CN112421002B - High-capacity silicon-carbon material and preparation method thereof - Google Patents
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Abstract
The invention relates to a high-capacity silicon-carbon material and a preparation method thereof. The preparation method comprises the following steps: s1, uniformly mixing the silicon source, the coating agent and the conductive agent to obtain a mixed material; s2, fusing the mixed materials; s3, high-temperature coating treatment; and S4, high-temperature carbonization treatment. The silicon source, the coating agent and the conductive agent can be more uniformly and tightly bonded in the fusion process, the addition of the conductive agent can enhance the conductivity of the silicon-carbon material, the agglomeration among conductive agent particles can be avoided in the fusion process, so that the conductive agent particles are uniformly dispersed, meanwhile, through surface high-temperature dynamic coating, the coating agent on the outer layer of the silicon source can carry out surface modification on the exposed silicon source, and a layer of stable and smooth solid electrolyte interface film can be formed on the carbon surface, so that the prepared silicon-carbon material can have high capacity and efficiency, and the good coating layer can effectively relieve the volume expansion of the silicon-carbon material, so that the cycle performance is improved.
Description
Technical Field
The invention relates to the technical field of lithium batteries, in particular to a high-capacity silicon-carbon material and a preparation method thereof.
Background
Lithium ion batteries have the advantages of high energy density, long cycle life, little environmental pollution and the like, are the key points of research in various countries in the world, and are widely applied to computers, mobile phones and other portable electronic devices. However, with the rapid development of electric vehicles and advanced electronic devices, higher requirements are placed on the energy density of lithium ion batteries. The key to improving the energy density of lithium ion batteries is the improvement of electrode materials and the improvement of performance.
At present, the negative electrode material of the commercial lithium ion battery is mainly made of graphite materials, and has low theoretical specific capacity (the specific capacity is only 372 mAh/g) and poor rate capability. Therefore, scientists are dedicated to research novel high-capacity negative electrode materials, silicon attracts much attention due to the high theoretical specific capacity (4200 mAh/g), the voltage platform of the silicon-intercalated lithium is low (< 0.5V), the silicon-intercalated lithium has low reactivity with electrolyte, the silicon-intercalated lithium is rich in earth crust, the silicon-intercalated lithium ion battery has low price, and the silicon-intercalated lithium ion battery has wide development prospect as the negative electrode material of the lithium ion battery. However, silicon undergoes a large change (> 300%) in volume during lithium deintercalation, resulting in a sharp pulverization and exfoliation of the active material during charge and discharge cycles, so that electrical contact between the electrode active material and the current collector is lost. Meanwhile, due to the huge volume expansion of the silicon material, the solid electrolyte interface film cannot stably exist in the electrolyte, resulting in reduced cycle life and capacity loss. In addition, the low conductivity of silicon severely limits the full utilization of its capacity and rate capability of the silicon electrode material.
Patent document CN103441250A discloses a negative electrode material for a lithium ion secondary battery, which is prepared by using silicon-containing oxide as a raw material, fully mixing with graphite and asphalt, adding conductive metal salt, and performing high-energy ball milling and high-temperature heat treatment. In this patent document, a material is produced by using Silica (SiO) as a raw material, and although the cycle and the electric conductivity characteristics are improved, the reversible capacity is about 650mAh/g, and the first efficiency is less than 70%.
Patent document CN103474631A discloses a silica composite negative electrode material, which comprises a silica matrix, a nano-silicon material uniformly deposited on the silica matrix, and a nano-conductive material coating layer on the silica/nano-silicon surface. The preparation method of the silicon monoxide composite negative electrode material comprises the steps of nano silicon chemical vapor deposition, nano conductive material coating modification, sieving and demagnetizing treatment. Although the specific capacity (1600 mAh/g) and the first coulombic efficiency (80%) of the silicon oxide composite negative electrode material are improved to a certain extent, the silicon oxide composite negative electrode material is formed by artificially introducing a nano silicon material with large volume expansion on the surface of SiO particles in a physical combination mode on the basis of the original component structure of the SiO material, the crystal grain is large and difficult to control, the dispersibility is poor, the problem of huge volume expansion caused by the silicon material cannot be effectively buffered and avoided, and the cycle performance is poor.
Therefore, for the silicon-carbon material, the technical problems in the field are that the original component structure of the material system is maintained, the lower volume effect is ensured, the capacity exertion and the first coulombic efficiency of the silicon-carbon material are greatly improved, the electric conductivity and the cycle performance of the silicon-carbon material are improved, and the volume expansion of the silicon-carbon material is further reduced.
Disclosure of Invention
The invention provides a high-capacity silicon-carbon material and a preparation method thereof for solving the technical problems.
The invention is realized by the following technical scheme:
a high-capacity silicon-carbon material takes a silicon material as a core and takes a carbon layer doped with a conductive agent as a shell.
