CN111186841A - Preparation method of hollow silicon dioxide coated polyhedral carbon composite material - Google Patents
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Abstract
A preparation method of a hollow silicon dioxide coated polyhedral carbon composite material is characterized in that an in-situ synthesis method is utilized to prepare ZIF-8@ SiO on ZIF-82The precursor is carbonized at high temperature to form PC @ SiO2The present invention is different from a single hollow structure and a single carbon clad structure. The hollow silicon dioxide designed by the invention is coated with muchA surface-body carbon composite material as a high-performance LIBs negative electrode. Due to its novel structure, it consists of a carbon inner layer, SiO2And an outer layer. Thus, Li+Directly with SiO2And the reaction promotes the dynamic performance. On the other hand, the carbon inner layer improves charge transport and conductivity. In addition, the cavity in the middle of the new structure provides a buffer space for volume expansion, thereby enhancing the performance of electrochemistry and LIBs.
Description
Technical Field
The invention belongs to the technical field of lithium ion battery cathode materials, and particularly relates to a preparation method of a hollow silicon dioxide coated polyhedral carbon composite material.
Background
Lithium Ion Battery (LIBs)The method is widely applied to portable electronic products. With the development of electric vehicles, higher requirements are put on high energy density batteries. The specific capacity of the commercial graphite material is only 372 mAh g-1This means that the development of high energy density LIBs is limited.
In recent years, since the discovery of SiO by researchers2For Li+Has the theoretical specific capacity of 1965mAh g since the electrochemical activity-1And is considered to be the most promising next-generation anode material. However, SiO has some defects2Cannot be practically used as a negative electrode of a lithium ion battery. For example, the volume change is large during charge and discharge, the intrinsic conductivity is poor, and the electrochemical performance is poor. To improve SiO2As the electrochemical performance of the negative electrode. In recent years, researchers have developed a variety of SiO2Materials such as nanoparticles, films, nanocrystals, etc., all have good properties. It is noted that in order to improve SiO2There are two main strategies for electrochemical performance of (2). An effective method is to design SiO that buffers volume changes2And (3) a hollow structure. Another method is to design the SiO on the surface of a carbon coating2The conductivity is improved. But they cannot satisfy more charge-discharge cycle times at high current densities. On the one hand, although the hollow structure strategy solves the problem of volume change, it still has the problem of low conductivity. Carbon coating strategies, on the other hand, address conductivity issues and partial volume changes. However, during the reaction, Li+The carbon layer must be penetrated, which greatly hinders its dynamic properties.
Disclosure of Invention
In view of the above, it is necessary to provide a method for preparing a hollow silica-coated polyhedral carbon composite material.
A method for preparing a hollow silica-coated polyhedral carbon composite material comprises ZIF-8@ SiO2Preparation procedure and PC @ SiO2A preparation step of the ZIF-8@ SiO2The preparation method specifically comprises the following steps:
adding 40mg of ZIF-8 powder into 204mL of absolute ethyl alcohol, and ultrasonically stirring for 5min to form a first solution;
adding 3.3mL of sodium hydroxide solution into the first solution, wherein the mass concentration of the sodium hydroxide solution is 0.1mol/L to form a second solution;
adding 2.4mL of an absolute ethyl alcohol solution containing 20% tetraethyl orthosilicate into the second solution for three times at intervals of 30min every time, adding 0.8mL of an absolute ethyl alcohol solution containing 20% tetraethyl orthosilicate every time, and stirring at room temperature for 18-26 h to form a third solution;
centrifuging the formed third solution to obtain a first precipitate, centrifuging and washing the first precipitate with absolute ethyl alcohol for three times, and drying at 60 ℃ for 12h to obtain ZIF-8@ SiO2Powder;
the PC @ SiO2The preparation method specifically comprises the following steps:
ZIF-8@ SiO2Placing the powder into a porcelain boat, placing the porcelain boat into a vacuum furnace, and evacuating the vacuum furnace to a vacuum degree of 1.0 × 10- 2pa；
Nitrogen gas was injected into the vacuum furnace at a flow rate of 50sccm to maintain the vacuum degree of the vacuum furnace at 1.0X 10-2pa, heating the vacuum furnace from room temperature to 800 ℃ at the heating rate of 5 ℃/min, and keeping the temperature for 1.5 h;
naturally cooling the mixture to room temperature in a vacuum furnace to obtain PC @ SiO2。
Preferably, in ZIF-8@ SiO2In the preparation step, 2.4mL of an absolute ethyl alcohol solution containing 20% tetraethyl orthosilicate was added to the second solution three times, each time at intervals of 30min, 0.8mL of an absolute ethyl alcohol solution containing 20% tetraethyl orthosilicate was added each time, and then the mixture was stirred at room temperature for 18h to form a third solution.
