CN110833799B - Graphene-elemental silicon composite aerogel and preparation method thereof - Google Patents
Graphene-elemental silicon composite aerogel and preparation method thereof Download PDFInfo
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- C01B33/1585—Dehydration into aerogels
Abstract
The invention discloses a graphene-simple substance silicon composite aerogel and a preparation method thereof, wherein a silicon source, deionized water and absolute ethyl alcohol are uniformly mixed to obtain a mixed solution A, a graphene oxide aqueous solution is added, ultrasonic dispersion is uniform to obtain a mixed solution B, a hydrochloric acid ethanol solution is added, stirring is uniform, the pH value of the mixed solution is adjusted to 2-3, an ammonia water ethanol solution is added, stirring is uniform, the pH value of the mixed solution is adjusted to 6.5-7.8, then gelation is waited at 20-70 ℃, the obtained gel is added into the absolute ethyl alcohol for solvent replacement to obtain a composite wet gel, and then CO is carried out to obtain a composite wet gel2Performing supercritical drying treatment to obtain composite aerogel, performing high-temperature reduction to obtain graphene-silicon dioxide composite aerogel, finally mixing with magnesium powder, and performing heat treatment under the protection of inert gas to obtain the graphene-silicon dioxide composite aerogel. According to the method, the active substance simple substance silicon is used as the framework material of the aerogel, the graphene is used as the reinforcing material, the content of the active substance in the prepared graphene-simple substance silicon composite aerogel is more than 90 wt%, and the cycle performance is remarkably improved.
Description
Technical Field
The invention belongs to the technical field of preparation of inorganic nano materials with high lithium storage capacity, and particularly relates to graphene-elemental silicon composite aerogel and a preparation method thereof.
Background
With the improvement of the scientific and technical level, the demand of people on energy sources is more and more increased, people convert renewable energy sources such as solar energy, wind energy, nuclear energy, biomass energy and the like into electric energy to put into production and life, the storage of the electric energy is also changed into a new problem, and the development of a secondary battery which has high charge and discharge capacity, high cycle rate, long-term use and low cost is an effective way for realizing sustainable development. The vast majority of secondary batteries on the market today are lithium ion batteries, but the capacity of commercial graphite electrodes (376mAh/g) has been difficult to meet. Silicon-based negative electrode materials have the highest theoretical specific capacity (4200mAh/g) in the currently known materials, but a material with a stable porous structure is needed to provide space for the huge volume expansion (300%), and aerogel is the most ideal material. The existing graphene-silicon dioxide composite aerogel does not have lithium storage performance, and the graphene aerogel loaded with silicon nanoparticles has smaller capacity due to the low content of the active substance, namely simple substance silicon.
Disclosure of Invention
The invention aims to overcome the defects of low capacity, poor cyclicity of a silicon-based negative electrode material and the like of the existing commercial lithium ion battery, and provides graphene-simple substance silicon composite aerogel with higher capacity and better cyclicity and a preparation method thereof.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:
a preparation method of graphene-elemental silicon composite aerogel comprises the following steps:
(1) uniformly mixing a silicon source, deionized water and absolute ethyl alcohol to obtain a mixed solution A;
(2) adding a graphene oxide aqueous solution into the mixed solution A obtained in the step (1), and performing ultrasonic dispersion uniformly to obtain a mixed solution B;
(3) adding an ethanol hydrochloride solution into the mixed solution B obtained in the step (2), uniformly stirring, and adjusting the pH value of the mixed solution to 2-3;
(4) adding an ammonia water ethanol solution into the mixed solution obtained in the step (3), uniformly stirring, adjusting the pH value of the mixed solution to 6.5-7.8, and waiting for gelation at the temperature of 20-70 ℃;
(5) adding the gel obtained in the step (4) into absolute ethyl alcohol for solvent replacement to obtain a composite wet gel;
(6) subjecting the composite wet gel obtained in the step (5) to CO2Performing supercritical drying treatment to obtain the composite aerogel;
(7) performing high-temperature reduction on the composite aerogel obtained in the step (6), and naturally cooling to room temperature to obtain graphene-silicon dioxide composite aerogel;
(8) and (3) mixing the graphene-silicon dioxide composite aerogel obtained in the step (7) with magnesium powder, carrying out heat treatment under the protection of inert gas, naturally cooling to room temperature after the treatment is finished, soaking the product in an excessive hydrochloric acid ethanol solution, repeatedly washing with ethanol and deionized water, and drying in a vacuum drying oven to obtain the graphene-silicon dioxide composite aerogel.
Specifically, in the step (1), the silicon source is one of tetraethyl orthosilicate, tetramethyl orthosilicate or 3-aminopropyltriethoxysilane; and mixing the silicon source, the deionized water and the absolute ethyl alcohol according to a molar ratio of 1: 10-20: 5-10, preferably 1:10: 5.