Preferably, the silicon material is silicon powder and/or silicon monoxide.
More preferably, the carbon layer is made of at least one of glucose, sucrose, high-temperature asphalt, polyvinyl alcohol, polyvinylpyrrolidone, phenolic resin, polyacrylonitrile, polystyrene, polyacrylic acid, lithium polyacrylate, and polyaniline.
Further preferably, the conductive agent is selected from at least one of carbon nanotubes, fullerenes, graphene, graphite, and carbon black.
A preparation method of a high-capacity silicon-carbon material comprises the following steps:
s1, uniformly mixing the silicon source, the coating agent and the conductive agent to obtain a mixed material;
s2, fusing the mixed materials to obtain fused materials;
s3, high-temperature coating treatment;
and S4, carrying out high-temperature carbonization treatment to obtain the high-capacity silicon-carbon material.
Preferably, the mass ratio of the silicon source to the coating agent to the conductive agent is A: B: C;
wherein, A =1, B =0.01% -20%, C =0.01% -5%.
Further preferably, the silicon source has a particle size D50=1-10 μm; the particle size of the coating agent is 0.5-10 μm; the particle size of the conductive agent is 0.1-2 μm.
Further, the S2 specifically includes: and (3) placing the mixed material obtained in the step (S1) into a fusion machine for fusion, wherein the fusion rate is 20-50HZ, the rotation speed is 500-1000rmp, and the fusion time is 5-60 min.
Further, the S3 specifically includes: and (3) dynamically coating the fused material obtained in the step (S2) in a high-temperature coating machine, wherein the heat preservation temperature is 200-500 ℃, and the heat preservation time is 2-10 h.
Further, the S4 specifically includes: and (3) placing the coated material in a tubular furnace, heating to the temperature of 500-1100 ℃, and preserving the heat for 2-10h to obtain the high-capacity silicon-carbon material.
Compared with the prior art, the invention has the following beneficial effects:
according to the silicon-carbon material, the carbon layer shell on the outer layer of the silicon material can be used for carrying out surface modification on an exposed silicon source, and the addition of the conductive agent can enhance the conductivity of the silicon-carbon material and avoid the agglomeration of silicon nano particles, so that the silicon-carbon material has high capacity and efficiency, and the good coating layer can effectively relieve the volume expansion of the silicon-carbon material, so that the cycle performance is improved;
2, the fusion process of the method can ensure that the silicon source, the coating agent and the conductive agent are more uniformly and more tightly bonded, and simultaneously, a layer of stable and smooth solid electrolyte interface film is formed on the carbon surface while the surface of the silicon source is modified by surface high-temperature dynamic coating, so that the volume expansion of the silicon-carbon material can be effectively relieved, and the cycle performance is improved.
Drawings
The accompanying drawings, which are included to provide a further understanding of the embodiments of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention.
FIG. 1 is a schematic structural diagram of a high capacity silicon carbon material of the present invention;
FIG. 2 is a scanning electron micrograph of a high capacity silicon carbon material of example 1;
fig. 3 is a charge-discharge graph of the high capacity silicon carbon material of example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples and accompanying drawings, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not meant to limit the present invention.
As shown in fig. 1, the high-capacity silicon-carbon material disclosed in the present invention uses a silicon material as a core and a carbon layer doped with a conductive agent as a shell.
Wherein, the silicon material can be silicon powder and/or silicon monoxide. The carbon layer is prepared from at least one of glucose, sucrose, high temperature asphalt, polyvinyl alcohol, polyvinylpyrrolidone, phenolic resin, polyacrylonitrile, polystyrene, polyacrylic acid, lithium polyacrylate, and polyaniline. The conductive agent is selected from at least one of carbon nanotubes, fullerenes, graphene, graphite, and carbon black.
The invention discloses a preparation method of a high-capacity silicon-carbon material, which comprises the following steps:
s1, weighing a silicon source, a coating agent and a conductive agent, adding the silicon source, the coating agent and the conductive agent into a high-speed stirrer in proportion, and uniformly mixing at a stirring speed of 5-50rmp for 10-60min to obtain a mixed material;
s2, placing the mixed material obtained in the S1 into a fusion machine for fusion, and introducing inert protective gases such as N2, Ar, He and the like; wherein the fusion rate is 20-50HZ, the rotation speed is 500-1000rmp, and the fusion time is 5-60 min;
s3, placing the silicon source coated with the coating agent on the outer layer in a high-temperature coating machine for dynamic coating; wherein the heat preservation temperature is 200-;
s4, placing the coated material in a tube furnace, heating to 1100 ℃ in a nitrogen atmosphere, and preserving heat for 2-10h to obtain the high-capacity silicon-carbon material. Wherein the heating rate is 1-10 ℃/min.
