CN112510185A - Silicon-carbon composite negative electrode material and manufacturing method thereof - Google Patents
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Abstract
The invention discloses a silicon-carbon composite negative electrode material and a manufacturing method thereof. The nano silicon particles coated by the carbon layer have the size of 2-5nm, and the small particle size can relieve the volume expansion of silicon. The thickness of the carbon layer coated on the surface of the nano silicon particles is only 1-3nm, so that the agglomeration of nano silicon can be avoided. The gaps of the main spherical graphite particles provide expansion spaces for the composite nano silicon. The lithium ion battery prepared by the composite silicon-carbon cathode material has high energy density, greatly improved cycle performance and excellent conductivity. The lithium electronic battery has high first efficiency, high mass specific capacity, good cycling stability and long service life. All the performances can meet the industrial production requirements, and the method is suitable for industrial application.
Description
Technical Field
The invention relates to a lithium ion battery cathode material, and particularly provides a lithium ion battery silicon-carbon composite cathode material and a preparation method thereof.
Background
Lithium ion batteries are a common energy storage and conversion device in modern life. Nowadays, with the development of renewable energy sources and electric automobiles, higher and higher requirements are put forward on the energy density of lithium ion batteries, and the improvement of the energy density of the lithium ion batteries by graphite negative electrode materials (the theoretical specific capacity is only 372mAh/g) mainly applied in the market is a bottleneck, and the improvement of the space of the lithium ion batteries is difficult to realize. In order to improve the energy density of the lithium ion battery, a negative electrode material with high capacity and long service life needs to be developed, and the theoretical specific lithium storage capacity of silicon is 4200mAh/g, which is more than 10 times of that of the traditional graphite (the theoretical specific mass capacity is 372mAh/g) negative electrode. Among all elements capable of alloying to store lithium, the specific capacity of silicon is the highest, and the ultrahigh theoretical specific capacity of silicon makes silicon one of the most competitive candidate materials for the next-generation high-performance lithium ion battery cathode material.
In addition, the silicon element is rich in the earth crust, has no toxicity and is environment-friendly, and the silicon element and the earth crust make the silicon anode material have advantages compared with other competitors. But it is accompanied by a large volume change of nearly 300% during charge and discharge due to its ultra-high lithium storage capacity. The volume change is fatal to the material, the repeated huge volume change can cause the material to generate fatigue, the mechanical strength of the material is seriously influenced, and finally, the electrode material is cracked, pulverized and dropped to lose good electric contact with a current collector, so that a large part of the electrode material cannot continuously and reversibly participate in the charging and discharging process of the battery, and the battery capacity is rapidly attenuated. This problem has been a stumbling stone in the commercial application of silicon negative electrode materials. To solve this problem, numerous scholars have given many different solutions. Some researchers proposed to control the size of silicon material at nanometer level, to make silicon particles into nanometer, and to make lithium ion (Li) after nanometer+) The diffusion distance in the electrode material is greatly shortened, however, the surface energy of nano silicon particles is higher, secondary agglomeration is easy to occur, the capacity is quickly attenuated, and the silicon negative electrode with excellent electrical property is difficult to prepare only by reducing the particle size of the materialA pole material. In addition, researchers have proposed that the structure of silicon nanoparticles is optimized and the electrochemical reaction kinetics is improved, for example, silicon nanowires, silicon nanotubes or mesoporous silicon are selected, and the porous silicon material is rich in pores to greatly relieve the stress of swelling and shrinking, but the method for synthesizing mesoporous silicon or silicon powder with a net structure is high in cost and harsh in synthesis conditions. None of these solutions described above fundamentally solves the problem of silicon expansion.
The carbon material has small specific capacity as a negative electrode material, has certain electrochemical activity and relatively stable structure, and can be used as a 'buffer matrix' of a silicon electrode. The carbonaceous negative electrode material has a relatively small volume change during charge and discharge and is a good conductor of electrons, and thus is selected as a dispersion carrier for dispersing silicon particles. In addition, the silicon and the carbon have similar chemical properties and can be tightly combined. If the silicon particles can be dispersed in the carbon material in a nano manner, the structure of the carbon material and the gaps among the silicon particles in the nano dispersion state can provide a large number of channels for lithium ions, and the insertion positions of the lithium ions are increased. The carbon-silicon composite can achieve the purposes of improving the silicon volume effect and improving the electrochemical stability.