Specifically, in the step (2), the concentration of the graphene oxide aqueous solution is 5-15 mg/ml, and the molar ratio of the silicon source to the graphene oxide is 1 (0.02-0.12).
Specifically, in the step (3) and the step (8), the solubility of the hydrochloric acid ethanol solution is 0.5-1.5 mol/L, and the pH of the hydrochloric acid ethanol solution is adjusted to 2-3, so that the hydrolysis reaction of a silicon source is promoted.
Specifically, in the step (4), the solubility of the ammonia-water ethanol solution is 0.5-1 mol/L, and the pH of the ammonia-water ethanol solution is adjusted to 6.5-7.8, so that the polycondensation reaction of the silicon source hydrolysate is promoted.
Specifically, in the step (5), the absolute ethyl alcohol is replaced once every 10-12 hours, the total replacement time is 6-8 times, and the absolute ethyl alcohol is subjected to solvent replacement to remove impurity ions in a gel system in a replacement manner.
Preferably, in step (6), the CO2The supercritical drying treatment is carried out under the condition of adopting CO2Under the protection of gas, the reaction temperature is 45-50 ℃, the pressure of a high-pressure reaction kettle is controlled at 10-12 MPa, the reaction time is 12-24 h, and CO is added2The supercritical drying treatment converts the liquid phase solvent in the gel system into gas phase and maintains the skeleton structure.
Preferably, in the step (7), the reducing atmosphere of the high-temperature reduction is nitrogen or argon, the reducing temperature is 400-500 ℃, the heating rate is 2-4 ℃/min, and the reducing time is 2-3 h; and reducing the graphene oxide into graphene by high-temperature reduction.
Preferably, in the step (8), the molar ratio of the graphene-silicon dioxide composite aerogel to the magnesium powder is 1 (2-2.5); heating the heat treatment to 650-700 ℃ at a heating rate of 2-4 ℃/min, and keeping the temperature for 2-3 h; soaking the product in an excessive ethanol hydrochloride solution for 18-24 hours; the drying temperature is 50-70 ℃; the silica is reduced to elemental silicon by magnesiothermic reduction.
The graphene-elemental silicon composite aerogel prepared by the preparation method is also within the protection scope of the invention.
Has the advantages that:
according to the method, the active substance simple substance silicon is used as a framework material of the aerogel, the graphene is used as a reinforcing material, and in the prepared graphene-simple substance silicon composite aerogel, the content of the active substance simple substance silicon is more than 90 wt%, and the lithium storage capacity is large; the graphene-simple substance silicon composite aerogel enhances the structural strength of the aerogel by means of the unique pore structure of the aerogel and the graphene, so that the aerogel structure cannot be damaged due to the volume expansion of silicon, and the cycle performance is obviously improved.
Drawings
The foregoing and/or other advantages of the invention will become further apparent from the following detailed description of the invention when taken in conjunction with the accompanying drawings.
Fig. 1 is a photograph of a graphene-elemental silicon composite aerogel prepared in example 1.
Fig. 2 is an SEM photograph of the graphene-elemental silicon composite aerogel prepared in example 1.
Fig. 3 is a graph of cycle efficiency of the graphene-elemental silicon composite aerogel prepared in example 1.
Detailed Description
The invention will be better understood from the following examples.
Example 1
1mol of tetraethyl orthosilicate, 10mol of deionized water and 5mol of absolute ethyl alcohol are uniformly stirred for 5min, then 0.02mol of 10mg/ml graphene oxide aqueous solution is added into the mixed solution, and ultrasonic dispersion is carried out for 30 min. Then adding 1mol/L hydrochloric acid ethanol solution, measuring the pH value of the solution to 2 by a pH test paper, and stirring for 20 min. Finally adding 0.5mol/L ammonia water ethanol solution, and measuring the pH valueMeasuring pH to 6.5, stirring for 5min, pouring into a mold, and waiting for gelation at 20 deg.C. And (3) replacing impurity ions in the wet gel for 6 times by using absolute ethyl alcohol as an aging solution, wherein each time is 10 hours. Then the composite wet gel is put into a high-temperature high-pressure kettle, and CO is utilized2Drying the sample by supercritical drying method, wherein the CO2The pressure is controlled at 10MPa, the temperature is controlled at 45 ℃, and the supercritical drying time is 12 h. And then heating the sample to 400 ℃ at a heating rate of 2 ℃/min under the protection of nitrogen atmosphere, keeping the temperature for 2 hours, and cooling to room temperature to obtain the graphene-silicon dioxide composite aerogel. Mixing 1mol of graphene-silicon dioxide composite aerogel and 2mol of magnesium powder in a vacuum glove box in an argon environment, and sealing in a stainless steel reaction container. Heating the stainless steel reaction vessel to 650 ℃ at the heating rate of 2 ℃/min under the protection of argon atmosphere, carrying out heat treatment for 2h, naturally cooling to room temperature, and taking out the product in the vessel. And finally, soaking the product in an excessive 1mol/L hydrochloric acid ethanol solution for 18h, then repeatedly centrifuging and cleaning for 6 times by using ethanol and deionized water, wherein the rotation speed of a centrifuge is 8000r/min, the centrifuging time is 4min each time, and placing the product in a vacuum drying oven at 50 ℃ for drying to obtain the graphene-simple substance silicon composite aerogel. The picture of the solid is shown in figure 1, and the SEM picture is shown in figure 2. The characterization shows that: the specific surface area of the prepared graphene-elemental silicon composite aerogel is 425.96m2The content of the active substance simple substance silicon is more than 90 wt%, and the circulation efficiency is maintained at 87.86% after the circulation for 400 times under the current density of 200mA/g (see figure 3).