In the embodiment, the mass ratio of the silicon source to the coating agent to the conductive agent is A to B to C; wherein, A =1, B =0.01% -20%, C =0.01% -5%.
The particle size of the silicon source D50=1-10 μm, the particle size of the coating agent is 0.5-10 μm, and the particle size of the conductive agent is 0.1-2 μm.
The silicon source, the coating agent and the conductive agent can be more uniform and more tightly bonded in the fusion process, the addition of the conductive agent can enhance the conductivity of the silicon-carbon material, the aggregation among conductive agent particles can be avoided in the fusion process, the conductive agent particles are uniformly dispersed, and meanwhile, the coating agent on the outer layer of the silicon source can carry out surface modification on the exposed silicon source through surface high-temperature dynamic coating, and a layer of relatively stable and smooth solid electrolyte interface film can be formed on the carbon surface, so that the prepared silicon-carbon material can have high capacity and efficiency, and the volume expansion of the silicon-carbon material can be effectively relieved through a good coating layer, and the cycle performance is improved.
Based on the high-capacity silicon-carbon material and the preparation method, the invention discloses 3 specific embodiments.
Example 1
Weighing 1kg of silica with the particle size D50=5.18 μm, adding the silica, 16.48g of phenolic resin and 131g of carbon black into a high-speed stirrer together, stirring at 50rmp for 50min, and uniformly mixing; uniformly mixing the silicon monoxide, the coating machine and the conductive agent, adding the mixture into a fusion machine for fusion, introducing N2 serving as protective gas, and performing fusion at the rate of 30HZ and the rotation speed of 1000rmp for 30 min; dynamically coating the mixture in a high-temperature coating machine, wherein the heat preservation temperature is 150 ℃, the heating rate is 1.5 degrees/min, and the heat preservation time is 2 hours; and finally, performing high-temperature carbonization treatment on the mixture, placing the mixture in a tubular furnace, raising the temperature to 1000 ℃ at a heating rate of 3 ℃/min, and preserving the heat for 2 hours to obtain the high-capacity silicon-carbon material.
Example 2
Weighing 2kg of silica, wherein the particle size of the raw material D50=1.32 μm, adding the silica, 15.82g of polyvinyl alcohol and 220g of carbon nano tubes into a high-speed stirrer together, stirring at 20rmp for 30min, and uniformly mixing; uniformly mixing silicon powder, a coating machine and a conductive agent, adding the mixture into a fusion machine for fusion, introducing Ar serving as protective gas, wherein the fusion rate is 50HZ, the rotation speed is 800rmp, and the fusion time is 50 min; dynamically coating the mixture in a high-temperature coating machine, wherein the heat preservation temperature is 300 ℃, the heating rate is 3 ℃/min, and the heat preservation time is 4 h; and finally, performing high-temperature carbonization treatment on the mixture, placing the mixture in a tubular furnace, raising the temperature to 1100 ℃ at a heating rate of 5 ℃/min, and preserving the heat for 3 hours to obtain the high-capacity silicon-carbon material.
Example 3
Weighing 2kg of silica with a particle size of D50=3.56 μm, adding silica, 20.48 g of sodium carboxymethylcellulose and 189g of carbon black into a high-speed stirrer together at a stirring speed of 50rmp for 60min, and uniformly mixing; uniformly mixing the silicon monoxide, the coating machine and the conductive agent, adding the mixture into a fusion machine for fusion, introducing Ar as protective gas, wherein the fusion rate is 30HZ, the rotation speed is 1000rmp, and the fusion time is 40 min; and finally, performing high-temperature carbonization treatment on the mixture, placing the mixture in a tubular furnace, raising the temperature to 1000 ℃ at the heating rate of 8 DEG/min, and preserving the heat for 2 hours to obtain the high-capacity silicon-carbon material.
Comparative example 1
Comparative example 1 this example uses the starting silica material of example 1 with a particle size D50=5.18 μm. Adding the silicon monoxide, 16.48g of phenolic resin and 131g of carbon black into a high-speed stirrer together, stirring at the speed of 50rmp for 50min, directly carrying out high-temperature carbonization on the mixture, placing the mixture into a tubular furnace, raising the temperature to 1000 ℃ at the rate of 3 ℃/min, and preserving the temperature for 2h to obtain the silicon-carbon material.
In order to detect the performance of the lithium ion battery cathode material made of the silicon-carbon material, performance tests were performed on the lithium ion batteries made of the silicon-carbon materials of example 1, example 2, example 3, and comparative example 1.
The testing method adopts a half-cell testing method, and comprises the following specific steps: prepared silicon carbon material, SP and PVDF in the weight ratio of 7 to 1.5 are mixed with NMP to form slurry, the slurry is coated on copper foil and dried in a vacuum drying oven for 12 hours to form a negative plate, and a battery is assembled by taking a polypropylene microporous membrane as a diaphragm and a lithium plate as a counter electrode. And (3) carrying out a constant-current charge and discharge experiment in the LAND battery test system, limiting the charge and discharge voltage to be 0.005-2.0V, and carrying out data acquisition and control by using a charge and discharge cabinet controlled by a computer. The test results are shown in table 1, fig. 2 and fig. 3.
