CN110544766A - Expanded graphite nano-silicon composite negative electrode material and preparation method thereof - Google Patents
Expanded graphite nano-silicon composite negative electrode material and preparation method thereof Download PDFInfo
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- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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- Y02E60/10—Energy storage using batteries
Abstract
an expanded graphite nano-silicon composite negative electrode material and a preparation method thereof relate to a silicon-carbon composite negative electrode material and a preparation method thereof. The expanded graphite nano-silicon composite negative electrode material is prepared from a nano-silicon turbid liquid, expanded graphite and a wrapped carbon source. The preparation method comprises the following steps: firstly, preparing a nano silicon suspension; mixing and stirring the expanded graphite and the nano-silicon turbid liquid; then heating and drying the graphite oxide under protective atmosphere to obtain an expanded graphite nano-silicon composite; and thirdly, mixing the expanded graphite nano-silicon composite with a wrapping carbon source, and then heating and carbonizing. The expanded graphite in the expanded graphite nano-silicon composite negative electrode material has the characteristics of natural graphite and also has the unique property of the expanded graphite. The preparation method disclosed by the invention is simple in process, strong in operability, low in production cost and easier to realize large-scale generation.
Description
Technical Field
the invention relates to a silicon-carbon composite negative electrode material and a preparation method thereof.
background
With the rapid development of technology, batteries require higher energy density, longer cycle life, and higher safety performance. The cathode material is an important component of the lithium ion battery and is also the focus of research on the lithium ion battery. At present, the graphite type negative electrode material accounts for more than 90% of the market share, but the gram capacity of the graphite type negative electrode material can be 360mAh/g, which is close to the theoretical value of 372mAh/g, and the upward space is very limited.
The silicon and the carbon have similar chemical properties, the theoretical gram capacity is as high as 4200mAh/g, and the silicon-carbon composite anode material is a novel generation anode material with great potential. But silicon is easy to generate volume expansion (more than 300 percent) in the charging and discharging processes, and continuously consumes electrolyte to generate an SEI film, so that Li + is consumed, the capacity is reduced, and the cycle is poor; moreover, silicon is a semiconductor material, and the conductivity is far lower than that of graphite, so that the application of silicon in the aspect of lithium ion battery cathode materials is seriously influenced by the problems.
disclosure of Invention
the invention aims to provide a lithium battery negative electrode material and a preparation method thereof.
The expanded graphite nano-silicon composite negative electrode material is prepared from a nano-silicon turbid liquid, expanded graphite and a wrapped carbon source.
The expanded graphite nano-silicon composite negative electrode material is prepared by the following method:
firstly, preparing a nano silicon suspension;
Mixing and stirring the expanded graphite and the nano-silicon turbid liquid; then heating and drying the graphite oxide under protective atmosphere to obtain an expanded graphite nano-silicon composite;
and thirdly, mixing the expanded graphite nano-silicon composite body with a wrapping carbon source, and then heating and carbonizing to obtain the expanded graphite nano-silicon composite cathode material.
The expanded graphite in the expanded graphite nano-silicon composite negative electrode material has the characteristics of natural graphite and also has the unique property of the expanded graphite. The expanded graphite has high expansion rate, conductive performance and specific compression resilience, not only provides space for the expansion of silicon, but also can better play the high-capacity property of the silicon, and simultaneously avoids the problems of potential safety hazard and service life caused by the expansion); and the expanded graphite can rebound in the process of silicon delithiation, so that a channel is provided for Li + movement when the silicon volume is reduced, the conductivity is enhanced, and the rate capability of the lithium ion battery is improved. The amorphous carbon coated on the outermost layer protects the expanded graphite and the nano-silicon in a certain space, so that the machining performance of the material is ensured; the preparation method disclosed by the invention is simple in process, strong in operability, low in production cost and easier to realize large-scale generation.
Detailed Description
The first embodiment is as follows: the expanded graphite nano-silicon composite negative electrode material is prepared from a nano-silicon turbid liquid, expanded graphite and a wrapped carbon source.
The second embodiment is as follows: the present embodiment is different from the first embodiment in that: the nano-silicon suspension is formed by mixing nano-silicon and dispersion liquid, and the dispersion liquid is selected from industrial oil or vegetable oil. The rest is the same as the first embodiment.
in the embodiment, the dispersion liquid is adopted to suspend the nano silicon, and the amorphous carbon is formed after the dispersion liquid is carbonized, so that the particle conductivity can be obviously enhanced, and the charging and discharging speed of the lithium ion battery is improved. In this embodiment, the industrial oil is gasoline or diesel oil, and the vegetable oil is soybean oil, peanut oil, or rapeseed oil.
the third concrete implementation mode: the present embodiment is different from the first or second embodiment in that: the solid content of the nano-silicon in the nano-silicon suspension is 1 to 15 percent. The other is the same as in the first or second embodiment.
