. 1 is a charge-discharge cycle curve of a button cell prepared by using the carbon-coated silicon-based negative electrode material in example 1 of the present invention.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
the invention relates to a preparation method of a carbon-coated silicon-based negative electrode material, which comprises the following steps:
lithium carbonate having an average particle diameter D50 of 8 to 10 μm and Silica (SiO) having an average particle diameter D50 of 10 to 15 μm were mixedxAnd x is more than or equal to 0.5 and less than or equal to 1.7) is mixed in a VC machine with the rotating speed of 1000rpm for 30min, the mass of lithium carbonate accounts for 3 wt% of the total mass of lithium carbonate and silicon monoxide, after uniform mixing, the mixture is placed in a reaction furnace, 5L/min of nitrogen is introduced, the temperature is increased to 750 ℃ at the heating rate of 5 ℃/min, stirring is started, the stirring rotating speed is kept at 50rpm, heat is preserved for 1h, then methane gas is introduced, the molar ratio of methane to silicon monoxide is 0.35, the temperature is continuously increased to 1000 ℃ at the heating rate of 5 ℃/min, and high-temperature calcination is carried out for 2h, so that the carbon-coated silicon-based negative electrode material is obtained.
Through tests, the first charge-discharge cycle curve of the button cell prepared from the carbon-coated silicon-based anode material is shown in fig. 1, and it can be seen from the graph that the first charge specific capacity of the button cell prepared from the carbon-coated silicon-based anode material of the embodiment is 1103.2mAh/g, the first charge-discharge efficiency is 77.45%, and the capacity retention rate is 83% after 300 cycles.
Example 2:
the invention relates to a preparation method of a carbon-coated silicon-based negative electrode material, which comprises the following steps:
lithium carbonate having an average particle diameter D50 of 15 μm and Silica (SiO) having an average particle diameter D50 of 12 μm were mixedxX is more than or equal to 0.5 and less than or equal to 1.7) planetary ball with rotating speed of 800rpmBall-milling for 5h in a mill, wherein the mass of lithium carbonate accounts for 10 wt% of the total mass of lithium carbonate and silicon monoxide, uniformly mixing, placing the mixture in a reaction furnace, introducing 5L/min of argon, raising the temperature to 750 ℃ at the temperature rise rate of 5 ℃/min, carrying out pre-lithiation reaction for 1h, subsequently introducing acetylene gas, keeping the molar ratio of acetylene to silicon monoxide at 0.2, continuing to raise the temperature to 1200 ℃ at the temperature rise rate of 5 ℃/min, and carrying out high-temperature calcination for 2h to obtain the carbon-coated silicon-based negative electrode material.
Through tests, the button cell prepared from the carbon-coated silicon-based negative electrode material has the specific first charge capacity of 1296.2mAh/g, the first charge-discharge efficiency of 73.22% and the capacity retention rate of 84.5% after 300 cycles.
Example 3:
the invention relates to a preparation method of a carbon-coated silicon-based negative electrode material, which comprises the following steps:
lithium oxide having an average particle diameter D50 of 12 μm and Silica (SiO) having an average particle diameter D50 of 10 μmxX is more than or equal to 0.5 and less than or equal to 1.7) are evenly mixed in a double-cone mixer with the rotating speed of 800rpm, the mass of lithium oxide accounts for 5 wt% of the total mass of lithium oxide and silicon monoxide, the mixture is placed in a reaction furnace, 5L/min of argon is introduced, the temperature is increased to 900 ℃ at the temperature rising rate of 5 ℃/min, pre-lithiation reaction is carried out for 1h, then ethane gas is introduced, the molar ratio of ethane to silicon monoxide is 0.2, the temperature is continuously raised to 1100 ℃ at the temperature rising rate of 5 ℃/min, the pressure of the reaction furnace is kept at 1bar, high-temperature calcination is carried out for 1.5h, after natural cooling, the distance is released, and magnetism is removed, and the carbon-coated silicon-based negative electrode material is obtained.
Through tests, the button cell prepared from the carbon-coated silicon-based anode material has the specific first charge capacity of 1378.6mAh/g, the first charge-discharge efficiency of 77.59% and the capacity retention rate of 83.8% after 300 cycles.
Comparative example 1:
a preparation method of a silicon-based negative electrode material comprises the following steps:
lithium hydroxide having an average particle diameter D50 of 8 μm and Silica (SiO) having an average particle diameter D50 of 10 μm were mixedxX is more than or equal to 0.5 and less than or equal to 1.7) is mixed for 30min in a VC machine with the rotating speed of 1000rpm, and the mass of lithium carbonate accounts for lithium hydroxide and lithium oxide3 wt% of the total weight of the silicon, uniformly mixing, placing the mixture in a reaction furnace, introducing 5L/min of nitrogen, raising the temperature to 750 ℃ at the heating rate of 5 ℃/min, carrying out pre-lithiation reaction for 1h, and after natural cooling, carrying out gapping and demagnetizing to obtain the silicon-based negative electrode material.
Through tests, the button cell prepared from the silicon-based negative electrode material of the comparative example has the first charging specific capacity of 778.2mAh/g, the first charging and discharging efficiency of 68.32 percent and the capacity retention rate of 21.1 percent after 30 cycles.
Comparative example 2:
a preparation method of a silicon-based negative electrode material comprises the following steps:
silica (SiO) having an average particle diameter D50 of 10 μmxX is more than or equal to 0.5 and less than or equal to 1.7) is placed in a reaction furnace, 5L/min of nitrogen is introduced, the temperature is raised to 1000 ℃ at the heating rate of 5 ℃/min, the calcination is carried out for 1h, then ethane gas is introduced, the molar ratio of methane to silicon monoxide is 0.2, the temperature is continuously raised to 1200 ℃ at the heating rate of 5 ℃/min, the high-temperature calcination is carried out for 1.5h, and after the natural cooling, the silicon-based negative electrode material is obtained through spacing and demagnetization.