Therefore, the silicon-carbon composite negative electrode material with high capacity and excellent cycle performance can be prepared by combining the performances of silicon and carbon, and the purpose of advantage complementation is achieved by utilizing the synergistic effect among the components of the composite material. At present, researches show that the graphene and the nano silicon powder are directly mixed to synthesize the composite negative electrode material, the obtained material shows better cycle performance, the specific capacity can still keep 1600mAh/g after 30 cycles, and the material still slowly attenuates. Therefore, the development of a preparation process which is simple and stable in process, high in specific capacity and capable of effectively inhibiting the volume effect of silicon is one of the difficult problems to be solved in the fields of preparation of high-capacity silicon-based negative electrode materials and preparation of high-capacity lithium ion batteries.
Disclosure of Invention
The invention aims to provide a silicon-carbon composite negative electrode material and a manufacturing method thereof, wherein the material has ultrahigh specific capacity, controls the volume expansion problem of silicon materials, has good chemical properties and long service life, and is suitable for industrial application.
The purpose of the invention is realized by the following technical method, and the silicon-carbon composite negative electrode material comprises carbon-coated nano silicon particles, micron-sized spherical graphite particles, a binder and a conductive agent.
The size of the carbon-coated nano silicon particles is 2-5nm, and the thickness of the carbon layer coated on the outer layer of the nano silicon is 1-3 nm.
The preparation method of the carbon-coated nano silicon particle adopts one of CVD method silane cracking, chemical wet method, etching method or spray drying method.
The carbon-coated nano silicon particle is characterized in that: the carbon layer coated on the outer layer of the nano silicon has stronger mechanical strength, inhibits the volume expansion of the silicon material and has better conductivity.
The carbon-coated nano silicon particles are prepared by one of a vapor deposition method, a chemical adsorption method and the like.
The micron spherical graphite particles have the particle size distribution range of 0.5-20 mu m.
The micron-sized spherical graphite particles are one of artificial graphite, natural graphite, mesocarbon microbeads, soft carbon or hard carbon and the like.
The micron-sized spherical graphite particles form surface micropore depressions through surface etching, and provide adsorption points for the carbon-coated nano silicon particles.
The adhesive is one or more of sodium carboxymethylcellulose (CMC), polyacrylic acid (PAA), styrene-butadiene rubber emulsion (SBR), polyacrylate and acrylonitrile copolymer.
The conductive agent is one or more of conductive graphite, acetylene black, graphene, single-arm carbon nanotubes and multi-arm carbon nanotubes.
The preparation method of the carbon-coated nano silicon particle comprises the following steps:
(1) placing polysilane in a tubular furnace, and introducing argon for protection;
(2) heating at 2-5 deg.C/min at 800 deg.C for 1-5 hr;
(3) cooling to obtain nano silicon, and performing vapor deposition and carbon coating after passing through a sand mill to obtain carbon-coated nano silicon particles.
The invention provides a preparation method of a silicon-carbon composite negative electrode material, which comprises the following steps:
(1) firstly, adding an adhesive (with the content of 0.5-10%) into a hydrosolvent, stirring and dissolving, and then adding a conductive agent (with the content of 0.05-10%);
(2) adding the prepared carbon-coated nano silicon and spherical graphite particles into the mixed solution according to the proportion of 1-20%, and fully and uniformly stirring;
(3) and coating the mixed solution on an aluminum foil substrate, and heating and drying to form the silicon-carbon negative electrode material.
The silicon-carbon composite negative electrode material, the positive electrode material, the diaphragm, the electrolyte and the like are assembled into the lithium ion battery for testing, the energy density of the battery is 300Wh/kg, the gram capacity of the negative electrode material can be up to 800mAh/g, and the capacity maintenance rate is 90% after 500 times of circulation.
The invention has the beneficial effects that:
1. the silicon-based negative electrode material inhibits the volume expansion of silicon, thereby reducing the problem of narrow lithium ion transmission channel caused by the volume expansion of the silicon and improving the cycle performance of the lithium ion battery.
