CN114180548A - Preparation method of silicon-carbon composite negative electrode material and lithium storage application - Google Patents
Preparation method of silicon-carbon composite negative electrode material and lithium storage application Download PDFInfo
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- C01B32/00—Carbon; Compounds thereof
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- H01M4/362—Composites
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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
- 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
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- 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
Abstract
The invention belongs to the technical field of composite materials, and particularly relates to a preparation method of a silicon-carbon composite anode material, which comprises the following steps: ball-milling silkworm excrement and waste silicon powder respectively, mixing the silkworm excrement and the waste silicon powder with an acid solution in proportion, ultrasonically stirring, centrifugally drying, and calcining the waste silicon; and (3) ultrasonically treating the pretreated carbon material, silicon powder and deionized water according to the proportion of 1mg: 1-10 mg: 0.1-0.5 mL for 20-50 min, transferring the pretreated carbon material, silicon powder and deionized water into a reaction kettle for hydrothermal reaction for 6-12 h at the temperature of 150-200 ℃, cooling to room temperature, washing, centrifuging, precipitating, drying, grinding, and calcining for 1-5 h at the temperature of 500-900 ℃ in an inert atmosphere to obtain the carbon material. According to the invention, the silicon-carbon precursor is prepared into the negative electrode material by adopting waste silicon and silkworm excrement through a hydrothermal method, doping is not required, the reaction condition is simple, the used material is low in price, and the negative electrode material is non-toxic and harmless, and the synthesized negative electrode material has high reversible specific capacity, rate capability, cycle performance and long cycle life, and is beneficial to meeting the actual demand.
Description
Technical Field
The invention belongs to the technical field of composite materials, relates to a composite electrode material, and particularly relates to a preparation method of a silicon-carbon composite negative electrode material and application of lithium storage.
Background
With the rapid development of clean energy, all countries actively promote the application of renewable energy, the development of the solar industry is rapid, and a large amount of waste materials and resources of solar crystalline silicon cutting are wasted. In the field of recycling of solar crystalline silicon cutting waste materials, a purification recycling mode is mostly adopted, but the purification process is complex, the energy consumption is high, and the recovery rate is low, so that a novel recycling method is very necessary for treating the crystalline silicon cutting waste materials.
The silicon can be used as the negative electrode material of the lithium ion battery, the theoretical specific capacity of the silicon is about ten times of that of the current commercial carbon, and the maximum specific capacity reaches 4200mAh g-1. However, silicon undergoes a large volume expansion (about 300%) during the charging and discharging processes, resulting in poor electrochemical cycling stability and seriously affecting the service life of the battery. The carbon material, which is one of the lithium ion negative electrode materials, has good cycle stability and excellent conductivity with small volume change during charge and discharge. Therefore, the volume expansion of silicon during charge and discharge can be effectively slowed down through carbon coating. In the current silicon-carbon composite cathode material, the carbon material is mainly prepared by organic substances such as fossil fuel and the like, and the preparation process has strict processing conditions and higher cost. The carbon material of the biomass in the nature has the advantages of specific structure, high carbon content, large specific surface area, excellent conductivity, wide and renewable sources, low price, environmental protection and the like. Through pretreatment and carbonization in an inert gas atmosphere, the biomass carbon-based material in the flaky silicon-carbon composite material has high specific surface area and many active sites. Based on the characteristics, the biomass is used as a precursor of the carbon material, has higher advantages, is improved into an electrode material with good performance through a simple process, and has market value.
Disclosure of Invention
In order to solve the existing problems, the invention aims to provide a preparation method of a low-cost and environment-friendly silicon-carbon composite negative electrode material.
