CN111129477A - Method for preparing super-assembled lithium storage material with silicon nano dots embedded in carbon skeleton - Google Patents
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- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- 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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- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to a method for preparing a super-assembled lithium storage material with silicon nano dots embedded into a carbon skeleton, which comprises the steps of sealing silane and triphenyltin hydride in a quartz tube at room temperature, placing the quartz tube in a muffle furnace, heating to 200 ℃ at the rate of 5 ℃ per minute and keeping for 2 hours, then heating to 800 ℃ at the rate of 10 ℃ per minute and cycling at 800 DEG CKeeping the mixture under the environment for 5 hours, finally injecting ethanol into a quartz tube for ultrasonic oscillation, and centrifuging to obtain a black powder final product. Compared with the prior art, the silicon nanodots synthesized by the methodThe carbon skeleton material has high reversible lithium storage capacity, excellent cycle performance and excellent cycle performance.
Description
Technical Field
The invention relates to a preparation method of an inorganic material with a controllable structure, in particular to a method for preparing a super-assembled lithium storage material with a carbon skeleton embedded with silicon nano-dots, wherein the super-assembled lithium storage material has excellent lithium electrical property and is prepared by a space-limited cluster catalysis strategy in one step.
Background
For applications in portable electronic devices and electric/hybrid vehicles, there is a strong need to develop rechargeable Lithium Ion Batteries (LIBs) with higher energy capacity and longer cycle life. However, the existing LIBs using graphite anodes with low specific capacities cannot meet strict requirements. Due to its high theoretical lithium storage capacity (Li)22Si5Is 4200mAh g-1) Si is considered one of the most promising anode materials, about ten times the commercial graphite capacity, and its modest lithium absorption potential (0.4V vs Li/Li)+) And natural abundance. However, severe volume changes (-400%) of Si electrodes during charge/discharge often cause electrode pulverization and active material loss, resulting in deterioration of the overall performance of the battery. In addition, Si also has low conductivity and poor electron transport as a semiconductor material. To solve the problem, carbon materials having good electrical conductivity and excellent mechanical properties have been strongly introduced into Si-based anodes to accommodate volume changes and simultaneously improve the electrical conductivity of the electrodes. Previously reported Si/C composites prepared by physical mixing of two components often cause weak interfacial interactions and non-uniform dispersion of the two components, which is detrimental to electron transfer at the interface and cycling stability of the composite anode.
Notably, Chemical Vapor Deposition (CVD) strategies based on metal catalysts, in which catalyst nanoparticles are dispersed on an essential substrate as catalytic sites for in situ growth of Si nanowires with a vapor-liquid-solid (VLS) mechanism, offer a good possibility of uniformity. Anchoring the Si into a carbon matrix in the Si/C composite. However, the introduction of the metal catalyst into the carbon substrate is mainly an additional operation by physical sputtering or chemical deposition, and is subject to a complicated process and a poor distribution of the metal catalyst. Furthermore, catalytic growth of Si is mainly performed in an unrestricted space, uninterrupted Si source feed, leading to overgrowth of Si and formation of long nanometer (hundreds of nanometers to micrometers) Si nanowires. Furthermore, in most cases the catalyst used is in the form of nanoparticles with a relatively large diameter, which, according to a catalytic growth mechanism, lead to the production of large diameter Si nanowires (over 50 nm). In principle, Si nanowires with long length and large diameter do not favour electron transfer from Si to the current collector through the Si-carbon interface and volume change suppression of Si. Therefore, there is a great need to develop simple and efficient metal catalytic strategies for manufacturing Si/C composites with advantageous structures for high performance LIBs.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, provides a method for preparing a super-assembled lithium storage material with a carbon skeleton and silicon nano-dots embedded in the super-assembled lithium storage material in one step by a space-limited cluster catalysis strategy, and solves the technical problems that the size of Si particles cannot be controlled and the stability of a Si cathode material is poor in a circulation process in the prior art.
