CN108987693B - Preparation method of high-performance carbon-silicon composite material for lithium battery - Google Patents
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Abstract
The invention belongs to the technical field of lithium batteries, and particularly relates to a preparation method of a high-performance carbon-silicon composite material for a lithium battery, which comprises the following steps: step 1, putting the nano carbon material and the nano silicon material into absolute ethyl alcohol, uniformly stirring, and then putting into a ball mill for ball milling reaction for 1-3 hours at constant temperature to obtain mixed alcohol liquid; step 2, adding hydroxypropyl cellulose into the mixed alcohol solution, uniformly stirring, and carrying out ultrasonic reaction for 30-60min to obtain a dispersion suspension; step 3, putting the dispersed suspension into a reduced pressure distillation kettle, and carrying out reduced pressure distillation reaction for 30-70min to obtain viscous liquid; step 4, adding the viscous liquid into distilled water, uniformly stirring, and putting the viscous liquid into a grinding tool for gradient curing distillation reaction for 3-6 hours to obtain a carbon-silicon composite prefabricated body; and 5, adding the carbon-silicon composite preform into a reaction kettle for a gradient oxygen-free carbonization reaction for 5-7 hours to obtain the carbon-silicon composite nano material. The invention solves the problems of easy pulverization and pulverization of the carbon-silicon composite particles in the prior art.
Description
Technical Field
The invention belongs to the technical field of lithium batteries, and particularly relates to a preparation method of a high-performance carbon-silicon composite material for a lithium battery.
Background
Lithium ion batteries are a device of great interest for energy storage. In recent years, lithium ion batteries have been widely used in portable electronic devices, and also have attracted attention for use in transportation vehicles such as automobiles.
The working principle of the lithium ion battery is roughly as follows: the anode (i.e., negative electrode) absorbs lithium ions from the cathode as the battery is charged and absorbs electrons from the external circuit through the charging device, releasing these ions and electrons back to the cathode as the battery is discharged. The specific mass capacity is an important parameter of the anode material because it determines the amount of lithium ions that the battery system can retain. Another important parameter, which directly affects the service life of the battery system, is the cyclability of the anode material, i.e. the number of cycles that the anode material is able to absorb and release lithium ions without degradation or without significant loss of capacity.
Graphite carbon anodes are mostly adopted in the current lithium ion batteries. The graphitic carbon has a low volume change during the binding process with lithium ions, and thus has high cyclicity and safety. However, its specific mass capacity is low, with a theoretical limit of 372mAh/g graphite, which corresponds to about 1/10 of the specific mass capacity of 4235mAh/g lithium theoretically achievable with lithium metal.
Alternatively, silicon has certain advantages as the anode of lithium ion battery systems, for example binary compounds of lithium and silicon have a very high lithium content, up to the theoretical value of Li4.4And (3) Si. However, when using silicon as anode, the insertion and extraction of lithium is also accompanied by a very large volume expansion which leads to a very strong grain stress load and thus to a fragmentation and pulverization of the particles with loss of electrical contact.
Disclosure of the invention
Aiming at the problems in the prior art, the invention provides a preparation method of a high-performance carbon-silicon composite material for a lithium battery, which solves the problems of easy fragmentation and pulverization of carbon-silicon composite particles in the prior art.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
a preparation method of a high-performance carbon-silicon composite material for a lithium battery comprises the following steps:
step 1, putting the nano carbon material and the nano silicon material into absolute ethyl alcohol, uniformly stirring, and then putting into a ball mill for ball milling reaction for 1-3 hours at constant temperature to obtain mixed alcohol liquid;
step 2, adding hydroxypropyl cellulose into the mixed alcohol solution, uniformly stirring, and carrying out ultrasonic reaction for 30-60min to obtain a dispersion suspension;
step 3, putting the dispersed suspension into a reduced pressure distillation kettle, and carrying out reduced pressure distillation reaction for 30-70min to obtain viscous liquid;
step 4, adding the viscous liquid into distilled water, uniformly stirring, and putting the viscous liquid into a grinding tool for gradient solidification distillation reaction for 3-6 hours to obtain a carbon-silicon composite prefabricated body;
and 5, adding the carbon-silicon composite preform into a reaction kettle for a gradient oxygen-free carbonization reaction for 5-7 hours to obtain the carbon-silicon composite nano material.
