CN111900368A - Lithium ion battery-grade silicon monoxide negative electrode material, and preparation method and application thereof - Google Patents
Lithium ion battery-grade silicon monoxide negative electrode material, and preparation method and application thereof Download PDFInfo
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Abstract
A lithium ion battery-grade silicon monoxide negative electrode material and a preparation method and application thereof are disclosed, wherein under the protective atmosphere, silicon monoxide and a lithium source are uniformly mixed, and after heat preservation is carried out at 300-700 ℃, pre-lithiated silicon monoxide is obtained; putting the pre-lithiated silicon monoxide into a rotary kiln, and performing carbon coating by adopting vapor deposition to obtain a pre-lithiated silicon monoxide/carbon composite material; and uniformly mixing the metal oxide and the pre-lithiated silicon oxide/carbon composite material to ensure that the metal oxide is uniformly coated on the surface of the silicon oxide/carbon composite material to obtain the lithium ion battery-grade silicon oxide negative electrode material. The invention improves the slurry stability and electrochemical performance of the pre-lithiated silicon oxide raw material through vapor deposition and metal oxide coating, and simultaneously, the invention has the advantages of simple process method, excellent performance and wide application prospect in lithium ion batteries.
Description
Technical Field
The invention belongs to the field of lithium ion battery negative electrode active material, and relates to a lithium ion battery-grade silicon monoxide negative electrode material, and a preparation method and application thereof.
Background
With the great development of economic society, environmental problems become important factors restricting economic development. Lithium ion batteries have received much attention from people because of their environmental protection advantages. In recent years, with the vigorous development of electric vehicles, fuel-oil vehicle sale prohibition dates have been proposed in many countries. At present, the endurance mileage of the electric automobile is generally 300-355 km, and the main reason for restricting further increase of endurance mileage is that the capacity of the currently commercialized graphite cathode is between 350-355mAh/g, which is close to the theoretical specific capacity of 372mAh/g, and is difficult to be greatly improved.
Silicon-based negative electrode materials are considered to be negative electrode materials of next-generation lithium ion batteries due to the advantages of high theoretical specific capacity, low price and the like, and mainly comprise two major types of nano silicon-based materials and silicon monoxide (SiO). Among them, much research has been started in about 2000 years on SiO materials, and the defects of low conductivity and high expansion of SiO can be effectively improved by coating hot carbon through vapor deposition, and at present, the energy density of a battery can be effectively improved by doping 3% -5% of SiO negative electrode materials in commercialized negative electrode materials, but the first coulombic efficiency of a conventional silicon monoxide negative electrode is only 76% -77% at present, and higher silicon monoxide doping amount is limited.
Aiming at the problem of low first rate of SiO, part of irreversible components are converted into lithium silicate (Li) by a lithium pre-supplement technology2SiO3、Li4SiO4、Li2Si2O5) The first coulombic efficiency of the silicon monoxide can be improved to 85-90 percent, and Li2Si2O5Has better water resistance, while Li2SiO3And Li4SiO4Then hydrophilic, where Li4SiO4The separation speed is high, and the separation speed is high,Li2SiO3will slowly precipitate due to Li during the pulp coating of the material2SiO3And Li4SiO4The pH of the slurry is increased, the material is agglomerated and then settled, the quality of a battery pole piece is affected, and finally the performance of the battery is deteriorated.
Disclosure of Invention
In order to solve the problem of poor stability of battery slurry after lithium is pre-supplemented by a silicon monoxide material in the prior art, the invention aims to provide a lithium ion battery-grade silicon monoxide negative electrode material and a preparation method thereof.
The invention also aims to provide application of the silicon monoxide negative electrode material of the lithium ion battery in preparation of the lithium ion battery.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a lithium ion battery-grade silicon monoxide negative electrode material comprises the following steps:
s1, uniformly mixing the silicon monoxide with a lithium source under a protective atmosphere, and preserving heat at 300-700 ℃ to obtain pre-lithiated silicon monoxide;
s2, putting the pre-lithiated silicon monoxide into a rotary kiln, and performing carbon coating by adopting vapor deposition to obtain a pre-lithiated silicon monoxide/carbon composite material;
and S3, uniformly mixing the metal oxide with the pre-lithiated silicon oxide/carbon composite material to ensure that the metal oxide is uniformly coated on the surface of the silicon oxide/carbon composite material to obtain the lithium ion battery-grade silicon oxide negative electrode material.
In a further improvement of the present invention, in the step S1, the mass ratio of the silicon monoxide to the lithium source is 1: (0.01-1).