The purpose of the invention can be realized by the following technical scheme:
a method for preparing a super-assembled silicon nano-dot-embedded carbon skeleton lithium storage material, comprising the following steps of:
mixing silane and triphenyl tin hydride and sealing the mixture in a reactor;
placing the reactor in a muffle furnace, and controlling the heating rate to carry out high-temperature reaction;
and injecting ethanol into the reactor, performing ultrasonic oscillation, and centrifuging to obtain the silicon nanodot-embedded carbon skeleton lithium storage material.
The silane is monophenyl silane, diphenyl silane, triphenyl silane or tetraphenyl silane.
Further, the silane adopts diphenyl silane. The reason is that the carbon material can be uniformly distributed beside the Si particles to limit the Si particles to a smaller size while having a higher Si content.
The silane and the triphenyltin hydride are mixed according to the molar ratio of Si to Sn of 10: 1-20: 1.
Further, the silane and triphenyltin hydride are mixed in a molar ratio of Si to Sn of 15: 1.
The reactor is a quartz tube, and is dried in a vacuum environment after being repeatedly cleaned by acetone and ethanol.
The reactor is heated to 200-300 ℃ in a muffle furnace at the rate of 5-10 ℃ per minute and then kept for 2-3 h, and then heated to 800-900 ℃ at the rate of 10-20 ℃ per minute and then kept for 5-10 h.
Further, the reactor was heated to 200 ℃ at a rate of 5 ℃ per minute in a muffle furnace and then held for 2 hours, and then heated to 800 ℃ at a rate of 10 ℃ per minute and then held for 5 hours.
And (5) ultrasonic oscillation of 20-40 kW.
Compared with the prior art, the invention provides a novel Sn atomic cluster catalysis strategy for the super-assembly of the Si nanodots embedded into the carbon framework of the high-performance lithium ion battery. This is achieved by the design of co-decomposition of triphenyltin hydride and diphenylsilane, in the process of which Sn clusters are first produced by thermolysis of triphenyltin hydride and serve as catalysts for thermolysis and Si-catalyzed growth of diphenylsilane. Thereby obtain the super assembled structure of Si nanodot embedding carbon frame, have following advantage:
(1) the super-assembly material is synthesized simply and efficiently in one step,
(2) silicon particles of 5-10 nm, small size and uniform encapsulation in a carbon skeleton,
(3) the method has the advantages that the method shows good cycle stability performance in charge and discharge tests, the carbon skeleton can buffer the volume expansion/contraction of the silicon nano-wire during the insertion/extraction of lithium ions, all the characteristics are beneficial to improving the capacity of the battery, accelerating the reaction rate and enhancing the cycle stability, and the super-assembled silicon nano-dots are prepared in one step based on the strategy of space-limited domain cluster catalysisThe battery of the carbon skeleton lithium storage material shows high lithium storage capacity (at 0.1A g) in the silicon-carbon negative electrode material with low silicon content-1At a current density of 837mA hg-1) And high rate capability (at 1A g)-1At a current density of 647mA hg-1At 2A g-1At a current density of 527mA hg-1)。
Drawings
FIG. 1 shows scanning electron microscopes (a-b, e), transmission electron microscopes (c, d), scanning electron micrographs (e) and X-ray diffraction patterns (f) of the materials obtained in example 1.
Fig. 2 is a graph showing the results of the battery performance test of the material obtained in example 1.
Fig. 3 is a graph showing the results of the full cell performance test of the material obtained in example 1.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Super-assembled silicon nano-dots prepared in one step by space-limited cluster catalysis strategy and having excellent lithium electrical propertyA method of making a carbon-backbone lithium storage material, the method comprising the steps of:
(1) cleaning a quartz tube with acetone with the purity of 99% and ethanol with the purity of 99.9%, repeating for many times, and then drying in a vacuum environment;
(2) mixing monophenyl silane, diphenyl silane, triphenyl silane or tetraphenyl silane and triphenyl tin hydride in an atomic ratio (Si: Sn ═ 10-20:1) at room temperature, and sealing in a quartz tube;
(3) placing the quartz tube in a muffle furnace, heating to 200-300 ℃ at the rate of 5-10 ℃ per minute, keeping for 2-3 h, heating to 800-900 ℃ at the rate of 10-20 ℃ per minute, and keeping for 5-10 h;
(4) and finally, injecting ethanol with the purity of 99.9% into the quartz tube for ultrasonic oscillation, wherein the power of the ultrasonic oscillation is 20-40 kW, and centrifuging to obtain a black powder final product.