The fourth concrete implementation mode: the present embodiment is different from one of the first to third embodiments in that: the grain size of the nano silicon is D50 not more than 100nm, and the purity of the nano silicon is not less than 99.9%. The others are the same as in one of the first to third embodiments.
the fifth concrete implementation mode: the present embodiment is different from one of the first to fourth embodiments in that: the mass ratio of the nano-silicon suspension to the expanded graphite is 28-40: 1. The other is the same as one of the first to fourth embodiments.
The sixth specific implementation mode: the present embodiment is different from one of the first to fifth embodiments in that: the purity of the expanded graphite is more than or equal to 99.95%, and the granularity of the expanded graphite is 14-25 mu m. The other is the same as one of the first to fifth embodiments.
The seventh embodiment: the present embodiment is different from one of the first to sixth embodiments in that: and mixing and drying the nano-silicon turbid liquid and the expanded graphite to form an expanded graphite nano-silicon complex, and then mixing the wrapped carbon source and the expanded graphite nano-silicon complex according to a mass ratio of 1-5: 10. The other is the same as one of the first to sixth embodiments.
the specific implementation mode is eight: the present embodiment is different from the first to seventh embodiments in that: the carbon source is asphalt, resin or alcohol organic compound. The other is the same as one of the first to seventh embodiments.
The specific implementation method nine: the expanded graphite nano-silicon composite negative electrode material is prepared by the following method:
Firstly, preparing a nano silicon suspension;
Mixing and stirring the expanded graphite and the nano-silicon turbid liquid; then heating and drying the graphite oxide under protective atmosphere to obtain an expanded graphite nano-silicon composite;
And thirdly, mixing the expanded graphite nano-silicon composite body with a wrapping carbon source, and then heating and carbonizing to obtain the expanded graphite nano-silicon composite cathode material.
The nano-silicon suspension solvent can be recovered by heating and drying in the second step of the embodiment. The surface of the particles of the expanded graphite nano-silicon composite negative electrode material prepared by the embodiment is not attached with silicon particles, the nano-silicon is completely coated in the natural graphite and the amorphous carbon, and the silicon is not contacted with the electrolyte, so that a stable SEI (solid electrolyte interphase) film is formed on the negative electrode of the lithium ion battery, and the cycle service life of the negative electrode material is prolonged.
the detailed implementation mode is ten: the present embodiment is different from the ninth embodiment in that: and step two, drying, namely reducing the water content of the expanded graphite nano silicon composite to below 1%. The rest is the same as the embodiment nine.
The concrete implementation mode eleven: this embodiment is different from the ninth or tenth embodiment in that: the heating carbonization treatment in the third step is divided into 2 stages of heating and carbonization,
a heating stage: heating the expanded graphite nano-silicon composite and the carbon source wrapping mixture to 150-350 ℃ under a protective atmosphere, keeping the temperature for 0.5-2 hours, continuously heating to 500-700 ℃, keeping the temperature for 0.5-5 hours, and then cooling to room temperature;
and (3) carbonization: and heating the material cooled in the heating stage in a protective atmosphere at 800-1300 ℃, keeping the temperature for 1-5 hours, and cooling to room temperature. The others are the same as the ninth or tenth embodiment.
the specific implementation mode twelve: this embodiment is different from one of the ninth to eleventh embodiments in that: the nano-silicon suspension is formed by mixing nano-silicon and dispersion liquid, and the dispersion liquid is selected from industrial oil or vegetable oil. The others are the same as in one of the ninth to eleventh embodiments.
The specific implementation mode is thirteen: this embodiment is different from the ninth to twelfth embodiment in that: the solid content of the nano-silicon in the nano-silicon suspension is 1 to 15 percent. The rest is the same as the ninth to twelfth embodiments.
The specific implementation mode is fourteen: this embodiment is different from one of the ninth to thirteenth embodiments in that: the industrial oil is gasoline or diesel oil, and the vegetable oil is soybean oil, peanut oil or rapeseed oil. The others are the same as in one of the ninth to thirteenth embodiments.
the concrete implementation mode is fifteen: this embodiment is different from one of the ninth to fourteenth embodiments in that: the mass ratio of the nano-silicon turbid liquid to the expanded graphite is 28-40: 1. The others are the same as in one of the ninth to the fourteenth embodiments.
the specific implementation mode is sixteen: the present embodiment is different from one of the ninth to fifteenth embodiments in that: and mixing and drying the nano-silicon turbid liquid and the expanded graphite to form an expanded graphite nano-silicon complex, and then mixing the wrapped carbon source and the expanded graphite nano-silicon complex according to a mass ratio of 1-5: 10. The others are the same as in one of the ninth to fifteenth embodiments.