2. The preparation process is simple, the prepared lithium ion negative electrode material has excellent conductivity, and the lithium ion battery prepared by using the silicon-carbon composite material has the advantages of high first efficiency, high mass specific capacity, good cycling stability and long service life, and is suitable for industrial application.
Drawings
The invention is described in further detail below with reference to the following figures and embodiments:
FIG. 1 and FIG. 2 show carbon-coated nano-silicon particles synthesized according to the present invention;
Detailed Description
Example 1
The following examples of the present invention are described in detail, and it will be understood by those skilled in the art that the following examples are intended to illustrate the present invention, but should not be construed as limiting the present invention. Unless otherwise indicated, specific techniques or conditions are not explicitly described in the following examples, and those skilled in the art may follow techniques or conditions commonly employed in the art or in accordance with the product specifications.
The preparation method of the carbon-coated nano silicon comprises the following steps:
(1) placing polysilane in a tubular furnace, and introducing argon for protection;
(2) heating at 2 deg.C/min, maintaining at 500 deg.C for 1 hr;
(3) cooling to obtain nano silicon, and performing vapor deposition and carbon coating after passing through a sand mill to obtain carbon-coated nano silicon particles.
The preparation method of the silicon-carbon composite negative electrode material comprises the following steps:
(1) firstly, adding an adhesive (with the content of 0.5%) into a hydrosolvent, stirring to dissolve, and then adding a conductive agent (with the content of 0.05%);
(2) adding the prepared carbon-coated nano silicon and graphite cathode into the mixed solution according to the proportion of 1%, and fully and uniformly stirring;
(3) and coating the mixed solution on an aluminum foil substrate, and heating and drying to form the silicon-carbon negative electrode material.
The silicon-carbon composite negative electrode material, the positive electrode material, the diaphragm, the electrolyte and the like are assembled into the lithium ion battery for testing, the energy density of the battery is 210Wh/kg, the gram capacity of the negative electrode material is exerted at 390mAh/g, and the capacity maintenance rate is 88% after 500 times of circulation.
Example 2
The preparation method of the carbon-coated nano silicon comprises the following steps:
(1) placing polysilane in a tubular furnace, and introducing argon for protection;
(2) heating at the speed of 2 ℃/min, keeping the temperature at 600 ℃, and keeping the temperature for 2 hours;
(3) cooling to obtain nano silicon, and performing vapor deposition and carbon coating after passing through a sand mill to obtain carbon-coated nano silicon particles.
The preparation method of the silicon-carbon composite negative electrode material comprises the following steps:
(1) firstly, adding an adhesive (with the content of 1.5%) into a hydrosolvent, stirring to dissolve, and then adding a conductive agent (with the content of 1.0%);
(2) adding the prepared carbon-coated nano silicon and graphite cathode into the mixed solution according to the proportion of 5%, and fully and uniformly stirring;
(3) and coating the mixed solution on an aluminum foil substrate, and heating and drying to form the silicon-carbon negative electrode material.
The silicon-carbon composite negative electrode material, the positive electrode material, the diaphragm, the electrolyte and the like are assembled into the lithium ion battery for testing, the energy density of the battery is 260Wh/kg, the gram capacity of the negative electrode material is exerted at 450mAh/g, and the capacity maintenance rate is 98% after 500 times of circulation.
Example 3
The preparation method of the carbon-coated nano silicon comprises the following steps:
(1) placing polysilane in a tubular furnace, and introducing argon for protection;
(2) heating at 5 deg.C/min, maintaining at 800 deg.C for 5 hr;
(3) cooling to obtain nano silicon, and performing vapor deposition and carbon coating after passing through a sand mill to obtain carbon-coated nano silicon particles.
The preparation method of the silicon-carbon composite negative electrode material comprises the following steps:
(1) firstly, adding an adhesive (with the content of 2%) into a hydrosolvent, stirring to dissolve, and then adding a conductive agent (with the content of 1.0%);
(2) adding the prepared carbon-coated nano silicon and graphite cathode into the mixed solution according to the proportion of 20%, and fully and uniformly stirring;
(3) and coating the mixed solution on an aluminum foil substrate, and heating and drying to form the silicon-carbon negative electrode material.
The silicon-carbon composite negative electrode material, the positive electrode material, the diaphragm, the electrolyte and the like are assembled into the lithium ion battery for testing, the energy density of the battery is 300Wh/kg, the gram capacity of the negative electrode material is exerted at 800mAh/g, and the capacity maintenance rate is 97% after 500 times of circulation.