The following are more detailed embodiments, and the technical solutions and the technical effects obtained by the present invention will be further described by the following embodiments.
Example 1
The quartz tube was washed with acetone, ethanol, and repeated several times, followed by drying in a vacuum environment. Diphenylsilane and triphenyltin hydride were mixed in an atomic ratio (Si: Sn 15:1) at room temperature, and sealed in a quartz tube; the quartz tube was placed in a muffle furnace and heated to 200 ℃ at a rate of 5 ℃ per minute and held for 2 hours. Then raising the temperature to 800 ℃ at the rate of 10 ℃ per minute and keeping the temperature for 5 hours in an environment of 800 ℃; and finally, injecting ethanol into the quartz tube for ultrasonic oscillation with the power of 30kW, and centrifuging to obtain a black powder final product.
FIG. 1 shows scanning electron microscopes (a-b, e), transmission electron microscopes (c, d), scanning electron microscope (e) and X-ray diffraction patterns (f) of the prepared materials. (a) Indicating the general morphology of the particles; (b) the morphology of the particle sheet is shown; (c) the distribution of Si inside the particles in the framework material in low resolution is shown; (d) the distribution condition of Si in the carbon skeleton in high resolution is shown; (e) the distribution state of elements in the particles is shown;
fig. 2 is a battery performance test of the prepared material, (a) illustrates a CV curve test of the material; (b) testing a charge-discharge curve of the material; (c) the material is 1Ag-1And 2Ag-1Long cycle performance (at 1A g)-1At a current density of 647mA hg-1At 2A g-1At a current density of 527mAhg-1(ii) a (d) The multiplying power cycling performance of the material.
Fig. 3 is a full battery performance test of the prepared material, (a) is a schematic diagram of charge and discharge curves of a full battery formed by the material and LFP, LCO and NCA respectively; (b) the charge-discharge cycle curve of the full cell is shown.
Example 2
The quartz tube was washed with acetone, ethanol, and repeated several times, followed by drying in a vacuum environment. Mixing monophenyl silane and triphenyl tin hydride at room temperature in an atomic ratio (Si: Sn 15:1) and sealing in a quartz tube; the quartz tube was placed in a muffle furnace and heated to 200 ℃ at a rate of 5 ℃ per minute and held for 2 hours. Then raising the temperature to 800 ℃ at the rate of 10 ℃ per minute and keeping the temperature for 5 hours in an environment of 800 ℃; and finally, injecting ethanol into the quartz tube for ultrasonic oscillation with the power of 30kW, and centrifuging to obtain a black powder final product.
Example 3
The quartz tube was washed with acetone, ethanol, and repeated several times, followed by drying in a vacuum environment. Diphenylsilane and triphenyltin hydride were mixed in an atomic ratio (Si: Sn 15:1) at room temperature, and sealed in a quartz tube; the quartz tube was placed in a muffle furnace and heated to 300 ℃ at a rate of 5 ℃ per minute and held for 2 hours. Then raising the temperature to 800 ℃ at the rate of 10 ℃ per minute and keeping the temperature for 5 hours in an environment of 800 ℃; and finally, injecting ethanol into the quartz tube for ultrasonic oscillation with the power of 20kW, and centrifuging to obtain a black powder final product.
Example 4
The quartz tube was washed with acetone, ethanol, and repeated several times, followed by drying in a vacuum environment. Diphenylsilane and triphenyltin hydride were mixed in an atomic ratio (Si: Sn 15:1) at room temperature, and sealed in a quartz tube; the quartz tube was placed in a muffle furnace and heated to 200 ℃ at a rate of 5 ℃ per minute and held for 2 hours. Then raising the temperature to 900 ℃ at the rate of 10 ℃ per minute and keeping the temperature for 5 hours in an environment of 900 ℃; and finally, injecting ethanol into the quartz tube for ultrasonic oscillation with the power of 40kW, and centrifuging to obtain a black powder final product.