Seventeenth embodiment: this embodiment is different from one of the ninth to sixteenth embodiments in that: the grain size of the nano silicon is D50 not more than 100nm, and the purity of the nano silicon is not less than 99.9%. The others are the same as in one of the ninth to sixteenth embodiments.
The specific implementation mode is eighteen: this embodiment is different from one of the ninth to seventeenth embodiments in that: the purity of the expanded graphite is more than or equal to 99.95%, and the granularity of the expanded graphite is 14-25 mu m. The others are the same as in one of the ninth to seventeenth embodiments.
The detailed embodiment is nineteen: this embodiment is different from one of the ninth to eighteen embodiments in that: the carbon source is asphalt, resin or alcohol organic compound. The others are the same as in one of the ninth to eighteen embodiments.
Example 1
The expanded graphite silicon carbon composite negative electrode material of the embodiment is prepared by the following method:
Firstly, preparing a nano silicon suspension;
mixing and stirring the expanded graphite and the nano-silicon turbid liquid; then heating and drying the graphite oxide in the nitrogen atmosphere to obtain an expanded graphite nano-silicon composite;
And thirdly, mixing the expanded graphite nano-silicon composite body with a wrapping carbon source, and then heating and carbonizing to obtain the expanded graphite nano-silicon composite cathode material.
drying in the second step, and reducing the water content of the expanded graphite nano silicon composite to below 1%;
the heating carbonization treatment in the third step is divided into 2 stages of heating and carbonization,
A heating stage: heating the expanded graphite nano-silicon composite and the mixture wrapping the carbon source to 350 ℃ under the nitrogen atmosphere, keeping the temperature for 40min, continuing to heat to 550 ℃, keeping the temperature for 2.5 hours, and then cooling to room temperature;
and (3) carbonization: heating the material cooled in the heating stage at 1100 ℃ in a nitrogen atmosphere, keeping the temperature for 3 hours, and cooling to room temperature;
The nano-silicon suspension is formed by mixing nano-silicon and dispersion liquid according to the proportion of 50g to 1800g, and the dispersion liquid is soybean oil;
Stirring and mixing the nano-silicon turbid liquid and the expanded graphite according to a ratio of 1850g to 50g for adsorption;
mixing and drying the nano-silicon turbid liquid and the expanded graphite to form an expanded graphite nano-silicon complex, and then mixing the wrapped carbon source and the expanded graphite nano-silicon complex according to the mass ratio of 30: 1900; the carbon source is coated by asphalt, and the granularity of the asphalt is D50-5 mu m; the grain diameter of the nano silicon is D50-60 nm, and the purity of the nano silicon is more than or equal to 99.9%; the purity of the expanded graphite is more than or equal to 99.95 percent, and the particle size of the expanded graphite is D50-20 mu m.
Comparative example 1:
the preparation method of the embodiment is as follows:
Uniformly dispersing nano silicon powder according to the proportion that 50g of nano silicon powder (D50-60 nm), 50g of artificial graphite and 30g of asphalt are added into 200g of washing oil to obtain a mixed dispersion liquid;
Heating the mixed dispersion to 320 ℃, keeping the temperature for 1 hour, continuously heating to 400 ℃, keeping the temperature for 0.5 hour, continuously heating to 550 ℃, keeping the temperature for 1.5 hours, cooling to room temperature, and carrying out nitrogen protection in the whole process;
And heating to 1250 ℃ under the protection of nitrogen again, keeping the temperature for 2 hours, and cooling to room temperature to obtain the silicon-carbon composite cathode material.
comparative example 2:
The preparation method of the embodiment is as follows:
50g of expanded graphite with high expansion rate is placed in a rotary furnace, and the temperature is raised to 700 ℃ under the protection of nitrogen;
Introducing SiCl4 gas at a flow rate of 1L/min, introducing a mixed gas of H2 and Ar at the same time, wherein the volume ratio of H2 to Ar is 1:49, the flow rate is 5L/min, and continuously introducing for 1 hour;
stopping introducing SiCl4 gas, stopping introducing the mixed gas for 15 minutes, and continuously introducing N2 gas to cool to room temperature;
And uniformly mixing the expanded graphite subjected to vapor deposition with 30g of asphalt, heating to 600 ℃ in a nitrogen atmosphere, keeping the temperature for 2 hours, and cooling to obtain the silicon-carbon composite negative electrode material.
