CN110148729B - Preparation method and application of carbon-coated silicon monoxide material - Google Patents
Preparation method and application of carbon-coated silicon monoxide material Download PDFInfo
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- CN110148729B CN110148729B CN201910452164.0A CN201910452164A CN110148729B CN 110148729 B CN110148729 B CN 110148729B CN 201910452164 A CN201910452164 A CN 201910452164A CN 110148729 B CN110148729 B CN 110148729B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 86
- 239000000463 material Substances 0.000 title claims abstract description 74
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 88
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 5
- 239000010406 cathode material Substances 0.000 claims abstract description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 27
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 12
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 2
- -1 ethylene, propylene, acetylene Chemical group 0.000 claims description 2
- MWWATHDPGQKSAR-UHFFFAOYSA-N propyne Chemical compound CC#C MWWATHDPGQKSAR-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000005086 pumping Methods 0.000 claims 1
- 238000000576 coating method Methods 0.000 abstract description 26
- 239000007790 solid phase Substances 0.000 abstract description 13
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 11
- 229910052710 silicon Inorganic materials 0.000 abstract description 11
- 239000010703 silicon Substances 0.000 abstract description 11
- 239000011248 coating agent Substances 0.000 abstract description 8
- 239000012071 phase Substances 0.000 abstract description 6
- 239000011247 coating layer Substances 0.000 abstract description 2
- 239000003792 electrolyte Substances 0.000 abstract description 2
- 239000007773 negative electrode material Substances 0.000 description 7
- 238000007599 discharging Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 238000000197 pyrolysis Methods 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 2
- 230000001351 cycling effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000002210 silicon-based material Substances 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- 229910005321 Li15Si4 Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention relates to a preparation method and application of a carbon-coated silicon monoxide material, wherein the method comprises the following steps: putting the silicon monoxide into a closed reaction furnace with an electrode, vacuumizing the furnace chamber, and injecting organic gas to keep the furnace chamber in a low vacuum state; high-voltage current is conducted between the two electrodes to decompose the organic gas to generate carbon which is then deposited on the surface of the silicon oxide to obtain a carbon-coated silicon oxide material; the method is different from the traditional solid-phase coating and high-temperature gas-phase coating methods, the organic gas is decomposed by high-voltage current to generate carbon to carry out carbon coating on the silicon protoxide material, the obtained carbon coating layer is thin and uniform, the volume expansion of the silicon protoxide material in the charge and discharge process is inhibited, the direct contact between the silicon protoxide material and electrolyte is avoided, the first coulombic efficiency and the cycle stability of the silicon protoxide material are improved, and the method is an excellent choice of the lithium ion battery cathode material.
Description
Technical Field
The invention relates to the technical field of a silicon oxide material, in particular to a preparation method and application of a carbon-coated silicon oxide material.
Background
The endurance mileage of the power electric vehicle is related to the change of the requirements of people and the development of the future automobile industry, and in order to realize the energy density of 300wh/kg of the power battery, a ternary material is inevitably selected to replace the commercial lithium iron phosphate and lithium cobaltate as the anode material of the lithium ion battery; and the silicon-carbon material is used for replacing a graphite cathode, so that the energy density of the battery is improved by times, and the inevitable trend of the development of the new energy automobile industry is also provided.
Because silicon has a low plateau potential, the theoretical capacity is ultra-high (3800 mAh/g, Li)15Si4；4200mAh/g，Li15Si4Nearly 10 times the capacity of the marketized graphite), high surface area, high tap density, simple preparation and the like, thereby having great application prospect.
However, when the silicon material is used as a negative electrode material, the volume of the silicon material is greatly changed in the charge and discharge processes, so that the performance of the battery is sharply attenuated; while the silica materials have a higher theoretical capacity and a lower volume expansion that is of increasing interest.
In order to improve the first coulombic efficiency and the cycle performance of the silicon protoxide material, the silicon protoxide material needs to be subjected to surface coating, the simplest and most effective method is carbon coating, and the most common carbon coating methods in the prior art are solid-phase coating and high-temperature gas-phase coating.
Disclosure of Invention
The invention aims to provide a novel preparation method and application of a carbon-coated silicon oxide material, and compared with a mainstream product prepared by a traditional method, the carbon-coated silicon oxide material prepared by the method has basically the same or better performance.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a carbon-coated silicon monoxide material comprises the following steps:
s1, putting the silicon monoxide into a sealed reaction furnace with electrodes, vacuumizing the furnace chamber, and injecting organic gas to keep the furnace chamber in a low vacuum state;
and S2, introducing high-voltage current between the two electrodes to decompose the organic gas to generate carbon, and depositing the carbon on the surface of the silicon oxide to obtain the carbon-coated silicon oxide material.