Example 4
The preparation method of the carbon-coated nano silicon comprises the following steps:
(1) placing polysilane in a tubular furnace, and introducing argon for protection;
(2) heating at 4 deg.C/min, maintaining at 500 deg.C for 4 hr;
(3) cooling to obtain nano silicon, and performing vapor deposition and carbon coating after passing through a sand mill to obtain carbon-coated nano silicon particles.
The preparation method of the silicon-carbon composite negative electrode material comprises the following steps:
(1) firstly, adding an adhesive (with the content of 3.0%) into a hydrosolvent, stirring to dissolve, and then adding a conductive agent (with the content of 5.0%);
(2) adding the prepared carbon-coated nano silicon and graphite cathode into the mixed solution according to the proportion of 10%, and fully and uniformly stirring;
(3) and coating the mixed solution on an aluminum foil substrate, and heating and drying to form the silicon-carbon negative electrode material.
The silicon-carbon composite negative electrode material, the positive electrode material, the diaphragm, the electrolyte and the like are assembled into the lithium ion battery for testing, the energy density of the battery is 230Wh/kg, the gram capacity of the negative electrode material is exerted at 550mAh/g, and the capacity maintenance rate is 92% after 500 times of circulation.
Example 5
The preparation method of the carbon-coated nano silicon comprises the following steps:
(1) placing polysilane in a tubular furnace, and introducing argon for protection;
(2) heating at the speed of 2 ℃/min, keeping the temperature at 600 ℃, and keeping the temperature for 5 hours;
(3) cooling to obtain nano silicon, and performing vapor deposition and carbon coating after passing through a sand mill to obtain carbon-coated nano silicon particles.
The preparation method of the silicon-carbon composite negative electrode material comprises the following steps:
(1) firstly, adding an adhesive (with the content of 6.5%) into a hydrosolvent, stirring to dissolve, and then adding a conductive agent (with the content of 8.0%);
(2) adding the prepared carbon-coated nano silicon particles and the graphite cathode into the mixed solution according to the proportion of 20%, and fully and uniformly stirring;
(3) and coating the mixed solution on an aluminum foil substrate, and heating and drying to form the silicon-carbon negative electrode material.
The silicon-carbon composite negative electrode material, the positive electrode material, the diaphragm, the electrolyte and the like are assembled into the lithium ion battery for testing, the energy density of the battery is 360Wh/kg, the gram capacity of the negative electrode material is exerted to 750mAh/g, and the capacity maintenance rate is 97% after 500 times of circulation.
Example 6
The preparation method of the carbon-coated nano silicon comprises the following steps:
(1) placing polysilane in a tubular furnace, and introducing argon for protection;
(2) heating at 4 deg.C/min, maintaining at 500 deg.C for 4 hr;
(3) cooling to obtain nano silicon, and performing vapor deposition and carbon coating after passing through a sand mill to obtain carbon-coated nano silicon particles.
The preparation method of the silicon-carbon composite negative electrode material comprises the following steps:
(1) firstly, adding an adhesive (with the content of 5.5%) into a hydrosolvent, stirring to dissolve, and then adding a conductive agent (with the content of 1.0%);
(2) adding the prepared carbon-coated nano silicon and graphite cathode into the mixed solution according to the proportion of 2%, and fully and uniformly stirring;
(3) and coating the mixed solution on an aluminum foil substrate, and heating and drying to form the silicon-carbon negative electrode material.
The silicon-carbon composite negative electrode material, the positive electrode material, the diaphragm, the electrolyte and the like are assembled into the lithium ion battery for testing, the energy density of the battery is 200Wh/kg, the gram capacity of the negative electrode material is exerted at 250mAh/g, and the capacity maintenance rate is 96% after 500 times of circulation.
Example 7
The preparation method of the carbon-coated nano silicon comprises the following steps:
(1) placing polysilane in a tubular furnace, and introducing argon for protection;
(2) heating at 3 deg.C/min, maintaining at 500 deg.C for 5 hr;
(3) cooling to obtain nano silicon, and performing vapor deposition and carbon coating after passing through a sand mill to obtain carbon-coated nano silicon particles.