Example 5
The quartz tube was washed with acetone, ethanol, and repeated several times, followed by drying in a vacuum environment. Diphenylsilane and triphenyltin hydride were mixed in an atomic ratio (Si: Sn ═ 10:1) at room temperature, and sealed in a quartz tube; the quartz tube was placed in a muffle furnace and heated to 300 ℃ at a rate of 10 ℃ per minute and held for 2 hours. Then raising the temperature to 800 ℃ at the rate of 15 ℃ per minute, and keeping the temperature for 10 hours in an environment of 800 ℃; and finally, injecting ethanol into the quartz tube for ultrasonic oscillation with the power of 20kW, and centrifuging to obtain a black powder final product.
Example 6
The quartz tube was washed with acetone, ethanol, and repeated several times, followed by drying in a vacuum environment. Diphenylsilane and triphenyltin hydride were mixed in an atomic ratio (Si: Sn ═ 20:1) at room temperature, and sealed in a quartz tube; the quartz tube was placed in a muffle furnace and heated to 300 ℃ at a rate of 8 ℃ per minute and held for 2.5 hours. Then raising the temperature to 900 ℃ at the rate of 20 ℃ per minute and keeping the temperature in an environment of 900 ℃ for 8 hours; and finally, injecting ethanol into the quartz tube for ultrasonic oscillation with the power of 30kW, and centrifuging to obtain a black powder final product.
Example 7
The quartz tube was washed with acetone, ethanol, and repeated several times, followed by drying in a vacuum environment. Diphenylsilane and triphenyltin hydride were mixed in an atomic ratio (Si: Sn 15:1) at room temperature, and sealed in a quartz tube; the quartz tube was placed in a muffle furnace and heated to 300 ℃ at a rate of 10 ℃ per minute and held for 3 hours. Then raising the temperature to 800 ℃ at the rate of 20 ℃ per minute, and keeping the temperature for 10 hours in an environment of 800 ℃; and finally, injecting ethanol into the quartz tube for ultrasonic oscillation with the power of 20kW, and centrifuging to obtain a black powder final product.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The embodiments described above are intended to facilitate the understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (8)
1. A method for preparing a super-assembled lithium storage material with silicon nano dots embedded in a carbon skeleton, which is characterized by comprising the following steps:
mixing silane and triphenyl tin hydride and sealing the mixture in a reactor;
placing the reactor in a muffle furnace, and controlling the heating rate to carry out high-temperature reaction;
and injecting ethanol into the reactor, performing ultrasonic oscillation, and centrifuging to obtain the silicon nanodot-embedded carbon skeleton lithium storage material.
2. The method of claim 1, wherein the silane is a monophenyl silane, a diphenyl silane, a triphenyl silane, or a tetraphenyl silane.
3. The method for preparing a super-assembled lithium storage material with silicon nano dots embedded in a carbon skeleton according to claim 1, wherein the silane is preferably diphenylsilane.
4. The method for preparing the super-assembled lithium storage material with the silicon nano dots embedded in the carbon skeleton according to any one of claims 1 to 3, wherein the molar ratio of the silane to the triphenyltin hydride is 10: 1-20: 1, were mixed.
5. The method for preparing the super-assembled lithium storage material with silicon nanodots embedded in a carbon skeleton according to claim 1, wherein the reactor is a quartz tube, and the quartz tube is repeatedly cleaned by acetone and ethanol and then dried in a vacuum environment.
6. The method for preparing a super-assembled lithium storage material with a carbon skeleton and silicon nanodots embedded therein according to claim 1, wherein the reactor is heated to 200-300 ℃ at a rate of 5-10 ℃ per minute in a muffle furnace and then kept for 2-5 h, and then heated to 800-900 ℃ at a rate of 10-20 ℃ per minute and then kept for 5-10 h.
7. The method of claim 1 or 6, wherein the reactor is heated to 200 ℃ at a rate of 5 ℃ per minute in a muffle furnace and then held for 2 hours, and then heated to 800 ℃ at a rate of 10 ℃ per minute and then held for 5 hours.
8. The method of claim 1, wherein the ultrasonic vibration is 20-40 kW.
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CN111180687A (en) * | 2019-12-30 | 2020-05-19 | 同济大学 | Method for preparing super-assembled lithium storage material with silicon nano dots embedded in carbon skeleton |
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