The adding amount of the nano silicon material in the step 1 is 50-60% of the mass of the nano carbon material, and the concentration of the nano carbon material in the absolute ethyl alcohol is 30-60 g/L.
The stirring speed in the step 1 is 500-800r/min, and the ball milling reaction temperature is 50-60 ℃.
The adding amount of the hydroxypropyl cellulose in the step 2 is 5-10% of the mass of the nano carbon material, and the rotating speed for uniformly stirring is 300-500 r/min.
The temperature of the ultrasonic reaction in the step 2 is 20-30 ℃, and the ultrasonic frequency is 30-50 kHz.
The pressure of the reduced pressure distillation reaction in the step 3 is 60-70 ℃ of the atmospheric pressure, the temperature is 80-90 ℃, and the volume of the viscous liquid is 10-15% of the volume of the dispersion suspension liquid.
The adding amount of the distilled water in the step 4 is 150-:
| temperature of | Time |
| 70-80℃ | 20-30min |
| 90-100℃ | 30-40min |
| 120℃ | Time remaining |
The gradient oxygen-free carbonization reaction in the step 5 adopts an inert gas atmosphere, and the carbonization reaction procedure is as follows
| Temperature of | Time |
| 150-200℃ | 30-50min |
| 400-450℃ | 30-50min |
| 700-800℃ | 100-140min |
| 900-1000℃ | Time remaining |
Step 1, mixing the nano carbon material and the nano silicon material in absolute ethyl alcohol, and carrying out constant-temperature ball milling to ensure that the nano carbon material and the nano silicon material are in the same particle size range, and simultaneously forming a mixed precipitate with good mixing uniformity under the condition of full stirring.
And 2, adding hydroxypropyl cellulose into the mixed alcohol solution, and allowing the hydroxypropyl cellulose to act on the surfaces of the nano carbon material and the nano silicon material under an ultrasonic reaction to form a good dispersion system to obtain a suspension.
And 3, carrying out reduced pressure distillation reaction on the dispersed suspension to remove the absolute ethyl alcohol to form viscous liquid, so as to achieve the viscosity.
And 4, adding distilled water into the viscous liquid to form an ethanol aqueous solution to achieve a good mutual dissolving effect, simultaneously placing the solution into a mold to perform gradient solidification evaporation reaction, removing the ethanol by a gradient reaction mode, then removing the distilled water to form good solidification to obtain a preform structure, and completely connecting the nano silicon material and the nano carbon material by using hydroxypropyl cellulose as a binder.
And 5, performing gradient pentacarbonization reaction on the preform, forming gradient reaction by using a gradient reaction mode, preferentially removing residual solvent impurities, and then improving the cohesiveness and the cohesiveness firmness of the hydroxypropyl cellulose.
From the above description, it can be seen that the present invention has the following advantages:
1. the invention solves the problems of easy pulverization and pulverization of the carbon-silicon composite particles in the prior art.
2. The invention adopts the nano carbon material and the nano silicon material as the carbon source and the silicon source to form good mixing property, thereby being beneficial to improving understanding of the carbon source and the silicon source.
3. The invention adopts the hydroxypropyl cellulose as the binder and the dispersant, not only can form a good dispersion system, but also can be used as the binder of the nano material, and can form a good connection effect.
Detailed Description
The present invention is described in detail with reference to examples, but the present invention is not limited to the claims.
Example 1
A preparation method of a high-performance carbon-silicon composite material for a lithium battery comprises the following steps:
step 1, putting a nano carbon material and a nano silicon material into absolute ethyl alcohol, uniformly stirring, and then putting into a ball mill for constant-temperature ball milling reaction for 1h to obtain a mixed alcohol solution;
step 2, adding hydroxypropyl cellulose into the mixed alcohol solution, uniformly stirring, and carrying out ultrasonic reaction for 30min to obtain a dispersion suspension;
step 3, putting the dispersed suspension into a reduced pressure distillation kettle for reduced pressure distillation reaction for 30min to obtain viscous liquid;
step 4, adding the viscous liquid into distilled water, uniformly stirring, and putting the viscous liquid into a grinding tool for gradient solidification distillation reaction for 3 hours to obtain a carbon-silicon composite prefabricated body;
and 5, adding the carbon-silicon composite preform into a reaction kettle for a gradient oxygen-free carbonization reaction for 5 hours to obtain the carbon-silicon composite nano material.