The preparation method of the silicon-carbon composite negative electrode material comprises the following steps:
(1) firstly, adding an adhesive (with the content of 6.5%) into a hydrosolvent, stirring to dissolve, and then adding a conductive agent (with the content of 2.0%);
(2) adding the prepared carbon-coated nano silicon and graphite cathode into the mixed solution according to the proportion of 19 percent, and fully and uniformly stirring;
(3) and coating the mixed solution on an aluminum foil substrate, and heating and drying to form the silicon-carbon negative electrode material.
The silicon-carbon composite negative electrode material, the positive electrode material, the diaphragm, the electrolyte and the like are assembled into the lithium ion battery for testing, the energy density of the battery is 290Wh/kg, the gram capacity of the negative electrode material is exerted at 270mAh/g, and the capacity maintenance rate is 98% after 500 times of circulation.
The above embodiments are merely preferred examples to illustrate the present invention, and it should be apparent to those skilled in the art that any obvious variations and modifications can be made without departing from the spirit of the present invention.
Claims (9)
1. A silicon-carbon composite negative electrode material is characterized in that: comprises carbon-coated nano silicon particles, micron-sized spherical graphite particles, a binder and a conductive agent.
2. The silicon-carbon composite anode material according to claim 1, characterized in that: the size of the nano silicon particles of the carbon-coated nano silicon particles is 2-5nm, and the thickness of the carbon layer coated on the outer layer of the nano silicon is 1-3 nm.
3. The silicon-carbon composite anode material according to claim 1, characterized in that: the preparation method of the nano-silicon particles in the carbon-coated nano-silicon particles is one of a CVD thermal cracking method, a chemical wet method, an etching method or a spray drying method.
4. The silicon-carbon composite anode material according to claim 1, characterized in that: the carbon layer coated on the outer layer of the carbon-coated nano silicon particles is one of conductive graphite and a graphite cathode.
5. The silicon-carbon composite anode material according to claim 1, characterized in that: the particle size of the micron-sized spherical graphite particles is 0.5-20 mu m.
6. The silicon-carbon composite anode material according to claim 1, characterized in that: the micron-sized spherical graphite particles form surface micropore depressions through surface etching, and provide adsorption points for the carbon-coated nano silicon particles.
7. The silicon-carbon composite anode material as claimed in claim 4, wherein the coating method of the carbon layer of the nano-silicon outer layer is one of a vapor deposition method and a chemical adsorption method.
8. The silicon-carbon composite anode material according to claim 1, characterized in that: the preparation method of the carbon-coated nano silicon particles comprises the following specific steps:
(1) placing polysilane in a tubular furnace, and introducing argon for protection;
(2) heating at 2-5 deg.C/min at 800 deg.C for 1-5 hr;
(3) cooling to obtain nano silicon, and performing vapor deposition and carbon coating after passing through a sand mill to obtain carbon-coated nano silicon particles.
9. A method for preparing a silicon-carbon composite anode material according to any one of claims 1 to 8, comprising the steps of:
(1) firstly, adding an adhesive into a hydrosolvent, stirring and dissolving, and then adding a conductive agent;
(2) adding the prepared carbon-coated nano silicon and graphite cathode into the mixed solution according to the proportion of 1-20%, and fully and uniformly stirring;
(3) and coating the mixed solution on an aluminum foil substrate, and heating and drying to form the silicon-carbon negative electrode material.
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| CN114068901A (en) * | 2021-11-15 | 2022-02-18 | 陕西煤业化工技术研究院有限责任公司 | Silicon-carbon composite negative electrode material, preparation method and application |
| CN114792791A (en) * | 2022-05-27 | 2022-07-26 | 欣旺达电动汽车电池有限公司 | Negative electrode material, preparation method and application thereof |
| CN114792791B (en) * | 2022-05-27 | 2024-04-09 | 欣旺达动力科技股份有限公司 | Negative electrode material, preparation method and application thereof |
| CN115832254A (en) * | 2022-12-07 | 2023-03-21 | 银硅(宁波)科技有限公司 | Silicon-carbon composite negative electrode material and preparation method thereof |
| CN115832254B (en) * | 2022-12-07 | 2023-10-20 | 银硅(宁波)科技有限公司 | Silicon-carbon composite anode material and preparation method thereof |
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