CN118026181A - Induction thermal plasma in-situ synthesis method of silicon-carbon nanocomposite for lithium ion battery anode material - Google Patents
Induction thermal plasma in-situ synthesis method of silicon-carbon nanocomposite for lithium ion battery anode material Download PDFInfo
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Abstract
An induction thermal plasma in-situ synthesis method of a silicon-carbon nanocomposite for a lithium ion battery cathode material belongs to the field of lithium ion batteries. The sectional feeding mode is adopted, and the formation of silicon nanowires and the temperature zone of the carbon-silicon composite process are controlled, so that the reaction speed of carbon and silicon is restrained, and the formation of silicon carbide is effectively avoided; firstly, axially conveying a silicon source precursor into an induction thermal plasma high-temperature region, obtaining silicon vapor under the action of high temperature, cooling in the process of leaving the high-temperature region, and obtaining a silicon nanowire through nucleation growth; adding gas carbon sources such as acetylene, methane and the like into the tail part of the induction thermal plasma arc, and carrying out heterogeneous nucleation on the silicon surface by carbon formed by pyrolysis to obtain the silicon-carbon composite material. Solves the problems of uneven coating of the carbon layer, easy oxidation of the nano material, and the like.
Description
Technical Field
The invention belongs to the field of lithium ion batteries, and relates to an induction thermal plasma in-situ synthesis method of a silicon-carbon nanocomposite for a lithium ion battery negative electrode material.
Background
The explosive growth of electronic devices, automobiles and large-scale energy storage devices has placed higher demands on lithium ion battery energy density and cycle life. The silicon has high theoretical specific capacity (4200 mAh/g), low cost and rich reserve, and is the most promising cathode material for the next generation of lithium ion batteries. However, silicon anodes tend to cause severe volume expansion during cycling of lithium ion batteries, resulting in loss of electrolyte and capacity decay. In addition, the conductivity of silicon serving as a semiconductor is far lower than that of a graphite material, so that the transmission of lithium ions in the silicon negative electrode is seriously influenced, and the effective performance of the silicon negative electrode is greatly restricted.
In order to increase the structural stability and conductivity of silicon materials, the most common methods of improvement include nanocrystallization and material compounding. The research shows that the nano wire can release stress efficiently through axial expansion and contraction, inhibit the growth and the propagation of cracks, thus being capable of tolerating larger volume change and reducing damage to an electrode structure. In addition, nanowires can also provide fast electron and ion transport pathways in the axial direction, increasing the electrochemical reaction rate. Further, silicon and a carbon material are compounded, and the transfer and the transmission of charges are promoted by utilizing good conductivity of carbon, so that the rate capability of the battery can be effectively improved. Carbon can also serve as a buffer body, so that the structural stability of the silicon anode material is better maintained.
Nanowires are difficult to synthesize by mild physical or chemical processes because of the relatively stable chemical nature of silicon. The existing synthesis technology comprises a vapor deposition method, a template method, an electrochemical etching method and other technologies, the process flow is complex, and the mass production is difficult to realize. In addition, the current methods for preparing the silicon-carbon composite material comprise ball milling, high-temperature pyrolysis, vapor deposition and the like, and most of the methods adopt a two-step process, namely, the silicon nano material is prepared firstly and then carbon composite is carried out. The method not only increases the preparation flow, but also is difficult to realize uniform compounding with the carbon material because the nano material is easy to agglomerate, and is extremely easy to oxidize in the compounding process, so that the improvement on the electrochemical performance is limited.
The plasma has the characteristics of high temperature, high reaction atmosphere activity, high reaction speed, no electrode pollution and the like, and has remarkable advantages in the aspect of preparing nano-micro powder. For example, seo et al used a mixture of nickel and magnesium oxide as the raw material, gasified at a high temperature using plasma, and then cooled, and obtained magnesium oxide nanorods with nickel particles supported on the surface (Surface and Coatings Technology,2013,228, S91-S96) due to the difference in condensation and precipitation orders caused by the difference in melting points of the materials. Li et al adopt a similar principle, add the mixed raw materials into a high temperature region of hydrogen plasma together, generate gas phase tungsten and copper simple substances through chemical reduction, and then perform heterogeneous nucleation according to the difference of melting points to synthesize tungsten copper nano powder (Journal of Alloy and Compounds,2021,853,156958) with a core-shell structure in one step. However, carbon and silicon have strong reaction tendency at high temperature, so that silicon carbide is generated, and a composite structure of elemental silicon and carbon cannot be obtained by adopting a similar method.