In a further improvement of the present invention, in step S1, the lithium source is LiH, inert lithium powder, lithium aluminum hydride, or lithium borohydride; the protective atmosphere is argon or nitrogen.
In a further development of the invention, in step S1, the median particle size of the silica is 5 to 8 μm and the median particle size of the inert lithium powder or LiH is 1 to 3 μm.
The further improvement of the present invention is that in the step S1, the temperature is raised from room temperature to 700 ℃ at a temperature raising rate of 3-10 ℃/min, and the holding time is 1-10 h.
In a further improvement of the present invention, in step S2, the specific process of performing carbon coating by vapor deposition is as follows: introducing pyrolysis gas at the temperature of 700 ℃ and 900 ℃ and preserving heat for 1-10 h.
The invention is further improved in that the pyrolysis gas is one or a mixture of acetylene, methane, ethylene and propylene.
In a further improvement of the present invention, in step S3, the metal oxide is one of alumina, titania, magnesia and zirconia; the mass ratio of the metal oxide to the pre-lithiated silicon oxide/carbon composite material is (0.01-0.2): 1.
the lithium ion battery-grade silicon oxide negative electrode material is prepared according to the method.
The application of the lithium ion battery-grade silicon monoxide negative electrode material in the preparation of the lithium ion battery is provided.
Compared with the prior art, the invention has the following beneficial effects: on one hand, in the pre-lithium process, the type of the generated lithium silicate can be regulated and controlled by regulating and controlling the using amount and the type of the lithium source, so that the Li is improved2Si2O5In a ratio of (1), reduction of Li2SiO3、Li4SiO4On the other hand, the deposition of silicate and the sedimentation of the material can be inhibited by coating a layer of metal oxide on the surface of the material, which is of great help to improve the stability of the battery slurry. The invention improves the slurry stability and electrochemical performance of the pre-lithiated silicon oxide composite material through vapor deposition and metal oxide coating, and meanwhile, the process method provided by the invention is simple, has excellent performance and has wide application prospect in lithium ion batteries.
Drawings
Fig. 1 is a TEM image of a pre-lithiated silica/carbon composite anode material prepared in example 1.
Fig. 2 is a XRD test result of the pre-lithiated silicon oxide/carbon composite anode material prepared in example 1.
Detailed Description
The present invention will be described in detail with reference to specific examples.
According to the invention, the stability of the slurry can be effectively improved by metal oxide on the surface of the pre-lithiated silicon oxide material, and a layer of pyrolytic carbon is coated by vapor deposition, so that the silicon oxide negative electrode material with good water resistance, high capacity and good circulation is successfully prepared.
A preparation method of a silicon oxide negative electrode material comprises the following steps:
s1, under a protective atmosphere, uniformly mixing SiO and a lithium source in a glove box, taking out, placing in a tubular furnace, heating to 700 ℃ at 300 ℃, and preserving heat for a certain time to obtain pre-lithiated silicon monoxide;
s2, putting the pre-lithiated silicon monoxide into a rotary kiln, introducing pyrolysis gas at the temperature of 700-900 ℃ and preserving heat for a period of time to obtain a pre-lithiated silicon monoxide/carbon composite material;
and S3, uniformly mixing the metal oxide with the pre-lithiated silicon oxide/carbon composite material to ensure that the metal oxide can be uniformly coated on the surface of the composite material.
Preferably, the mass ratio of the silicon monoxide to the lithium source in step S1 is 1: (0.01-0.2);
preferably, the lithium source in step S1 is LiH, inert lithium powder, lithium borohydride, or lithium aluminum hydride;
preferably, the median particle size of the silica in step S1 is 5 to 6 μm, and the median particle size of the inert lithium powder or LiH is 1 to 2 μm.
Preferably, in the step S1, the temperature is raised from room temperature to 700 ℃ at a heating rate of 3-5 ℃/min, and the holding time is 1-3 h.
Preferably, in step S1, the protective atmosphere is argon or nitrogen.
Preferably, in the step S2, the temperature of the vapor deposition is 700-900 ℃, and the time is 1-10 h;
preferably, in step S2, the pyrolysis gas is one or a mixture of acetylene, methane, and ethylene and propylene;
preferably, the mixing manner in step S3 is solid phase mixing or liquid phase mixing;
preferably, in the step S3, the metal oxide is one of aluminum oxide, titanium oxide, magnesium oxide and zirconium oxide;
preferably, the mass ratio of the metal oxide to the pre-lithiated silica/carbon composite in the step S3 is (0.01-0.2): 1.
the invention also discloses application of the lithium ion battery-grade silicon monoxide negative electrode material in preparation of a lithium ion battery.
The following are specific examples.