Technical scheme
A preparation method of a silicon-carbon composite negative electrode material comprises the following steps:
A. ball-milling a carbon source precursor for 1-5 h, wherein the ball/solid mass ratio is 10-20: 1, the rotating speed is 200-1000 r/min, preparing a powder carbon source, carrying out acid washing, the leaching temperature is 15-25 ℃, the leaching time is 3-12 h, the mass ratio of the volume of a leaching solution to the mass of the powder carbon source is 20-200 mL:1g, and the stirring speed is 100-500 r/min; washing the carbon source after acid washing with deionized water to be neutral, and carrying out vacuum drying for 3-12 h at 50-100 ℃ to obtain a pretreated carbon material;
B. ball-milling the silicon source precursor, wherein the ball/solid mass ratio is 10-20: 1, acid-washing the waste silicon after ball-milling, the leaching temperature is 15-25 ℃, the leaching time is 3-12 h, the mass ratio of the volume of the leaching solution to the cutting waste is 20-200 mL:1g, and the stirring speed is 100-500 r/min; drying and grinding the waste silicon after pickling and water washing, and calcining the obtained powder for 1-5 hours at 500-900 ℃ in an inert atmosphere to obtain pretreated silicon powder;
C. and (3) uniformly mixing the pretreated carbon material, silicon powder and deionized water according to the proportion of 1mg: 1-10 mg: 0.1-0.5 mL by ultrasonic treatment for 20-50 min, transferring the mixture into a reaction kettle for hydrothermal reaction at 150-200 ℃ for 6-12 h, cooling to room temperature, washing with water, centrifuging, precipitating, drying, grinding, heating the room temperature to 500-900 ℃ in a tubular furnace in an inert atmosphere, calcining for 1-5 h, and preferably calcining for 2h at 700 ℃ to obtain the catalyst.
In the preferred embodiment of the invention, the carbon source precursor in the step A is a biomass carbon source, preferably silkworm excrement.
In a preferred embodiment of the invention, the silicon source precursor in the step B is crystalline silicon cutting waste silicon.
In the preferred embodiment of the invention, the pickling solution in the step A/B is hydrochloric acid or nitric acid with the mass fraction of 5-15%.
In the preferred embodiment of the invention, the inert gas in the step B/C is argon or nitrogen.
In the preferred embodiment of the invention, the carbonization in the step B/C is carried out by using a tubular furnace or a box furnace, and the heating rate is 2-15 ℃ per minute-1。
The silicon-carbon composite negative electrode material prepared by the method is applied to a lithium ion battery negative electrode.
The lithium ion battery negative electrode material is prepared from a silicon-carbon composite material, and further, negative electrode slurry consisting of the negative electrode active material, a conductive agent, a binder and a solvent in a mass ratio of 8:1:1 is coated on a metal copper foil by using an automatic coating machine, and the lithium ion battery negative electrode material is obtained after drying, wherein the negative electrode active material is the silicon-carbon composite material; the conductive agent is Ketjenblack EC-600 JD; the dispersant is N-methyl pyrrolidone (NMP); the binder is oily binder polyvinylidene fluoride (PVDF).
Further, the lithium ion battery negative electrode material obtained above was put in a glove box with a lithium sheet as a counter electrode and lithium hexafluorophosphate (LiPF)6) The electrolyte is Celgerd 2400 is a diaphragm, a half cell is assembled, and the rate performance and the cycle performance of the half cell are tested under different current densities in a potential window of 0.01-1.5V.
In published documents, silicon carbon is used for energy storage application, for example, chinese patent publication No. CN 112259719 a discloses a method for comprehensively recovering waste photovoltaic modules and preparing silicon carbon cathode materials, which focuses on removing surface impurities, uses chemical substances such as HF, metal salts and alcohols in the impurity removal process, and has the disadvantages of various reagents, long preparation process and increased treatment cost; chinese patent publication No. CN 113488640 a discloses a method for preparing a silicon-carbon negative electrode material, in which biomass carbon is used to coat nano-silicon, which improves the cycle performance, but the cost of the nano-silicon powder is high; these synthetic processes are complex and expensive, and biomass carbon materials generally exhibit low lithium storage capacity at higher current densities. The method for compounding the crystalline silicon cutting waste and the biomass carbon source is simple, low in price and environment-friendly, effectively avoids the problem that silicon is difficult to purify and reuse, and the biomass silkworm excrement carbon source is of a sheet structure and has high aspect ratio and electrical conductivity. High value-added utilization of waste silicon and silkworm excrement is realized, and meanwhile, the obtained experimental result shows that the prepared silicon-carbon composite material has excellent rate capability and cycle stability.