The adding amount of the nano silicon material in the step 1 is 50% of the mass of the nano carbon material, and the concentration of the nano carbon material in the absolute ethyl alcohol is 30 g/L.
The stirring speed in the step 1 is 500r/min, and the ball milling reaction temperature is 50 ℃.
The adding amount of the hydroxypropyl cellulose in the step 2 is 5% of the mass of the nano carbon material, and the rotating speed for uniformly stirring is 300 r/min.
The temperature of the ultrasonic reaction in the step 2 is 20 ℃, and the ultrasonic frequency is 30 kHz.
The pressure of the reduced pressure distillation reaction in the step 3 is 60 ℃ of the atmospheric pressure, the temperature is 80 ℃, and the volume of the viscous liquid is 10% of the volume of the dispersion suspension liquid.
The adding amount of the distilled water in the step 4 is 150% of the volume of the viscous liquid, and the gradient procedure of the gradient solidification distillation reaction is as follows:
| temperature of | Time |
| 70℃ | 20min |
| 90℃ | 30min |
| 120℃ | Time remaining |
The gradient oxygen-free carbonization reaction in the step 5 adopts an inert gas atmosphere, and the carbonization reaction procedure is as follows
| Temperature of | Time |
| 150℃ | 30min |
| 400℃ | 30min |
| 700℃ | 100min |
| 900℃ | Time remaining |
Example 2
A preparation method of a high-performance carbon-silicon composite material for a lithium battery comprises the following steps:
step 1, putting a nano carbon material and a nano silicon material into absolute ethyl alcohol, uniformly stirring, and then putting into a ball mill for constant-temperature ball milling reaction for 3 hours to obtain a mixed alcohol solution;
step 2, adding hydroxypropyl cellulose into the mixed alcohol solution, uniformly stirring, and carrying out ultrasonic reaction for 60min to obtain a dispersion suspension;
step 3, putting the dispersed suspension into a reduced pressure distillation kettle, and carrying out reduced pressure distillation reaction for 70min to obtain viscous liquid;
step 4, adding the viscous liquid into distilled water, uniformly stirring, and putting the viscous liquid into a grinding tool for gradient solidification distillation reaction for 6 hours to obtain a carbon-silicon composite prefabricated body;
and 5, adding the carbon-silicon composite preform into a reaction kettle for a gradient oxygen-free carbonization reaction for 7 hours to obtain the carbon-silicon composite nano material.
The adding amount of the nano silicon material in the step 1 is 60% of the mass of the nano carbon material, and the concentration of the nano carbon material in the absolute ethyl alcohol is 60 g/L.
The stirring speed in the step 1 is 800r/min, and the ball milling reaction temperature is 60 ℃.
The adding amount of the hydroxypropyl cellulose in the step 2 is 10% of the mass of the nano carbon material, and the rotating speed for uniformly stirring is 500 r/min.
The temperature of the ultrasonic reaction in the step 2 is 30 ℃, and the ultrasonic frequency is 50 kHz.
The pressure of the reduced pressure distillation reaction in the step 3 is 70 ℃ of the atmospheric pressure, the temperature is 90 ℃, and the volume of the viscous liquid is 15% of the volume of the dispersion suspension liquid.
The adding amount of the distilled water in the step 4 is 250% of the volume of the viscous liquid, and the gradient procedure of the gradient solidification distillation reaction is as follows:
| temperature of | Time |
| 80℃ | 30min |
| 100℃ | 40min |
| 120℃ | Time remaining |
The gradient oxygen-free carbonization reaction in the step 5 adopts an inert gas atmosphere, and the carbonization reaction procedure is as follows
| Temperature of | Time |
| 200℃ | 50min |
| 450℃ | 50min |
| 800℃ | 140min |
| 1000℃ | Time remaining |
Example 3
A preparation method of a high-performance carbon-silicon composite material for a lithium battery comprises the following steps:
step 1, putting a nano carbon material and a nano silicon material into absolute ethyl alcohol, uniformly stirring, and then putting into a ball mill for constant-temperature ball milling reaction for 2 hours to obtain a mixed alcohol solution;
step 2, adding hydroxypropyl cellulose into the mixed alcohol solution, uniformly stirring, and carrying out ultrasonic reaction for 50min to obtain a dispersion suspension;
step 3, putting the dispersed suspension into a reduced pressure distillation kettle for reduced pressure distillation reaction for 50min to obtain viscous liquid;
step 4, adding the viscous liquid into distilled water, uniformly stirring, and putting the viscous liquid into a grinding tool for gradient curing distillation reaction for 5 hours to obtain a carbon-silicon composite prefabricated body;
and 5, adding the carbon-silicon composite preform into a reaction kettle for a gradient oxygen-free carbonization reaction for 6 hours to obtain the carbon-silicon composite nano material.