Preferably, in S1, the vacuum degree in the furnace chamber is pumped to 1-0.1Pa, and then organic gas is introduced to maintain the pressure in the furnace chamber at 60-1400 Pa.
Preferably, the organic gas is one or more of methane, ethane, ethylene, propylene, acetylene or propyne.
Preferably, the voltage applied between the two electrodes in S2 is 400-.
Preferably, the high-voltage current between the two electrodes in S2 is direct current or alternating current.
Preferably, the frequency of the alternating current is 10 to 100Hz.
Preferably, the current density of the high-voltage current is 0.5-2.0 mA/cm.
The carbon-coated silica material prepared by the preparation method of the carbon-coated silica material can be applied to a lithium ion battery cathode material.
The invention has the following beneficial effects: the method is different from the traditional solid-phase coating and high-temperature gas-phase coating methods, the organic gas is decomposed by high-voltage current to generate carbon to carry out carbon coating on the silicon protoxide material, the obtained carbon coating layer is thin and uniform, the volume expansion of the silicon protoxide material in the charge and discharge process is inhibited, the direct contact between the silicon protoxide material and electrolyte is avoided, the first coulombic efficiency and the cycle stability of the silicon protoxide material are improved, and the method is an excellent choice of the lithium ion battery cathode material.
Drawings
FIG. 1 is an SEM image of a carbon-coated silica material prepared in example 1;
FIG. 2 is a first charging/discharging diagram of the charging/discharging of the carbon-coated silica material prepared by the solid-phase carbon coating method in example 1;
FIG. 3 is a chargecycle chart of the carbon-coated silica material obtained by the solid-phase carbon coating method in example 1;
FIG. 4 is an SEM image of a carbon-coated silica material prepared in example 2;
FIG. 5 is a first charging/discharging diagram of the charging/discharging of the carbon-coated SiOx material obtained in example 2 and the carbon-coated SiOx material obtained by the solid-phase carbon-coating method, respectively;
FIG. 6 is a chargecycle chart of the carbon-coated silica material obtained by the solid-phase carbon coating method in example 2;
FIG. 7 is an SEM image of a carbon-coated silica material prepared in example 3;
FIG. 8 is a first charging/discharging diagram of the carbon-coated SiOx material obtained in example 3 and the carbon-coated SiOx material obtained by the high-temperature vapor-phase carbon coating method;
FIG. 9 is a chargeback cycle chart of the carbon-coated SiOx material obtained in example 3 and the carbon-coated SiOx material obtained by the high-temperature vapor-phase carbon coating method, respectively.
Detailed Description
The invention is further illustrated by the following specific examples:
example 1:
a preparation method of a carbon-coated silicon monoxide material comprises the following steps:
the silicon monoxide is put into a closed reaction furnace with electrodes, the furnace chamber is vacuumized to 0.1Pa, and methane is injected to keep the pressure in the furnace chamber at 700 Pa.
Then, direct current with the voltage of 600V and the current density of 1mA/cm is applied between the two electrodes, and the high-voltage current enables methane to be decomposed to generate carbon which is then deposited on the surface of the silicon oxide, so that the carbon-coated silicon oxide material is obtained.
An SEM for examining the morphology of the carbon-coated silica material obtained in example 1 is shown in fig. 1.
As can be seen from fig. 1, in the carbon-coated silica material prepared in example 1, carbon is uniformly coated on the surface of the silica.
The button cell was prepared using the carbon-coated silica material prepared in example 1 as the negative electrode material, and the button cell was prepared using the carbon-coated silica material prepared by the solid-phase carbon-coating method as the negative electrode material, both of which were subjected to the first charge-discharge test and the cycle performance test, and the structures of which are shown in fig. 2 and 3.
As shown in fig. 2, compared with the conventional solid-phase carbon coating method, the button cell made of the carbon-coated silicon oxide material prepared in example 1 has a significantly improved first coulombic efficiency of the silicon oxide material.
As shown in fig. 3, compared with the conventional solid-phase carbon coating method, the cycling performance of the silicon oxide material is significantly improved in the button cell made of the carbon-coated silicon oxide material prepared in example 1.
Example 2
A preparation method of a carbon-coated silicon monoxide material comprises the following steps:
the silicon monoxide is put into a closed reaction furnace with electrodes, the furnace chamber is vacuumized to 0.2Pa, acetylene is injected, and the pressure in the furnace chamber is kept at 500 Pa.
Then, an alternating current with the voltage of 550V, the frequency of 50Hz and the current density of 0.5mA/cm is applied between the two electrodes, and the high-voltage current enables acetylene to be decomposed to generate carbon which is then deposited on the surface of the silicon oxide, so that the carbon-coated silicon oxide material is obtained.
An SEM which examined the morphology of the carbon-coated silica material obtained from example 2 is shown in fig. 4.