Advantageous effects
According to the invention, the silicon-carbon composite negative electrode material is prepared from the waste silicon and silkworm excrement derived carbon by a hydrothermal method, doping is not required, the reaction condition is simple, the used precursor is low in price, and the silicon-carbon composite negative electrode material is non-toxic and harmless, meets the environment-friendly requirement, and has a wide application prospect. The silicon-carbon composite material prepared by the invention has higher rate performance and long cycle life, and is beneficial to meeting the actual requirement. The silicon-carbon composite material prepared by the invention has good application prospect in lithium ion batteries, both of which have the characteristics of low price and environment-friendly material, and have higher multiplying power and cycle performance, and can be used as a cathode material of an energy storage device of the lithium ion battery.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) of a silicon carbon composite negative electrode material, wherein (a) is obtained in example 1 and (b) is obtained in example 2;
FIG. 2 is an X-ray powder diffraction pattern (XRD) of a silicon carbon composite anode material prepared for example 1(a), example 2(b), and example 3 (c);
FIG. 3 is a Raman spectrum (Raman) of the Si-C composite negative electrode material prepared in example 1;
FIG. 4 is a graph of rate and cycle performance of a silicon carbon composite anode material after use in a lithium ion battery, wherein (a) is obtained for example 1, (b) is obtained for example 2, and (c) is obtained for example 3.
Detailed Description
The present invention will be described in detail below with reference to examples to enable those skilled in the art to better understand the present invention, but the present invention is not limited to the following examples.
Example 1
A preparation method of a silicon-carbon composite material comprises the following steps: respectively placing 300mg of pretreated faeces Bombycis and 600mg of pretreated waste silicon in 50mL hydrothermal kettle, adding 30mL deionized water, placing in ultrasonic instrument, ultrasonic treating for 30min to mix them uniformly, and compounding by hydrothermal method at 6h and 180 deg.CWashing the carbon/waste silicon composite material solution with water, centrifuging, drying, collecting solids, grinding, and adding N2Calcining the sample in a tube furnace under the atmosphere, heating the sample to 700 ℃ from room temperature, and preserving the temperature for 2h to obtain the biomass carbon source (silkworm excrement)/waste silicon composite material.
The prepared silicon-carbon composite material is used as a working electrode, a commercial lithium sheet is used as a counter electrode, and an electrolyte is LiPF6For the electrolyte, Celgard 2500 is the separator, and the button cell is assembled for electrochemical performance test.
It can be seen from fig. 1(a) that the particle size of the prepared silicon-carbon composite electrode material is in the micrometer scale.
The position and relative intensity of the contrast diffraction peak in FIG. 2(a) are matched with JPCDS (27-1402) card, and the product is shown to be a silicon-carbon composite electrode material.
The peaks of silicon and carbon are observed in the raman spectrum of fig. 3, which also represents the degree of disordering of the carbon, indicating that the product is a silicon carbon composite.
The test results in FIG. 4(a) show that the Si-C composite electrode material is at 0.1A g-1、0.25A·g-1、0.5A·g-1、1A·g-1、0.1A·g-1The reversible capacity of the material reaches 450mAh g after 100 cycles of charge and discharge under the multiplying power of-1。
Example 2
A preparation method of a silicon-carbon composite material comprises the following steps: respectively placing 300mg of pretreated silkworm excrement and 300mg of pretreated waste silicon in a 50mL hydrothermal kettle, adding 30mL deionized water, placing in an ultrasonic instrument, performing ultrasonic treatment for 30min to uniformly mix, compounding by a hydrothermal method, wherein the hydrothermal condition is 6h and 180 ℃, washing and centrifuging the hydrothermal silkworm excrement derived carbon/waste silicon composite material solution, drying, collecting solids, grinding, and performing N-phase hydrothermal treatment2Calcining a sample in a tube furnace under the atmosphere, heating the sample to 700 ℃ from room temperature, and preserving the temperature for 2 hours to obtain the biomass carbon source (silkworm excrement)/waste silicon composite material.