The adding amount of the nano silicon material in the step 1 is 55% of the mass of the nano carbon material, and the concentration of the nano carbon material in the absolute ethyl alcohol is 50 g/L.
The stirring speed in the step 1 is 700r/min, and the ball milling reaction temperature is 55 ℃.
The adding amount of the hydroxypropyl cellulose in the step 2 is 8% of the mass of the nano carbon material, and the rotating speed for uniformly stirring is 400 r/min.
The temperature of the ultrasonic reaction in the step 2 is 25 ℃, and the ultrasonic frequency is 40 kHz.
The pressure of the reduced pressure distillation reaction in the step 3 is 65 ℃ of the atmospheric pressure, the temperature is 85 ℃, and the volume of the viscous liquid is 13% of the volume of the dispersion suspension liquid.
The adding amount of the distilled water in the step 4 is 210% of the volume of the viscous liquid, and the gradient procedure of the gradient solidification distillation reaction is as follows:
| temperature of | Time |
| 75℃ | 25min |
| 95℃ | 35min |
| 120℃ | Time remaining |
The gradient oxygen-free carbonization reaction in the step 5 adopts an inert gas atmosphere, and the carbonization reaction procedure is as follows
| Temperature of | Time |
| 180℃ | 40min |
| 430℃ | 40min |
| 750℃ | 120min |
| 950℃ | Time remaining |
Performance detection
| Example 1 | Example 2 | Example 3 | |
| Specific surface area | 257.2m2/g | 298.4m2/g | 312.6m2/g |
| Pore volume | 0.45cc/g | 0.46cc/g | 0.48cc/g |
| First discharge capacity | 2044mAh/g | 2134mAh/g | 2289mAh/g |
| First charge capacity | 1695mAh/g | 1623mAh/g | 1787mAh/g |
| Stability of 100 cycles | 91％ | 92％ | 93％ |
In summary, the invention has the following advantages:
1. the invention solves the problems of easy pulverization and pulverization of the carbon-silicon composite particles in the prior art.
2. The invention adopts the nano carbon material and the nano silicon material as the carbon source and the silicon source to form good mixing property, thereby being beneficial to improving understanding of the carbon source and the silicon source.
3. The invention adopts the hydroxypropyl cellulose as the binder and the dispersant, not only can form a good dispersion system, but also can be used as the binder of the nano material, and can form a good connection effect.
It should be understood that the detailed description of the invention is merely illustrative of the invention and is not intended to limit the invention to the specific embodiments described. It will be appreciated by those skilled in the art that the present invention may be modified or substituted equally as well to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.