Example 1
1) Under the protection of nitrogen, 100g of SiO with the median particle size of 5 microns and 10g of LiH with the median particle size of 1 micron are weighed in a glove box and are uniformly mixed, the mixture is heated to 500 ℃ from room temperature at the heating rate of 3 ℃/min, and the temperature is kept for 3 hours, so that the pre-lithiated silicon monoxide is obtained;
2) putting the pre-lithiated silicon monoxide obtained in the step (1) into a rotary kiln, heating to 800 ℃, introducing acetylene gas, and keeping the temperature for 1h to obtain a pre-lithiated silicon monoxide/carbon composite material;
3) weighing 5g of nano aluminum oxide, dispersing the nano aluminum oxide in 200g of ethanol, stirring for 24 hours to ensure uniform dispersion to obtain a solution, weighing 100g of the pre-lithiated silicon oxide/carbon composite material obtained in the step 2), adding the pre-lithiated silicon oxide/carbon composite material into the solution, stirring for 24 hours, filtering for three times, drying in a vacuum oven at 80 ℃, and drying for 12 hours to obtain the final lithium ion battery-grade silicon oxide negative electrode material.
Referring to fig. 1, it can be seen that the material has a uniformly coated carbon layer.
Referring to FIG. 2, the lithium salt generated by pre-lithiation is mainly Li2Si2O5、Li2SiO3And the stability of the material in the pulping process is facilitated.
Example 2
1) Under the protection of argon, 100g of SiO with the median particle size of 5 microns and 10g of LiH with the median particle size of 1 micron are weighed in a glove box and are uniformly mixed in a crucible, the mixture is heated to 600 ℃ from room temperature at the heating rate of 3 ℃/min, and the temperature is kept for 3h to obtain pre-lithiated silicon monoxide;
2) and (3) putting the pre-lithiated silicon monoxide obtained in the step (1) into a rotary kiln, heating to 800 ℃, introducing acetylene gas, and keeping the temperature for 1h to obtain the pre-lithiated silicon monoxide/carbon composite material.
3) Placing the pre-lithiated silicon monoxide/carbon composite material obtained in the step 2) and 6g of nano aluminum oxide into a ball milling tank, carrying out ball milling for 1h at the ball milling rotation speed of 200rpm/min, placing the material obtained by ball milling into a tubular furnace, heating to 600 ℃ at the heating rate of 3 ℃/min, and carrying out heat preservation for 3h to obtain the final lithium ion battery-grade silicon monoxide negative electrode material.
Example 3
Step 3) was not performed as compared with example 1), and the rest of the steps were the same as example 1.
Example 4
1) Under the protection of argon, 10g of inert metal lithium powder with the median particle size of 2 microns is weighed in a glove box and is soaked in toluene, then 100g of SiO with the median particle size of 6 microns is slowly added into the glove box, the soaking temperature is 20 ℃, the time is more than 20 hours, the SiO can fully absorb lithium, a dry solid is obtained by centrifugal collection, the temperature is increased to 300 ℃ from the room temperature at the heating rate of 3 ℃/min, and the temperature is kept for 3 hours, so that the pre-lithiated silicon monoxide is obtained.
2) Putting the pre-lithiated silicon monoxide obtained in the step 1) into a rotary kiln, heating to 800 ℃, introducing acetylene gas, and keeping the temperature for 1h to obtain the pre-lithiated silicon monoxide/carbon composite material.
3) Dispersing 5g of magnesium oxide and 10g of zinc oxide into 200g of ethanol solution, adding the pre-lithiated silicon oxide/carbon composite material obtained in the step 2) after uniform dispersion, uniformly stirring, centrifuging three times, taking a bottom material, and drying in a vacuum oven at 80 ℃ for 24 hours to obtain the final lithium ion battery-grade silicon oxide negative electrode material.
TABLE 1 Properties of examples 1-4
As can be seen from table 1, examples 1, 2, and 4 all used oxide coatings and had better cycling stability, while example 3 was not performed and had poorer cycling stability than examples 1, 2, and 4.
Example 5
1) Uniformly mixing 100g of silicon monoxide with the median particle size of 5-8 mu m and a lithium source under the protection of argon, heating to 600 ℃ from room temperature at the heating rate of 3 ℃/min, and preserving heat for 4h to obtain pre-lithiated silicon monoxide; wherein the mass ratio of the silicon monoxide to the lithium source is 1: 0.01. the lithium source is LiH with the median particle size of 1-3 mu m;
2) putting the pre-lithiated silicon monoxide into a rotary kiln, introducing pyrolysis gas at 700 ℃ and keeping the temperature for 10 hours to obtain a pre-lithiated silicon monoxide/carbon composite material; wherein the pyrolysis gas is acetylene.