As can be seen from fig. 4, in the carbon-coated silica material prepared in example 2, carbon is uniformly coated on the surface of the silica.
The button cell was prepared using the carbon-coated silica material prepared in example 2 as the negative electrode material, and the button cell was prepared using the carbon-coated silica material prepared by the solid-phase carbon-coating method as the negative electrode material, both of which were subjected to the first charge-discharge test and the cycle performance test, and the structures of which are shown in fig. 5 and 6.
As shown in fig. 5, compared with the conventional solid-phase carbon coating method, the button cell made of the carbon-coated silicon oxide material prepared in example 2 has a significantly improved first coulombic efficiency of the silicon oxide material.
As shown in fig. 6, compared with the conventional solid-phase carbon coating method, the button cell made of the carbon-coated silicon oxide material obtained in example 2 has significantly improved cycle performance of the silicon oxide material.
Example 3
A preparation method of a carbon-coated silicon monoxide material comprises the following steps:
the silicon monoxide is put into a closed reaction furnace with electrodes, the furnace chamber is vacuumized to 1Pa, and methane is injected to keep the pressure in the furnace chamber at 1000 Pa.
And then applying direct current with the voltage of 700V and the current density of 0.5mA/cm between the two electrodes, wherein the high-voltage current enables methane to be decomposed to generate carbon, and the carbon is deposited on the surface of the silicon oxide to obtain the carbon-coated silicon oxide material.
An SEM which examined the morphology of the carbon-coated silica material obtained in example 3 is shown in fig. 7.
As can be seen from fig. 7, in the carbon-coated silica material prepared in example 3, carbon is uniformly coated on the surface of the silica.
The button cell was prepared using the carbon-coated silicon monoxide material prepared in example 3 as the negative electrode material, and the button cell was prepared using the carbon-coated silicon monoxide material prepared by pyrolysis gas-phase carbon coating method as the negative electrode material, both of which were subjected to the first charge-discharge test and the cycle performance test, and the structures of which are shown in fig. 8 and 9.
As can be seen from fig. 8, compared with the conventional pyrolysis gas-phase carbon coating method, the button cell made of the carbon-coated silicon oxide material prepared in example 3 significantly improves the first coulombic efficiency of the silicon oxide material.
As shown in fig. 9, compared with the conventional pyrolysis gas phase carbon coating method, the cycling performance of the silicon oxide material is significantly improved in the button cell made of the carbon-coated silicon oxide material prepared in example 3.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solution of the present invention by those skilled in the art should fall within the protection scope defined by the claims of the present invention without departing from the spirit of the present invention.
Claims (6)
1. A preparation method of a carbon-coated silicon monoxide material is characterized by comprising the following steps: the method comprises the following steps:
s1, putting the silicon monoxide into a sealed reaction furnace with electrodes, pumping the vacuum degree in the furnace chamber to 0.1-1Pa, and introducing organic gas to keep the pressure in the furnace chamber at 60-1400 Pa;
s2, high-voltage current is conducted between the two electrodes to decompose the organic gas to generate carbon which is then deposited on the surface of the silicon oxide to obtain a carbon-coated silicon oxide material; the voltage applied between the two electrodes is 400-750V.
2. The method of claim 1, wherein the step of forming the carbon-coated silica material comprises: the organic gas is one or more of methane, ethane, ethylene, propylene, acetylene or propyne.
3. The method of claim 1, wherein the step of forming the carbon-coated silica material comprises: the high-voltage current between the two electrodes in the step S2 is direct current or alternating current.
4. The method according to claim 3, wherein the step of preparing the carbon-coated silica material comprises: the frequency of the alternating current is 10-100Hz.
5. The method of claim 1, wherein the step of forming the carbon-coated silica material comprises: the current density of the high-voltage current is 0.5-2.0mA/cm2。
6. The method for producing a carbon-coated silica material according to any one of claims 1 to 5, wherein: the prepared carbon-coated silicon monoxide material is used for a lithium ion battery cathode material.
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| CN111463423B (en) * | 2020-04-07 | 2021-09-28 | 山东斯艾诺德新材料科技有限公司 | Preparation method of negative electrode material of silicon oxide lithium ion battery and preparation method of negative electrode piece of battery |
| CN111342032B (en) * | 2020-04-14 | 2021-03-23 | 陕西煤业化工技术研究院有限责任公司 | Preparation method and application of oriented graphene coated silica material |
| CN111769264B (en) * | 2020-06-18 | 2022-06-07 | 合肥国轩高科动力能源有限公司 | Silicon-carbon composite material and preparation method and application thereof |
| CN112186145B (en) * | 2020-09-08 | 2022-06-07 | 合肥国轩高科动力能源有限公司 | Magnesium reduced carbon coated silica material and preparation method and application thereof |
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