Disclosure of Invention
The invention aims at providing an induction thermal plasma in-situ synthesis method of a silicon-carbon nanocomposite for a lithium ion battery anode material, which solves the problems of complex process flow, uneven carbon layer coating, easy oxidation of nano materials and the like in the prior art by effectively inhibiting the formation of silicon carbide.
In order to achieve the aim of the invention, the sectional feeding mode is adopted, and the reaction speed of carbon silicon is restrained by controlling the temperature zone in the process of forming the silicon nanowires and compounding carbon silicon, so that the formation of silicon carbide is effectively avoided. Firstly, axially conveying a silicon source precursor into an induction thermal plasma high-temperature region, obtaining silicon vapor under the action of high temperature, cooling in the process of leaving the high-temperature region, and obtaining a silicon nanowire through nucleation growth; adding gas carbon sources such as acetylene, methane and the like into the tail part of the induction thermal plasma arc, and carrying out heterogeneous nucleation on the silicon surface by carbon formed by pyrolysis to obtain the silicon-carbon composite material. The reaction speed of the carbon-silicon is greatly inhibited at low temperature, so that the formation of silicon carbide is avoided, and the formation of the silicon nanowire is not influenced in the compounding process.
The invention further provides application of the silicon-carbon nanocomposite as a negative electrode of a lithium ion battery. The silicon-carbon composite material obtained by the method can be used as a negative electrode material to effectively improve the cycle stability of the lithium ion battery, and has good application prospect.
The invention relates to an induction thermal plasma in-situ synthesis method of a silicon-carbon nanocomposite for a lithium ion battery cathode, which comprises the following steps:
(1) Introducing middle gas and side gas into the induction thermal plasma device, and starting a negative pressure device to form stable induction thermal plasma; the power of the induction thermal induction plasma device is 10-100KW, the medium gas is argon, and the medium gas flow is 0.1-10m 3/h, preferably 0.2-5m 3/h; the side gas is one or more of inert gases such as argon, nitrogen and the like, and the side gas flow is 0.1-10m 3/h, preferably 0.2-8m 3/h. The negative pressure range of the negative pressure device is 10-500mm water column, preferably 20-200mm water column;
(2) Micron silicon powder or silicon-containing gas is adopted as a precursor; the grain diameter of the micron silicon powder is 1-200 mu m, preferably 20-100 mu m; the silicon-containing gas includes gases such as silane;
(3) And (3) axially carrying the silicon precursor into the induction thermal plasma in the step (1) for reaction, wherein the carrier gas is one or more gases such as argon, hydrogen and the like, and the flow rate of the carrier gas is 0.05-5m 3/h, preferably 0.1-2m 3/h. If the precursor is silicon powder, the feeding amount is 1-100g/min, preferably 5-50g/min; if the precursor is a silicon-containing gas, the flow rate is 0.1-2m 3/h, preferably 0.5-1m 3/h.
(4) After 2s of the silicon precursor is conveyed, simultaneously conveying a carbon source to the arc tail flame part of the induction thermal plasma in the step (1), wherein the carbon source is carbon-containing gas such as methane, acetylene and the like, and the flow rate of the carbon source is 0.01-2m 3/h, preferably 0.05-1m 3/h;
(5) After the reaction is finished, the silicon precursor is stopped to be conveyed, the carbon source is stopped to be conveyed after 2 seconds, and the product enters a collector to be collected.
Because the whole synthesis process is carried out in continuous moving air flow, the particles are in a good dispersion state, and agglomeration of silicon is effectively avoided, so that uniform coating of carbon outside the silicon nanowire (the center of the nanowire is mainly silicon nanoparticles, the outer part of the nanowire is mainly coated by a carbon layer formed by carbon nanoparticles), and the diameter of the nanowire can be 10-50 nm. The in-situ coating method can also effectively avoid the oxidation of nano silicon particles and is easier to realize continuous production. Meanwhile, the method has the advantages of simple process, high raw material selectivity, environment friendliness, no pollution and the like.