3) According to the mass ratio of 0.01: 1, uniformly mixing the metal oxide and the pre-lithiated silicon oxide/carbon composite material to ensure that the metal oxide is uniformly coated on the surface of the silicon oxide/carbon composite material to obtain the lithium ion battery-grade silicon oxide negative electrode material. Wherein the metal oxide is alumina.
Example 6
1) Uniformly mixing 100g of silicon monoxide with the median particle size of 5-8 mu m and a lithium source under the protection of argon, heating to 600 ℃ from room temperature at the heating rate of 5 ℃/min, and preserving heat for 10 hours to obtain pre-lithiated silicon monoxide; wherein the mass ratio of the silicon monoxide to the lithium source is 1: 0.1. the lithium source is inert lithium powder with the median particle size of 1-3 mu m;
2) putting the pre-lithiated silicon monoxide into a rotary kiln, introducing pyrolysis gas at 800 ℃ and keeping the temperature for 5 hours to obtain a pre-lithiated silicon monoxide/carbon composite material; wherein the pyrolysis gas is methane.
3) According to the mass ratio of 0.1: 1, uniformly mixing the metal oxide and the pre-lithiated silicon oxide/carbon composite material to ensure that the metal oxide is uniformly coated on the surface of the silicon oxide/carbon composite material to obtain the lithium ion battery-grade silicon oxide negative electrode material. Wherein the metal oxide is titanium oxide.
Example 7
1) Uniformly mixing 100g of silicon monoxide with the median particle size of 5-8 mu m and a lithium source under the protection of argon, heating to 600 ℃ from room temperature at the heating rate of 7 ℃/min, and preserving heat for 5 hours to obtain pre-lithiated silicon monoxide; wherein the mass ratio of the silicon monoxide to the lithium source is 1: 1. the lithium source is lithium borohydride;
2) putting the pre-lithiated silicon monoxide into a rotary kiln, introducing pyrolysis gas at 900 ℃ and keeping the temperature for 1h to obtain a pre-lithiated silicon monoxide/carbon composite material; wherein, the pyrolysis gas is a mixed gas of ethylene and propylene.
3) According to the mass ratio of 0.2: 1, uniformly mixing the metal oxide and the pre-lithiated silicon oxide/carbon composite material to ensure that the metal oxide is uniformly coated on the surface of the silicon oxide/carbon composite material to obtain the lithium ion battery-grade silicon oxide negative electrode material. Wherein the metal oxide is a mixture of magnesium oxide and zirconium oxide.
Example 8
1) Uniformly mixing 100g of silicon monoxide with the median particle size of 5-8 mu m and a lithium source under the protection of argon, heating to 600 ℃ from room temperature at the heating rate of 10 ℃/min, and preserving heat for 1h to obtain pre-lithiated silicon monoxide; wherein the mass ratio of the silicon monoxide to the lithium source is 1: 0.5. the lithium source is lithium aluminum hydride;
2) putting the pre-lithiated silicon monoxide into a rotary kiln, introducing pyrolysis gas at 850 ℃ and keeping the temperature for 3 hours to obtain a pre-lithiated silicon monoxide/carbon composite material; wherein the pyrolysis gas is a mixed gas of acetylene and methane.
3) According to the mass ratio of 0.05: 1, uniformly mixing the metal oxide and the pre-lithiated silicon oxide/carbon composite material to ensure that the metal oxide is uniformly coated on the surface of the silicon oxide/carbon composite material to obtain the lithium ion battery-grade silicon oxide negative electrode material. Wherein the metal oxide is a mixture of aluminum oxide and titanium oxide.
Example 9
1) Uniformly mixing 100g of silicon monoxide with the median particle size of 5-8 mu m and a lithium source under the protection of argon, heating to 400 ℃ from room temperature at the heating rate of 8 ℃/min, and preserving heat for 7 hours to obtain pre-lithiated silicon monoxide; wherein the mass ratio of the silicon monoxide to the lithium source is 1: 0.06. the lithium source is lithium aluminum hydride;
2) putting the pre-lithiated silicon monoxide into a rotary kiln, introducing pyrolysis gas at 750 ℃ and keeping the temperature for 8 hours to obtain a pre-lithiated silicon monoxide/carbon composite material; wherein the pyrolysis gas is a mixed gas of acetylene, methane and ethylene.
3) According to the mass ratio of 0.15: 1, uniformly mixing the metal oxide and the pre-lithiated silicon oxide/carbon composite material to ensure that the metal oxide is uniformly coated on the surface of the silicon oxide/carbon composite material to obtain the lithium ion battery-grade silicon oxide negative electrode material. Wherein the metal oxide is alumina.