Example 2
the expanded graphite silicon carbon composite negative electrode material of the embodiment is prepared by the following method:
firstly, preparing a nano silicon suspension;
Mixing and stirring the expanded graphite and the nano-silicon turbid liquid; then heating and drying the graphite oxide in the nitrogen atmosphere to obtain an expanded graphite nano-silicon composite;
and thirdly, mixing the expanded graphite nano-silicon composite body with a wrapping carbon source, and then heating and carbonizing to obtain the expanded graphite nano-silicon composite cathode material.
Drying in the second step, and reducing the water content of the expanded graphite nano silicon composite to below 1%;
the heating carbonization treatment in the third step is divided into 2 stages of heating and carbonization,
a heating stage: heating the expanded graphite nano-silicon composite and the mixture wrapping the carbon source to 320 ℃ in the nitrogen atmosphere, keeping the temperature for 60min, continuing to heat to 600 ℃, keeping the temperature for 2 hours, and then cooling to room temperature;
And (3) carbonization: heating the material cooled in the heating stage at 1100 ℃ in a nitrogen atmosphere, keeping the temperature for 3 hours, and cooling to room temperature;
the nano-silicon suspension is formed by mixing nano-silicon and dispersion liquid according to the proportion of 50g to 1850g, and the dispersion liquid is diesel oil;
Stirring and mixing the nano-silicon turbid liquid and the expanded graphite according to a ratio of 1900g to 50g for adsorption;
Mixing and drying the nano-silicon turbid liquid and the expanded graphite to form an expanded graphite nano-silicon composite, and then mixing the wrapped carbon source and the expanded graphite nano-silicon composite according to the mass ratio of 20: 1950; the carbon source is coated by asphalt, and the granularity of the asphalt is D50-5 mu m; the grain diameter of the nano silicon is D50-60 nm, and the purity of the nano silicon is more than or equal to 99.9%; the purity of the expanded graphite is more than or equal to 99.95 percent, and the particle size of the expanded graphite is D50-20 mu m.
example 3
The expanded graphite silicon carbon composite negative electrode material of the embodiment is prepared by the following method:
firstly, preparing a nano silicon suspension;
mixing and stirring the expanded graphite and the nano-silicon turbid liquid; then heating and drying the graphite oxide in the nitrogen atmosphere to obtain an expanded graphite nano-silicon composite;
And thirdly, mixing the expanded graphite nano-silicon composite body with a wrapping carbon source, and then heating and carbonizing to obtain the expanded graphite nano-silicon composite cathode material.
Drying in the second step, and reducing the water content of the expanded graphite nano silicon composite to below 1%;
the heating carbonization treatment in the third step is divided into 2 stages of heating and carbonization,
A heating stage: heating the expanded graphite nano-silicon composite and the carbon source coating mixture to 380 ℃ under the nitrogen atmosphere, keeping the temperature for 30min, continuing to heat to 600 ℃, keeping the temperature for 1.5 h, and cooling to room temperature;
and (3) carbonization: heating the material cooled in the heating stage to 1250 ℃ in a nitrogen atmosphere, keeping the temperature for 2 hours, and cooling to room temperature;
the nano-silicon suspension is formed by mixing nano-silicon and dispersion liquid according to the proportion of 50g to 1800g, and the dispersion liquid is soybean oil;
Stirring and mixing the nano-silicon turbid liquid and the expanded graphite according to a ratio of 1850g to 50g for adsorption;
Mixing and drying the nano-silicon turbid liquid and the expanded graphite to form an expanded graphite nano-silicon composite, and then mixing the wrapped carbon source and the expanded graphite nano-silicon composite according to the mass ratio of 20: 1950; the carbon source is coated by asphalt, and the granularity of the asphalt is D50-5 mu m; the grain diameter of the nano silicon is D50-40 nm, and the purity of the nano silicon is more than or equal to 99.9%; the purity of the expanded graphite is more than or equal to 99.95 percent, and the granularity of the expanded graphite is D50-17 mu m.
Experiment:
the silicon-carbon composite negative electrode materials prepared in the examples 1 to 3 and the comparative examples 1 to 2 were used to prepare lithium ion batteries, and then electrochemical tests were performed. The test results are shown in table 1.