Drawings
FIG. 1 is an X-ray diffraction pattern of a silicon carbon nanocomposite prepared in example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of the silicon carbon nanocomposite prepared in example 1 of the present invention;
FIG. 3 is a transmission electron microscope image of the silicon carbon nanocomposite prepared in example 1 of the present invention;
FIG. 4 is an elemental distribution image of a silicon carbon nanocomposite prepared in example 1 of the present invention;
fig. 5 is battery cycle data for a silicon carbon nanocomposite prepared in example 1 of the present invention tested at a current density of 0.1C.
Detailed Description
The invention will be further illustrated with reference to the following examples, which are not intended to limit the scope of the invention.
Example 1
The induction thermal plasma reaction equipment is 10KW. Silicon powder having a particle diameter of 50 μm was first placed in a feeder of an induction thermal plasma reaction apparatus. Introducing middle gas and side gas, wherein the flow rate of the middle gas is argon, the flow rate of the middle gas is 0.2m 3/h, the flow rate of the side gas is argon, and the flow rate of the side gas is 1m 3/h. And opening the negative pressure device until 20mm of water column is filled for air suction. Simultaneously, carrier gas is introduced, a feeder is opened for feeding, the carrier gas is argon, the flow rate is 0.2m 3/h, and the feeding amount is 5g/min. After 2s of reaction, a carbon source is conveyed at the tail flame part of the induction thermal plasma, wherein the carbon source is acetylene gas, and the flow rate is 0.3m 3/h. After the reaction is finished, the silicon precursor is stopped to be conveyed, the carbon source is stopped to be conveyed after 2 seconds, and the product enters a collector to be collected.
And fully mixing the silicon-carbon nanocomposite obtained by the method, carbon black and sodium carboxymethylcellulose in a mass ratio of 8:1:1, and obtaining the negative electrode slurry by adjusting the proportion of deionized water. The slurry was uniformly smeared on a copper foil using a 100 μm doctor blade, and vacuum-dried at 80 ℃ for 10 hours to obtain a negative electrode sheet. Finally, taking metal lithium as a counter electrode, taking a polypropylene film as a diaphragm, and taking LiPF 6 (LX-025) with the molar concentration of 1mol/L as electrolyte. Button cells were assembled in an argon glove box and tested for electrochemical performance. The charge-discharge voltage interval is 0.01V-3.0V, and the current density is 0.1C. FIG. 5 is a graph of the cycle performance test of the SiC nanocomposite obtained in example 1, the SiC nanocomposite having a specific capacity for first discharge of 2626.74mAh/g, a specific capacity for charge of 2128.81mAh/g, and a first-turn coulombic efficiency of 81.04%. After 100 cycles, the capacity is kept at 1127.81mAh/g, and the single-cycle coulomb efficiency is as high as 98%.
Example 2
The induction thermal plasma reaction equipment is 10KW. Silicon powder having a particle diameter of 40 μm was first placed in a feeder of an induction thermal plasma reaction apparatus. Introducing middle gas and side gas, wherein the flow rate of the middle gas is argon, the flow rate of the middle gas is 0.5m 3/h, the flow rate of the side gas is argon, and the flow rate of the side gas is 1.5m 3/h. And opening the negative pressure device to 30mm water column for air suction. Simultaneously, carrier gas is introduced, a feeder is opened for feeding, the carrier gas is argon, the flow rate is 0.8m 3/h, and the feeding rate is 10g/min. After 2s of reaction, a carbon source is conveyed at the tail flame part of the induction thermal plasma, wherein the carbon source is acetylene gas, and the flow rate is 0.2m 3/h. After the reaction is finished, the silicon precursor is stopped to be conveyed, the carbon source is stopped to be conveyed after 2 seconds, and the product enters a collector to be collected.