The prepared silicon-carbon composite material is used as a working electrode, a commercial lithium sheet is used as a counter electrode, and an electrolyte is LiPF6Assembling the button cell for electrochemical by using Celgard 2500 as a separator as electrolyteAnd (5) testing the performance.
As can be seen from fig. 1(b), the particle size of the prepared silicon-carbon composite electrode material is in the micrometer scale.
The position and relative intensity of the contrast diffraction peak in FIG. 2(b) are matched with JPCDS (27-1402) card, and the product is shown to be a silicon-carbon composite electrode material.
The test results in FIG. 4(b) show that the Si-C composite electrode material is at 0.1A g-1、0.25A·g-1、0.5A·g-1、1A·g-1、0.1A·g-1The reversible capacity of the material reaches 400 mAh.g after 30 cycles of charge and discharge under the multiplying power of-1。
Example 3
A preparation method of a silicon-carbon composite material comprises the following steps: respectively placing 300mg of pretreated silkworm excrement and 600mg of pretreated waste silicon in a 50mL hydrothermal kettle, adding 35mL deionized water, placing in an ultrasonic instrument, performing ultrasonic treatment for 40min to uniformly mix, compounding by a hydrothermal method, wherein the hydrothermal condition is 12h and 180 ℃, washing and centrifuging the hydrothermal silkworm excrement derived carbon/waste silicon composite material solution, drying, collecting solids, grinding, and performing N-phase hydrothermal treatment2Calcining the sample in a tube furnace under the atmosphere, heating the sample to 700 ℃ from room temperature, and preserving the temperature for 2h to obtain the biomass carbon source (silkworm excrement)/waste silicon composite material.
The prepared silicon-carbon composite material is used as a working electrode, a commercial lithium sheet is used as a counter electrode, and an electrolyte is LiPF6For the electrolyte, Celgard 2500 is the separator, and the button cell is assembled for electrochemical performance test.
The position and relative intensity of the contrast diffraction peak in FIG. 2(c) are matched with JPCDS (27-1402) card, and the product is shown to be a silicon-carbon composite electrode material.
The test results in FIG. 4(c) show that the Si-C composite electrode material is at 0.1A g-1、0.25A·g-1、0.5A·g-1、1A·g-1、0.1A·g-1The reversible capacity of the material reaches 820mAh g after 40 cycles of charge and discharge at the multiplying power of-1。
Example 4
Preparation method of silicon-carbon composite material and packageComprises the following steps: respectively placing 300mg of pretreated silkworm excrement and 450mg of pretreated waste silicon in a 50mL hydrothermal kettle, adding 30mL deionized water, placing in an ultrasonic instrument, performing ultrasonic treatment for 50min to uniformly mix, compounding by a hydrothermal method, wherein the hydrothermal conditions are 12h and 160 ℃, washing and centrifuging the hydrothermal silkworm excrement derived carbon/waste silicon composite material solution, drying, collecting solids, grinding, and performing N-phase hydrothermal treatment2Calcining the sample in a tube furnace under the atmosphere, heating the sample to 800 ℃ from room temperature, and preserving the temperature for 2.5 hours to obtain the biomass carbon source (silkworm excrement)/waste silicon composite material.
The prepared silicon-carbon composite material is used as a working electrode, a commercial lithium sheet is used as a counter electrode, and an electrolyte is LiPF6For electrolyte, Celgard 2500 is a diaphragm, and the electrochemical performance test is carried out on the assembled button cell at 0.1 A.g-1、0.25A·g-1、0.5A·g-1、1A·g-1、0.1A·g-1The reversible capacity of the material reaches 510mAh g after 100 cycles of charge and discharge under the multiplying power of-1。
Example 5
A preparation method of a silicon-carbon composite material comprises the following steps: respectively placing 300mg of pretreated silkworm excrement and 300mg of pretreated waste silicon in a 50mL hydrothermal kettle, adding 30mL deionized water, placing in an ultrasonic instrument, performing ultrasonic treatment for 30min to uniformly mix, compounding by a hydrothermal method, wherein the hydrothermal condition is 8h and 180 ℃, washing and centrifuging the hydrothermal silkworm excrement derived carbon/waste silicon composite material solution, drying, collecting solids, grinding, and performing N-phase hydrothermal treatment2Calcining a sample in a tube furnace under the atmosphere, heating the sample to 700 ℃ from room temperature, and preserving the temperature for 2 hours to obtain the biomass carbon source (silkworm excrement)/waste silicon composite material.