TABLE 1
compared with the comparative experiment 1, the invention has higher first discharge capacity and cycle life and better service performance through the comparison of the implementation cases 1-3; compared with the comparative experiment 2, the implementation cases 1-3 have the advantages of simple process, convenient operation, no toxicity, contribution to controlling the generation cost and capability of saving the cost by 20-40% in the statistical calculation of the experiment cost.
Claims (10)
1. The expanded graphite nano-silicon composite negative electrode material is characterized by being prepared from a nano-silicon turbid liquid, expanded graphite and a wrapped carbon source.
2. The expanded graphite nano-silicon composite anode material as claimed in claim 1, wherein the nano-silicon suspension is formed by mixing nano-silicon and a dispersion liquid, and the dispersion liquid is selected from industrial oil or vegetable oil.
3. the expanded graphite nano-silicon composite anode material as claimed in claim 2, wherein the solid content of nano-silicon in the nano-silicon suspension is 1-15%.
4. the expanded graphite nano-silicon composite negative electrode material as claimed in claim 1, wherein the mass ratio of the nano-silicon suspension to the expanded graphite is 28-40: 1.
5. the expanded graphite nano-silicon composite negative electrode material as claimed in claim 1, wherein the nano-silicon suspension and the expanded graphite are mixed and dried to form an expanded graphite nano-silicon composite, and then the coated carbon source and the expanded graphite nano-silicon composite are mixed according to a mass ratio of 1-5: 10.
6. the method for preparing the expanded graphite nano-silicon composite negative electrode material as claimed in claim 1, wherein the expanded graphite nano-silicon composite negative electrode material is prepared by the following steps:
Firstly, preparing a nano silicon suspension;
Mixing and stirring the expanded graphite and the nano-silicon turbid liquid; then heating and drying the graphite oxide under protective atmosphere to obtain an expanded graphite nano-silicon composite;
and thirdly, mixing the expanded graphite nano-silicon composite body with a wrapping carbon source, and then heating and carbonizing to obtain the expanded graphite nano-silicon composite cathode material.
7. The method for producing the expanded graphite nano-silicon composite anode material according to claim 6, wherein the step two of drying reduces the moisture of the expanded graphite nano-silicon composite to 1% or less.
8. the method for preparing the expanded graphite nano-silicon composite anode material according to claim 6, characterized in that the heating carbonization treatment in the third step is divided into 2 stages of heating and carbonization,
A heating stage: heating the expanded graphite nano-silicon composite and the carbon source wrapping mixture to 150-350 ℃ under a protective atmosphere, keeping the temperature for 0.5-2 hours, continuously heating to 500-700 ℃, keeping the temperature for 0.5-5 hours, and then cooling to room temperature;
and (3) carbonization: and heating the material cooled in the heating stage in a protective atmosphere at 800-1300 ℃, keeping the temperature for 1-5 hours, and cooling to room temperature.
9. The method for preparing the expanded graphite nano-silicon composite negative electrode material as claimed in claim 6, wherein the nano-silicon suspension is formed by mixing nano-silicon and a dispersion liquid, and the dispersion liquid is selected from industrial oil or vegetable oil; the solid content of the nano-silicon in the nano-silicon suspension is 1 to 15 percent.
10. The preparation method of the expanded graphite nano-silicon composite negative electrode material as claimed in claim 6, wherein the mass ratio of the nano-silicon suspension to the expanded graphite is 28-40: 1; and mixing and drying the nano-silicon turbid liquid and the expanded graphite to form an expanded graphite nano-silicon complex, and then mixing the wrapped carbon source and the expanded graphite nano-silicon complex according to a mass ratio of 1-5: 10.
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| WO2021129125A1 (en) * | 2019-12-25 | 2021-07-01 | 广东凯金新能源科技股份有限公司 | Silicon-carbon composite negative electrode material with hollow core-shell structure, and preparation method therefor |
| WO2022121280A1 (en) * | 2020-12-07 | 2022-06-16 | 广东凯金新能源科技股份有限公司 | Pomegranate-like-structure silicon-based composite material, and preparation method therefor and application thereof |
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| CN105355870A (en) * | 2015-10-22 | 2016-02-24 | 清华大学深圳研究生院 | Expanded graphite and nano-silicon composite material, preparation method thereof, electrode plate and battery |
| JP2017130274A (en) * | 2016-01-18 | 2017-07-27 | 東ソー株式会社 | Negative electrode material for lithium secondary battery, manufacturing method thereof, and lithium secondary battery |
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| CN108063233A (en) * | 2017-12-20 | 2018-05-22 | 天津锦美碳材科技发展有限公司 | A kind of silicon-carbon cathode material and preparation method thereof |
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Application publication date: 20191206 |