Example 3
The induction thermal plasma reaction equipment is 10KW. Silicon powder having a particle diameter of 30 μm was first placed in a feeder of an induction thermal plasma reaction apparatus. Introducing middle gas and side gas, wherein the flow rate of the middle gas is argon, the flow rate of the middle gas is 1m 3/h, the flow rate of the side gas is argon, and the flow rate of the side gas is 2m 3/h. And opening the negative pressure device to 40mm water column for air suction. Simultaneously, carrier gas is introduced, a feeder is opened for feeding, the carrier gas is argon, the flow rate is 1m 3/h, and the feeding rate is 15g/min. After 2s of reaction, a carbon source is conveyed at the tail flame part of the induction thermal plasma, wherein the carbon source is acetylene gas, and the flow rate is 0.1m 3/h. After the reaction is finished, the silicon precursor is stopped to be conveyed, the carbon source is stopped to be conveyed after 2 seconds, and the product enters a collector to be collected.
Claims (5)
1. An induction thermal plasma in-situ synthesis method of a silicon-carbon nanocomposite is characterized in that a sectional feeding mode is adopted, and the reaction speed of carbon and silicon is restrained by controlling the formation of a silicon nanowire and the temperature zone of a carbon-silicon composite process, so that the formation of silicon carbide is effectively avoided; firstly, axially conveying a silicon source precursor into an induction thermal plasma high-temperature region, obtaining silicon vapor under the action of high temperature, cooling in the process of leaving the high-temperature region, and obtaining a silicon nanowire through nucleation growth; adding gas carbon sources such as acetylene, methane and the like into the tail part of the induction thermal plasma arc, and carrying out heterogeneous nucleation on the silicon surface by carbon formed by pyrolysis to obtain the silicon-carbon composite material.
2. The method according to claim 1, characterized in that it comprises in particular the following steps:
(1) Introducing middle gas and side gas into the induction thermal plasma device, and starting a negative pressure device to form stable induction thermal plasma; the power of the induction thermal induction plasma device is 10-100KW, the medium gas is argon, and the medium gas flow is 0.1-10m 3/h, preferably 0.2-5m 3/h; the side gas is one or more of inert gases such as argon, nitrogen and the like, and the side gas flow is 0.1-10m 3/h, preferably 0.2-8m 3/h. The negative pressure range of the negative pressure device is 10-500mm water column, preferably 20-200mm water column;
(2) Micron silicon powder or silicon-containing gas is adopted as a precursor; the grain diameter of the micron silicon powder is 1-200 mu m, preferably 20-100 mu m; the silicon-containing gas includes gases such as silane;
(3) And (3) axially carrying the silicon precursor into the induction thermal plasma in the step (1) for reaction, wherein the carrier gas is one or more gases such as argon, hydrogen and the like, and the flow rate of the carrier gas is 0.05-5m 3/h, preferably 0.1-2m 3/h. If the precursor is silicon powder, the feeding amount is 1-100g/min, preferably 5-50g/min; if the precursor is a silicon-containing gas, the flow rate is 0.1-2m 3/h, preferably 0.5-1m 3/h.
(4) After 2s of the silicon precursor is conveyed, simultaneously conveying a carbon source to the arc tail flame part of the induction thermal plasma in the step (1), wherein the carbon source is carbon-containing gas such as methane, acetylene and the like, and the flow rate of the carbon source is 0.01-2m 3/h, preferably 0.05-1m 3/h;
(5) After the reaction is finished, the silicon precursor is stopped to be conveyed, the carbon source is stopped to be conveyed after 2 seconds, and the product enters a collector to be collected.
3. The silicon carbon nanocomposite material is prepared according to the method of claim 1 or 2.
4. The silicon-carbon nanocomposite prepared by the method according to claim 1 or 2, wherein carbon is uniformly coated outside a silicon nanowire, the center of the nanowire is mainly silicon nanoparticles, the outside of the nanowire is mainly coated by a carbon layer formed by the carbon nanoparticles, and the diameter of the nanowire can be in the range of 10-50nm.
5. The use of the silicon carbon nanocomposite material prepared according to the method of claim 1 or 2 as a negative electrode of a lithium ion battery.
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