TABLE 1 comparison of the Power-on test for examples and comparative examples
As can be seen from table 1, the discharge capacity and the first efficiency of the high capacity silicon carbon materials prepared in examples 1 to 3 are increased relative to the silicon carbon material in comparative example 1, indicating that the coating effect and the conductivity of the high capacity silicon carbon material synthesized by the method of the present invention are improved, corresponding to the increase in the conductivity of the material.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (8)
1. A preparation method of a high-capacity silicon-carbon material is characterized by comprising the following steps: the silicon-carbon material takes a silicon material as a core and takes a carbon layer doped with a conductive agent as a shell, and the preparation method comprises the following steps:
s1, uniformly mixing the silicon source, the coating agent and the conductive agent to obtain a mixed material;
s2, fusing the mixed materials to obtain fused materials;
s3, dynamically coating the fused material obtained in the step S2 in a high-temperature coating machine, wherein the heat preservation temperature is 200-500 ℃, and the heat preservation time is 2-10 hours;
and S4, carrying out high-temperature carbonization treatment to obtain the high-capacity silicon-carbon material.
2. The method of claim 1, wherein: the silicon material is silicon powder and/or silicon monoxide.
3. The method of claim 1, wherein: the carbon layer is prepared from at least one of glucose, sucrose, high-temperature asphalt, polyvinyl alcohol, polyvinylpyrrolidone, phenolic resin, polyacrylonitrile, polystyrene, polyacrylic acid, lithium polyacrylate and polyaniline.
4. The method of claim 1, wherein: the conductive agent is selected from at least one of carbon nanotubes, fullerenes, graphene, graphite, and carbon black.
5. The production method according to any one of claims 1 to 4, characterized in that: the mass ratio of the silicon source to the coating agent to the conductive agent is A to B to C;
wherein, A =1, B =0.01% -20%, C =0.01% -5%.
6. The production method according to any one of claims 1 to 4, characterized in that: the particle size of the silicon source D50=1-10 μm; the particle size of the coating agent is 0.5-10 μm; the particle size of the conductive agent is 0.1-2 μm.
7. The method of claim 1, wherein: the S2 specifically includes: and (3) placing the mixed material obtained in the step (S1) into a fusion machine for fusion, wherein the fusion rate is 20-50HZ, the rotation speed is 500-1000rmp, and the fusion time is 5-60 min.
8. The production method according to any one of claims 1 to 4, characterized in that: the S4 specifically includes: and (3) placing the coated material in a tubular furnace, heating to the temperature of 500-1100 ℃, and preserving the heat for 2-10h to obtain the high-capacity silicon-carbon material.
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| CN110582876A (en) * | 2017-05-12 | 2019-12-17 | 株式会社Lg化学 | Negative electrode active material, negative electrode comprising the same, and secondary battery comprising the same |
| CN107611369A (en) * | 2017-08-11 | 2018-01-19 | 天津爱敏特电池材料有限公司 | A kind of lithium-ion battery silicon-carbon anode material and preparation method thereof |
| CN109301184A (en) * | 2018-09-10 | 2019-02-01 | 江苏塔菲尔新能源科技股份有限公司 | Modified composite material, preparation method and the purposes in lithium ion battery of siliceous substrates material |
| CN109216689A (en) * | 2018-10-25 | 2019-01-15 | 湖北融通高科先进材料有限公司 | A kind of Si-C composite material and preparation method thereof and lithium ion battery |
| CN109671942A (en) * | 2018-12-24 | 2019-04-23 | 成都硅宝科技股份有限公司 | A kind of lithium-ion battery silicon-carbon anode material and preparation method thereof |
| CN110620224A (en) * | 2019-09-27 | 2019-12-27 | 广东省稀有金属研究所 | Negative electrode material for lithium battery, preparation method of negative electrode material and lithium battery |
| CN111146420A (en) * | 2019-12-26 | 2020-05-12 | 宁德新能源科技有限公司 | Negative electrode material, and electrochemical device and electronic device comprising same |
| CN111682173A (en) * | 2020-06-03 | 2020-09-18 | 湖南大学 | Composite material of multi-heteroatom co-doped carbon shell coated silicon and preparation method thereof |
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Denomination of invention: A high capacity silicon carbon material and its preparation method Effective date of registration: 20220929 Granted publication date: 20220329 Pledgee: Chengdu financial holding Financing Guarantee Co.,Ltd. Pledgor: CHENGDU AIMINTE NEW ENERGY TECHNOLOGY Co.,Ltd. Registration number: Y2022510000266 |