The invention improves the slurry stability and electrochemical performance of the pre-lithiated silicon oxide raw material through vapor deposition and metal oxide coating, and simultaneously, the invention has the advantages of simple process method, excellent performance and wide application prospect in lithium ion batteries.
Claims (10)
1. A preparation method of a lithium ion battery-grade silicon monoxide negative electrode material is characterized by comprising the following steps:
s1, uniformly mixing the silicon monoxide with a lithium source under a protective atmosphere, and preserving heat at 300-700 ℃ to obtain pre-lithiated silicon monoxide;
s2, putting the pre-lithiated silicon monoxide into a rotary kiln, and performing carbon coating by adopting vapor deposition to obtain a pre-lithiated silicon monoxide/carbon composite material;
and S3, uniformly mixing the metal oxide with the pre-lithiated silicon oxide/carbon composite material to ensure that the metal oxide is uniformly coated on the surface of the silicon oxide/carbon composite material to obtain the lithium ion battery-grade silicon oxide negative electrode material.
2. The method according to claim 1, wherein in step S1, the mass ratio of the silicon oxide to the lithium source is 1: (0.01-1).
3. The method for preparing a lithium ion battery-grade silicon monoxide negative electrode material according to claim 1, wherein in the step S1, the lithium source is LiH, inert lithium powder, lithium borohydride or lithium aluminum hydride; the protective atmosphere is argon or nitrogen.
4. The method of claim 3, wherein in step S1, the median particle size of the silica is 5-8 μm, and the median particle size of the inert lithium powder or LiH is 1-3 μm.
5. The method as claimed in claim 1, wherein in step S1, the temperature is raised from room temperature to 700 ℃ at a temperature raising rate of 3-10 ℃/min, and the holding time is 1-10 h.
6. The method for preparing a lithium ion battery-grade silicon monoxide negative electrode material according to claim 1, wherein in the step S2, the carbon coating by vapor deposition comprises the following specific steps: introducing pyrolysis gas at the temperature of 700 ℃ and 900 ℃ and preserving heat for 1-10 h.
7. The method for preparing the lithium ion battery-grade silicon monoxide negative electrode material as claimed in claim 6, wherein the pyrolysis gas is one or a mixture of acetylene, methane, ethylene and propylene.
8. The method for preparing a lithium ion battery grade silicon monoxide negative electrode material according to claim 1, wherein in step S3, the metal oxide is one or two of aluminum oxide, titanium oxide, magnesium oxide and zirconium oxide; the mass ratio of the metal oxide to the pre-lithiated silicon oxide/carbon composite material is (0.01-0.2): 1.
9. the lithium ion battery grade silicon oxide negative electrode material prepared according to any one of the methods of claims 1 to 8.
10. Use of a lithium-ion battery grade silicon monoxide negative electrode material as claimed in claim 9 for the preparation of a lithium-ion battery.
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| CN112670474A (en) * | 2020-12-23 | 2021-04-16 | 清华大学 | Pre-lithiation material and preparation thereof, precursor material, lithium battery negative electrode slurry and lithium battery |
| CN113036108A (en) * | 2021-03-11 | 2021-06-25 | 昆山宝创新能源科技有限公司 | Negative electrode material and preparation method and application thereof |
| CN113023738A (en) * | 2021-03-03 | 2021-06-25 | 昆山宝创新能源科技有限公司 | Silicon-based composite material, preparation method thereof and battery |
| CN113437280A (en) * | 2021-08-30 | 2021-09-24 | 北京壹金新能源科技有限公司 | Slurry-stabilized lithiated silicon-based composite material and preparation method and application thereof |
| CN114005974A (en) * | 2021-12-30 | 2022-02-01 | 常州硅源新能材料有限公司 | Silica anode material, preparation method of silica anode material and lithium ion battery |
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| CN114094090A (en) * | 2021-11-10 | 2022-02-25 | 中汽创智科技有限公司 | Silicon-based negative electrode material and preparation method and application thereof |
| CN114804118A (en) * | 2021-01-29 | 2022-07-29 | 中国科学技术大学 | Modified silicon monoxide material, preparation method thereof and lithium ion battery |
| CN114975967A (en) * | 2022-06-29 | 2022-08-30 | 宁波杉杉新材料科技有限公司 | Pre-lithiated silica composite material, preparation method thereof, negative pole piece, battery and application |
| CN115986094A (en) * | 2023-03-01 | 2023-04-18 | 江苏正力新能电池技术有限公司 | Pre-lithiated silicon oxide negative electrode material with core-shell structure and preparation method and application thereof |
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