Preferably, in ZIF-8@ SiO2In the preparation step, 2.4mL of an absolute ethyl alcohol solution containing 20% tetraethyl orthosilicate was added to the second solution three times, each time at intervals of 30min, 0.8mL of an absolute ethyl alcohol solution containing 20% tetraethyl orthosilicate was added each time, and then the mixture was stirred at room temperature for 26 hours to form a third solution.
The present invention is distinguished from a single hollow structure and a single carbon clad structure. The inventionThe designed hollow silicon dioxide coated polyhedral carbon composite material is used as a high-performance LIBs cathode. Due to its novel structure, it consists of a carbon inner layer, SiO2And an outer layer. Thus, Li+Directly with SiO2And the reaction promotes the dynamic performance. On the other hand, the carbon inner layer improves charge transport and conductivity. In addition, the cavity in the middle of the new structure provides a buffer space for volume expansion, thereby enhancing the performance of electrochemistry and LIBs.
Drawings
FIG. 1 is 18-PC @ SiO2And 26-PC @ SiO2At a current density of 100mA g-1Cyclic performance graph of time.
FIG. 2 is 18-PC @ SiO2At a current density of 200mA g-1Cyclic performance graph of time.
FIG. 3 is 18-PC @ SiO2And 26-PC @ SiO2Ac impedance plot of (1).
Detailed Description
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following will further describe the embodiments.
The embodiment of the invention provides a preparation method of a hollow silicon dioxide coated polyhedral carbon composite material, which comprises ZIF-8@ SiO2Preparation procedure and PC @ SiO2A preparation step of the ZIF-8@ SiO2The preparation method specifically comprises the following steps:
adding 40mg of ZIF-8 powder into 204mL of absolute ethyl alcohol, and ultrasonically stirring for 5min to form a first solution;
adding 3.3mL of sodium hydroxide solution into the first solution, wherein the mass concentration of the sodium hydroxide solution is 0.1mol/L to form a second solution;
adding 2.4mL of an absolute ethyl alcohol solution containing 20% tetraethyl orthosilicate into the second solution for three times at intervals of 30min every time, adding 0.8mL of an absolute ethyl alcohol solution containing 20% tetraethyl orthosilicate every time, and stirring at room temperature for 18-26 h to form a third solution;
centrifuging the third solution to obtain a first precipitate, and subjecting the first precipitate to anhydrous ethanolCentrifugally washing for three times, and drying for 12h at 60 ℃ to obtain ZIF-8@ SiO2Powder;
the PC @ SiO2The preparation method specifically comprises the following steps:
ZIF-8@ SiO2Placing the powder into a porcelain boat, placing the porcelain boat into a vacuum furnace, and evacuating the vacuum furnace to a vacuum degree of 1.0 × 10- 2pa；
Nitrogen gas was injected into the vacuum furnace at a flow rate of 50sccm to maintain the vacuum degree of the vacuum furnace at 1.0X 10-2pa, heating the vacuum furnace from room temperature to 800 ℃ at the heating rate of 5 ℃/min, and keeping the temperature for 1.5 h;
naturally cooling the mixture to room temperature in a vacuum furnace to obtain PC @ SiO2。
Further, in ZIF-8@ SiO2In the preparation step, 2.4mL of an absolute ethyl alcohol solution containing 20% tetraethyl orthosilicate was added to the second solution three times, each time at intervals of 30min, 0.8mL of an absolute ethyl alcohol solution containing 20% tetraethyl orthosilicate was added each time, and then the mixture was stirred at room temperature for 18h to form a third solution.
Further, in ZIF-8@ SiO2In the preparation step, 2.4mL of an absolute ethyl alcohol solution containing 20% tetraethyl orthosilicate was added to the second solution three times, each time at intervals of 30min, 0.8mL of an absolute ethyl alcohol solution containing 20% tetraethyl orthosilicate was added each time, and then the mixture was stirred at room temperature for 26 hours to form a third solution.