Through tests, the button cell prepared from the silicon-based negative electrode material of the comparative example has the first charging specific capacity of 1256.4mAh/g, the first charging and discharging efficiency of 68.26 percent and the capacity retention rate of 81.2 percent after 300 weeks of circulation.
Comparative example 3:
a preparation method of a silicon-based negative electrode material comprises the following steps:
lithium carbonate having an average particle diameter D50 of 8 to 10 μm and Silica (SiO) having an average particle diameter D50 of 10 to 15 μm were mixedxX is more than or equal to 0.5 and less than or equal to 1.7) is mixed for 30min in a VC machine with the rotating speed of 1000rpm, the mass of lithium carbonate accounts for 3 wt% of the total mass of lithium carbonate and silicon monoxide, after uniform mixing, the mixture is placed in a reaction furnace, 5L/min of nitrogen is introduced, the temperature is increased to 750 ℃ at the temperature rising rate of 5 ℃/min, stirring is started, the stirring rotating speed is kept at 50rpm, and heat preservation is carried out for 1 h; naturally cooling, discharging, sieving with 325 mesh sieve, placing the sieved material in a reaction furnace, heating to 1000 deg.C at a heating rate of 5 deg.C/min, introducing 5L/min of nitrogen and methane gas with a molar ratio of methane to silicon monoxide of 0.35, and calcining at high temperature for 2 hr to obtain the final productTo carbon-coated silicon-based cathode materials.
Through tests, the button cell prepared from the silicon-based negative electrode material of the comparative example has the first charge specific capacity of 1306.2mAh/g, the first charge-discharge efficiency of 71.28 percent and the capacity retention rate of 61.2 percent after 300 cycles.
Claims (8)
1. A preparation method of a carbon-coated silicon-based negative electrode material is characterized by comprising the following steps:
uniformly mixing a lithium source and a silicon source, heating the mixture under an inert atmosphere to perform a pre-lithiation reaction, adding an organic carbon source, continuously heating the mixture to perform high-temperature calcination, and not cooling the mixture in the process from the pre-lithiation reaction to the high-temperature calcination to obtain the carbon-coated silicon-based negative electrode material;
the temperature of the pre-lithiation reaction is 700-1000 ℃, and the time is 0.5-5 h; the high-temperature calcination temperature is 800-1200 ℃, and the time is 1.5-2.5 h; the heating rate is 3-10 ℃/min;
the silicon source is silicon monoxide with the chemical formula of SiOxWherein x is more than or equal to 0.5 and less than or equal to 1.7.
2. The method according to claim 1, wherein the lithium source is Li powder, LiOH, Li2O、Li2CO3、LiF、Li2SO4、LiH、Li3N、LiBH4At least one of (1).
3. The method according to claim 1, wherein the mass of the lithium source is 1 to 30wt% based on the total mass of the lithium source and the silicon source.
4. The method according to claim 1, wherein the average particle size D50 of the lithium source is 1 to 20 μm, and the average particle size D50 of the silicon source is 1 to 20 μm.
5. The method according to claim 1, wherein the organic carbon source is at least one of methane, ethane, propane, butane, pentane, isobutane, hexane, ethylene, propylene, butene, acetylene, benzene, toluene, and biphenyl.
6. The method according to claim 1, wherein the molar ratio of the organic carbon source to the silicon source is 0.1 to 3.
7. The method according to claim 1, wherein the inert atmosphere is nitrogen and/or argon.
8. A carbon-coated silicon-based negative electrode material prepared according to the preparation method of any one of claims 1 to 7.
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| CN113023738A (en) * | 2021-03-03 | 2021-06-25 | 昆山宝创新能源科技有限公司 | Silicon-based composite material, preparation method thereof and battery |
| CN113066972B (en) * | 2021-03-19 | 2022-06-17 | 厦门高容新能源科技有限公司 | Lithium-supplementing silicon material, preparation method thereof, electrode containing lithium-supplementing silicon material and battery |
| CN113314703B (en) * | 2021-05-28 | 2022-05-17 | 蜂巢能源科技有限公司 | Negative electrode material and preparation method and application thereof |
| CN114023948B (en) * | 2021-10-29 | 2023-03-03 | 合肥国轩高科动力能源有限公司 | Silicon-carbon negative electrode material, preparation method thereof and lithium ion battery |
| CN114388738B (en) * | 2021-12-29 | 2024-01-02 | 湖北亿纬动力有限公司 | Silicon-based anode material and preparation method and application thereof |
| CN114551872B (en) * | 2022-01-19 | 2024-02-27 | 惠州市豪鹏科技有限公司 | Negative electrode material, preparation method thereof, battery negative electrode and battery |
| CN114744166A (en) * | 2022-02-25 | 2022-07-12 | 深圳市翔丰华科技股份有限公司 | Preparation method of pre-lithiated silica composite material |
| CN114524436B (en) * | 2022-02-28 | 2023-11-17 | 长沙矿冶研究院有限责任公司 | Modified silicon-oxygen anode material precursor and preparation method thereof |
| JP2023151923A (en) * | 2022-04-01 | 2023-10-16 | 信越化学工業株式会社 | Negative electrode active material and manufacturing method thereof |
| CN114975967A (en) * | 2022-06-29 | 2022-08-30 | 宁波杉杉新材料科技有限公司 | Pre-lithiated silica composite material, preparation method thereof, negative pole piece, battery and application |
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