The prepared silicon-carbon composite material is used as a working electrode, a commercial lithium sheet is used as a counter electrode, and an electrolyte is LiPF6For electrolyte, Celgard 2500 is a diaphragm, and the electrochemical performance test is carried out on the assembled button cell at 0.1 A.g-1、0.25A·g-1、0.5A·g-1、1A·g-1、0.1A·g-1The reversible capacity of the material reaches 480mAh g after 100 cycles of charge and discharge under the multiplying power of-1。
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present invention or directly or indirectly applied to other related technical fields are included in the scope of the present invention.
Claims (10)
1. The preparation method of the silicon-carbon composite negative electrode material is characterized by comprising the following steps of:
A. ball-milling a carbon source precursor for 1-5 h, wherein the ball/solid mass ratio is 10-20: 1, the rotating speed is 200-1000 r/min, preparing a powder carbon source, leaching at 15-25 ℃ for 3-12 h in acid washing, the ratio of the volume of a leaching solution to the mass of the powder carbon source is 20-200 mL:1g, and the stirring speed is 100-500 r/min; washing the carbon source after acid washing with deionized water to be neutral, and carrying out vacuum drying for 3-12 h at 50-100 ℃ to obtain a pretreated carbon material;
B. ball-milling the silicon source precursor, wherein the ball/solid mass ratio is 10-20: 1, acid-washing the waste silicon after ball-milling, the leaching temperature is 15-25 ℃, the leaching time is 3-12 h, the mass ratio of the volume of the leaching solution to the cutting waste is 20-200 mL:1g, and the stirring speed is 100-500 r/min; drying and grinding the waste silicon after pickling and water washing, and calcining the obtained powder for 1-5 hours at 500-900 ℃ in an inert atmosphere to obtain pretreated silicon powder;
C. and (3) ultrasonically mixing the pretreated carbon material, silicon powder and deionized water according to the proportion of 1mg: 1-10 mg: 0.1-0.5 mL for 20-50 min, transferring the mixture into a reaction kettle for hydrothermal reaction at 150-200 ℃ for 6-12 h, cooling to room temperature, washing with water, centrifuging, precipitating, drying, grinding, and heating from room temperature to 500-900 ℃ in an inert atmosphere for calcining for 1-5 h to obtain the carbon material.
2. The method for preparing a silicon-carbon composite anode material according to claim 1, wherein: and B, the carbon source precursor in the step A is a biomass carbon source.
3. The method for preparing a silicon-carbon composite anode material according to claim 1, wherein: and the carbon source precursor in the step A is silkworm excrement.
4. The method for preparing a silicon-carbon composite anode material according to claim 1, wherein: and in the step B, the silicon source precursor is crystalline silicon cutting waste silicon.
5. The method for preparing a silicon-carbon composite anode material according to claim 1, wherein: the pickling solution in the step A or B is hydrochloric acid or nitric acid with the mass fraction of 5-15%.
6. The method for preparing a silicon-carbon composite anode material according to claim 1, wherein: and in the step B or C, the inert gas is argon or nitrogen.
7. The method for preparing a silicon-carbon composite anode material according to claim 1, wherein: and C, heating the mixture from room temperature to 700 ℃ in an inert atmosphere, and calcining the mixture for 2 hours.
8. The method for preparing a silicon-carbon composite anode material according to claim 1, wherein: and C, calcining, wherein the used equipment is a tubular furnace or a box furnace, and the heating rate is 2-15 ℃ per minute-1。
9. The silicon-carbon composite negative electrode material prepared by the preparation method according to any one of claims 1 to 8.
10. The use of the silicon-carbon composite anode material according to claim 8, wherein: the material is applied to the negative electrode material of the lithium ion battery.
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