The ZIF-8 is a metal organic framework, and the preparation method comprises the following steps: firstly, weighing 10.8g of dimethyl imidazole, ultrasonically dissolving the dimethyl imidazole in 100mL of deionized water, then transferring the solution to a magnetic stirring table, stirring the solution at room temperature, then adding 4mL of 0.01M hexadecyl trimethyl ammonium bromide (CTAB) solution, and continuously stirring the solution for 5 minutes to form a solution A; 0.7g of zinc nitrate hexahydrate (Zn (NO3) 2.6H 2O) was dissolved in 100mL of deionized water with sonication to form a solution B, which was poured into A, stirred for 5 minutes, and then allowed to stand at room temperature for 3 hours. And finally, taking the precipitate (10000 r/min 10 min) by adopting a centrifugal method, repeatedly centrifuging and washing the precipitate for 3 times by using deionized water, and drying the collected white precipitate for 12 hours at 70 ℃ to obtain ZIF-8 powder.
The above air chamberThe core silicon dioxide coated polyhedral carbon composite material is ZIF-8@ SiO2In the preparation step, the silica-coated polyhedral carbon composite material formed by stirring for 18 hours is 18-PC @ SiO when the third solution is formed2The expression is that the silicon dioxide coated polyhedral carbon composite material formed by stirring for 26h is 26-PC @ SiO2And (4) showing.
18-PC@SiO2The concrete structure is as follows: outer layer of SiO2Is hollow shell-like in SiO2The inside of the bag is wrapped with polyhedral carbon similar to egg yolk, the polyhedral carbon and SiO2The space between the two plates is a cavity, and the polyhedral carbon is porous.
26-PC@SiO2The concrete structure is as follows: outer layer of SiO2Is hollow shell-like in SiO2The inner cavity is covered with a polyhedral carbon layer, and the polyhedral carbon is also porous.
The invention prepares ZIF-8@ SiO on ZIF-8 by using an in-situ synthesis method2The precursor, tetraethyl orthosilicate (TEOS), forms Si (OH) during hydrolysis4Has an etching effect on ZIF-8, ZIF-8@ SiO2In the precursor, SiO is arranged on the outer layer2Is hollow shell-like in SiO2The inner part is ZIF-8 with reduced etching, and the outer SiO layer can be formed in one step by controlling the hydrolysis time of TEOS2Is a hollow shell, the inner layer ZIF-8 is yolk-shaped, and forms 18-PC @ SiO after high-temperature carbonization treatment2Further controlling the hydrolysis time of TEOS to form outer SiO layer2The hollow shell and the inner layer ZIF-8 are covered with the layered ZIF-8, and the 26-PC @ SiO is formed after high-temperature carbonization treatment2After high-temperature carbonization treatment, in SiO2The ZIF-8 in the inner part is porous.
18-PC@SiO2And 26-PC @ SiO2All have high specific capacity, long cycle performance and excellent rate performance.
The invention is further illustrated by the following examples and comparative examples, which are intended to illustrate the invention in detail and are not to be construed as limiting the scope of the invention in any way.
Example 1: 18-PC @ SiO2And (4) preparing.
Adding 40mg ZIF-8 powder into 204mL absolute ethanol, and ultrasonically stirring for 5min to obtain the final productAdding 3.3mL of sodium hydroxide solution to the first solution, wherein the sodium hydroxide solution has a mass concentration of 0.1mol/L to form a second solution, adding 2.4mL of an absolute ethanol solution containing 20% tetraethyl orthosilicate to the second solution in three portions at intervals of 30min, adding 0.8mL of an absolute ethanol solution containing 20% tetraethyl orthosilicate in each portion, stirring at room temperature for 18h to form a third solution, centrifuging the formed third solution to obtain a first precipitate, centrifuging and washing the first precipitate with absolute ethanol three times, drying at 60 ℃ for 12h, and drying ZIF-8@ SiO2Placing the powder into a porcelain boat, placing the porcelain boat into a vacuum furnace, and evacuating the vacuum furnace to a vacuum degree of 1.0 × 10-2pa, injecting nitrogen gas into the vacuum furnace at a flow rate of 50sccm, and maintaining the vacuum degree of the vacuum furnace at 1.0X 10-2pa, heating the vacuum furnace from room temperature to 800 ℃ at the heating rate of 5 ℃/min, keeping the temperature for 1.5h, and naturally cooling the vacuum furnace to the room temperature.