Claims (1)
1. A preparation method of a high-performance carbon-silicon composite material for a lithium battery is characterized by comprising the following steps: the method comprises the following steps:
step 1, putting the nano carbon material and the nano silicon material into absolute ethyl alcohol, uniformly stirring, and then putting into a ball mill for ball milling reaction for 1-3 hours at constant temperature to obtain mixed alcohol liquid;
step 2, adding hydroxypropyl cellulose into the mixed alcohol solution, uniformly stirring, and carrying out ultrasonic reaction for 30-60min to obtain a dispersion suspension;
step 3, putting the dispersed suspension into a reduced pressure distillation kettle, and carrying out reduced pressure distillation reaction for 30-70min to obtain viscous liquid;
step 4, adding the viscous liquid into distilled water, uniformly stirring, and putting the viscous liquid into a grinding tool for gradient curing distillation reaction for 3-6 hours to obtain a carbon-silicon composite prefabricated body;
step 5, adding the carbon-silicon composite preform into a reaction kettle for a gradient oxygen-free carbonization reaction for 5-7 hours to obtain a carbon-silicon composite nano material;
the adding amount of the nano silicon material in the step 1 is 50-60% of the mass of the nano carbon material, and the concentration of the nano carbon material in the absolute ethyl alcohol is 30-60 g/L;
the stirring speed in the step 1 is 500-800r/min, and the ball milling reaction temperature is 50-60 ℃;
the adding amount of the hydroxypropyl cellulose in the step 2 is 5-10% of the mass of the nano carbon material, and the rotating speed for uniformly stirring is 300-500 r/min;
the temperature of the ultrasonic reaction in the step 2 is 20-30 ℃, and the ultrasonic frequency is 30-50 kHz;
the pressure of the reduced pressure distillation reaction in the step 3 is 60-70 ℃ of the atmospheric pressure, the temperature is 80-90 ℃, and the volume of the viscous liquid is 10-15% of the volume of the dispersion suspension liquid;
the adding amount of the distilled water in the step 4 is 150-:
first gradient, keeping at 80-90 deg.C for 20-30 min; a second gradient, which is kept at the temperature of 900-100 ℃ for 30-40 min; a third gradient, which is kept at 120 ℃ until the reaction is finished;
the gradient oxygen-free carbonization reaction in the step 5 adopts an inert gas atmosphere, and the carbonization reaction procedure is as follows:
the first gradient is maintained at the temperature of 150-200 ℃ for 30-50min, the second gradient is maintained at the temperature of 400-450 ℃ for 30-50min, the third gradient is maintained at the temperature of 700-800 ℃ for 140min, and the fourth gradient is maintained at the temperature of 900-1000 ℃ until the reaction is finished.
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| CN103107315B (en) * | 2011-11-10 | 2016-03-30 | 北京有色金属研究总院 | A kind of nano-silicone wire/carbon composite material and preparation method thereof |
| CN102891297B (en) * | 2012-11-10 | 2015-05-13 | 江西正拓新能源科技股份有限公司 | Silicon-carbon composite material for lithium ion battery and preparation method thereof |
| CN102983310A (en) * | 2012-11-20 | 2013-03-20 | 江苏科捷锂电池有限公司 | Preparation method of nano-silicon carbide cathode material |
| JP6621994B2 (en) * | 2015-02-17 | 2019-12-18 | 大阪瓦斯株式会社 | Negative electrode material for lithium secondary battery and method for producing the same, composition for negative electrode active material layer for lithium secondary battery using the negative electrode material, negative electrode for lithium secondary battery, and lithium secondary battery |
| CN104716312B (en) * | 2015-03-11 | 2017-03-22 | 中国科学院化学研究所 | Silicon-carbon composite material for lithium ion battery, preparation method and application of silicon-carbon composite material |
| CN107204438B (en) * | 2016-03-17 | 2021-05-04 | 国家纳米科学中心 | Carbon-silicon composite material and preparation method and application thereof |
| KR101822744B1 (en) * | 2016-05-19 | 2018-01-30 | 숭실대학교산학협력단 | Preparing method for carbon nanofibers composites comprising silicon/ silicon nitride and silicon carbide core-shell composites |
| CN106257716B (en) * | 2016-08-30 | 2019-01-11 | 浙江超威创元实业有限公司 | A kind of preparation method and lithium ion battery of silicon-carbon composite cathode material |
| CN106450187B (en) * | 2016-10-11 | 2019-02-19 | 绍兴文理学院 | A kind of tertiary cathode material and preparation method thereof |
| CN107658452B (en) * | 2017-09-19 | 2020-06-12 | 合肥国轩高科动力能源有限公司 | Silicon/carbon nanotube/silicon oxycarbide composite material and preparation method and application thereof |
| CN107785552B (en) * | 2017-10-24 | 2020-09-01 | 武汉理工大学 | Nitrogen-doped flower-like hierarchical structure porous carbon-selenium composite positive electrode material and preparation method and application thereof |
| CN107845797B (en) * | 2017-11-02 | 2020-04-21 | 洛阳联创锂能科技有限公司 | Nano silicon-carbon composite negative electrode material for lithium ion battery and preparation method thereof |
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