Example 2: 26-PC @ SiO2And (4) preparing.
Adding 40mg of ZIF-8 powder into 204mL of absolute ethyl alcohol, ultrasonically stirring for 5min to form a first solution, adding 3.3mL of sodium hydroxide solution into the first solution, wherein the mass concentration of the sodium hydroxide solution is 0.1mol/L to form a second solution, adding 2.4mL of absolute ethyl alcohol solution containing 20% tetraethyl orthosilicate into the second solution in three times at intervals of 30min, adding 0.8mL of absolute ethyl alcohol solution containing 20% tetraethyl orthosilicate each time, stirring for 26h at room temperature to form a third solution, centrifuging the formed third solution to obtain a first precipitate, centrifugally washing the first precipitate with absolute ethyl alcohol for three times, drying for 12h at 60 ℃, and drying for ZIF-8@ SiO2Placing the powder into a porcelain boat, placing the porcelain boat into a vacuum furnace, and evacuating the vacuum furnace to a vacuum degree of 1.0 × 10-2pa, injecting nitrogen gas into the vacuum furnace at a flow rate of 50sccm, and maintaining the vacuum degree of the vacuum furnace at 1.0X 10-2pa, heating the vacuum furnace from room temperature to 800 ℃ at the heating rate of 5 ℃/min, keeping the temperature for 1.5h, and naturally cooling the vacuum furnace to the room temperature.
FIG. 1 shows the current density of 100mA g-1When, 26-PC @ SiO2And 18-PC @ SiO2Specific capacity of the negative electrode as a function of cycle number, and coulombic efficiency. As can be seen, 26-PC @ SiO2And 18-PC @ SiO2Initial discharge capacities of 541mAh g, respectively-1708.8 mAh g-1. After 60 cycles, the corresponding specific capacity is 421 mAh g-1And 554 mAh. g-1,26-PC@SiO2And 18-PC @ SiO2The capacity retention of (2) was 77% and 78%, respectively. In a cyclic process, 18-PC @ SiO2Ratio of 26-PC @ SiO2Has a higher specific capacity, which benefits from an improved specific surface area. In practice, 26-PC @ SiO after 10 cycles2And 18-PC @ SiO2The specific capacity of the negative electrode has stabilized. Up to 60 cycles, there was little change in the specific capacity, indicating ultra-stable cycling performance. This is because the new structure for preparing the electrode is composed of carbon-oxygen hybrid nanostructures. Thus, Li+Can be directly mixed with SiO2React to promote the dynamic performance. On the other hand, the carbon layer of the hybrid product not only enhances the structure of the hybrid product, but also with Li of the hybrid product+It is related. In addition, the cavity is SiO2Provides a buffer space, thereby improving the performance of the electrochemistry and LIBs.
FIG. 2 demonstrates 18-PC @ SiO2At 200mA · g-1Long term cycling performance at current density. The initial specific discharge capacity is 662.6 mAh g-1. After that, the capacity is slightly decreased until 10 cycles are reached. After 10 cycles, due to SiO2Activation is gradually carried out under high current density, and specific capacity is increased. After 100 times of circulation, the specific capacity is stabilized at 443.9 mAh g-1And the compound shows good cycling stability.
FIG. 3 is 18-PC @ SiO2And 26-PC @ SiO2The impedance spectrum of (A) generally indicates the equivalent series resistance (R) of an element such as an electrolyte or a separator at the intersection with the real axiss) The semicircular diameter of the high frequency region represents the charge transfer resistance (R)ct). Thus, 18-PC @ SiO2And 26-PC @ SiO287.9 and 110.8 omega respectively. This is probably due to the presence of polyhedral carbon, which promotes 18-PC @ SiO2Thereby improving the electrical conductivity.
18-PC @ SiO according to FIGS. 1 to 32And 26-PC @ SiO2Has high specific capacity, long cycle performance and excellent rate performance, 18-PC @ SiO2The lithium storage performance is more excellent.
The steps in the method of the embodiment of the invention can be sequentially adjusted, combined and deleted according to actual needs.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (3)
1. The preparation method of the hollow silicon dioxide coated polyhedral carbon composite material is characterized by comprising ZIF-8@ SiO2Preparation procedure and PC @ SiO2A preparation step of the ZIF-8@ SiO2The preparation method specifically comprises the following steps:
adding 40mg of ZIF-8 powder into 204mL of absolute ethyl alcohol, and ultrasonically stirring for 5min to form a first solution;
adding 3.3mL of sodium hydroxide solution into the first solution, wherein the mass concentration of the sodium hydroxide solution is 0.1mol/L to form a second solution;
adding 2.4mL of an absolute ethyl alcohol solution containing 20% tetraethyl orthosilicate into the second solution for three times at intervals of 30min every time, adding 0.8mL of an absolute ethyl alcohol solution containing 20% tetraethyl orthosilicate every time, and stirring at room temperature for 18-26 h to form a third solution;
centrifuging the formed third solution to obtain a first precipitate, centrifuging and washing the first precipitate with absolute ethyl alcohol for three times, and drying at 60 ℃ for 12h to obtain ZIF-8@ SiO2Powder;
the PC @ SiO2The preparation method specifically comprises the following steps:
ZIF-8@ SiO2Placing the powder into a porcelain boat, placing the porcelain boat into a vacuum furnace, and evacuating the vacuum furnace to a vacuum degree of 1.0 × 10- 2pa；
Nitrogen gas was injected into the vacuum furnace at a flow rate of 50sccm to maintain the vacuum degree of the vacuum furnace at 1.0X 10-2pa, heating the vacuum furnace from room temperature to 800 ℃ at the heating rate of 5 ℃/min, and keeping the temperature for 1.5 h;
naturally cooling the mixture to room temperature in a vacuum furnace to obtain PC @ SiO2。
2. The method for preparing a hollow silica-coated polyhedral carbon composite material according to claim 1, wherein: in ZIF-8@ SiO2In the preparation step, 2.4mL of an absolute ethyl alcohol solution containing 20% tetraethyl orthosilicate was added to the second solution three times, each time at intervals of 30min, 0.8mL of an absolute ethyl alcohol solution containing 20% tetraethyl orthosilicate was added each time, and then the mixture was stirred at room temperature for 18h to form a third solution.
3. The method for preparing a hollow silica-coated polyhedral carbon composite material according to claim 1, wherein: in ZIF-8@ SiO2In the preparation step, 2.4mL of an absolute ethyl alcohol solution containing 20% tetraethyl orthosilicate was added to the second solution three times, each time at intervals of 30min, 0.8mL of an absolute ethyl alcohol solution containing 20% tetraethyl orthosilicate was added each time, and then the mixture was stirred at room temperature for 26 hours to form a third solution.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113809282A (en) * | 2021-09-17 | 2021-12-17 | 河北工业大学 | High-capacity nitrogen-doped carbon-coated SiOxPreparation method of nano-beam lithium ion battery cathode material |
| CN114335533A (en) * | 2021-12-16 | 2022-04-12 | 珠海冠宇电池股份有限公司 | Negative electrode material and battery comprising same |
| CN114361454A (en) * | 2022-01-07 | 2022-04-15 | 中创新航科技股份有限公司 | Composite carbon material for lithium-sulfur battery, preparation method thereof and lithium-sulfur battery comprising same |
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2020
- 2020-01-13 CN CN202010029937.7A patent/CN111186841A/en active Pending
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113809282A (en) * | 2021-09-17 | 2021-12-17 | 河北工业大学 | High-capacity nitrogen-doped carbon-coated SiOxPreparation method of nano-beam lithium ion battery cathode material |
| CN113809282B (en) * | 2021-09-17 | 2023-02-14 | 河北工业大学 | High-capacity nitrogen-doped carbon-coated SiO x Preparation method of nano-beam lithium ion battery cathode material |
| CN114335533A (en) * | 2021-12-16 | 2022-04-12 | 珠海冠宇电池股份有限公司 | Negative electrode material and battery comprising same |
| CN114361454A (en) * | 2022-01-07 | 2022-04-15 | 中创新航科技股份有限公司 | Composite carbon material for lithium-sulfur battery, preparation method thereof and lithium-sulfur battery comprising same |
| CN114361454B (en) * | 2022-01-07 | 2023-08-15 | 中创新航科技股份有限公司 | Composite carbon material for lithium-sulfur battery, preparation method of composite carbon material and lithium-sulfur battery comprising composite carbon material |
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Application publication date: 20200522 |