Example 2
1mol of tetraethyl orthosilicate, 20mol of deionized water and 10mol of absolute ethyl alcohol are uniformly stirred for 5min, then 0.12mol of 10mg/ml graphene oxide aqueous solution is added into the mixed solution, and ultrasonic dispersion is carried out for 40 min. Then adding 1mol/L hydrochloric acid ethanol solution, measuring the pH value of the solution to be 3 by a pH test paper, and stirring for 30 min. And finally adding 0.5mol/L ammonia water ethanol solution, measuring the pH value of the solution to 7.8 by a pH meter, stirring for 10min, pouring into a mold, and waiting for gelation at 70 ℃. And (3) replacing impurity ions in the wet gel for 8 times by using absolute ethyl alcohol as an aging solution, wherein each time is 12 hours. Then the composite wet gel is put into a high-temperature autoclave for utilizationCO2Drying the sample by supercritical drying method, wherein the CO2The pressure is controlled at 12MPa, the temperature is controlled at 50 ℃, and the supercritical drying time is 24 h. And then heating the sample to 500 ℃ at a heating rate of 4 ℃/min under the protection of nitrogen atmosphere, keeping the temperature for 3 hours, and cooling to room temperature to obtain the graphene-silicon dioxide composite aerogel. 1mol of graphene-silicon dioxide composite aerogel and 2.5mol of magnesium powder are mixed in a vacuum glove box in an argon environment and sealed in a stainless steel reaction vessel. Heating the stainless steel reaction vessel to 700 ℃ at the heating rate of 4 ℃/min under the protection of argon atmosphere, carrying out heat treatment for 3h, naturally cooling to room temperature, and taking out the product in the vessel. And finally, soaking the product in an excessive 1mol/L hydrochloric acid ethanol solution for 24 hours, then repeatedly centrifuging and cleaning the product for 8 times by using ethanol and deionized water, wherein the rotation speed of a centrifuge is 10000r/min, the centrifuging time is 6min each time, and placing the product in a vacuum drying oven at 70 ℃ for drying to obtain the graphene-simple substance silicon composite aerogel. The characterization shows that: the specific surface area of the prepared graphene-elemental silicon composite aerogel is 293.01m2The circulation efficiency is maintained at 84.51% after 400 times of circulation under the current density of 200 mA/g.
Example 3
1mol of tetraethyl orthosilicate, 10mol of deionized water and 10mol of absolute ethyl alcohol are uniformly stirred for 7min, then 0.10mol of 10mg/ml graphene oxide aqueous solution is added into the mixed solution, and ultrasonic dispersion is carried out for 35 min. Then adding 1mol/L hydrochloric acid ethanol solution, measuring the pH value of the solution to 2 by a pH test paper, and stirring for 30 min. And finally adding 0.5mol/L ammonia water ethanol solution, measuring the pH value of the solution to 7.0 by a pH meter, stirring for 5min, pouring into a mold, and waiting for gelation at 50 ℃. And (3) replacing impurity ions in the wet gel for 6 times by using absolute ethyl alcohol as an aging solution, wherein each time is 12 hours. Then the composite wet gel is put into a high-temperature high-pressure kettle, and CO is utilized2Drying the sample by supercritical drying method, wherein the CO2The pressure is controlled at 10MPa, the temperature is controlled at 50 ℃, and the supercritical drying time is 24 h. And then heating the sample to 450 ℃ at a heating rate of 3 ℃/min under the protection of a nitrogen atmosphere, keeping the temperature for 3 hours, and cooling to room temperature to obtain the graphene-silicon dioxide composite aerogel. Will 1mixing mol of graphene-silicon dioxide composite aerogel and 2mol of magnesium powder in a vacuum glove box in an argon environment, and sealing in a stainless steel reaction container. Heating a stainless steel reaction vessel to 700 ℃ at a heating rate of 3 ℃/min under the protection of argon atmosphere, carrying out heat treatment for 2h, naturally cooling to room temperature, and taking out a product in the vessel. And finally, soaking the product in an excessive 1mol/L hydrochloric acid ethanol solution for 18h, then repeatedly centrifuging and cleaning for 6 times by using ethanol and deionized water, wherein the rotation speed of a centrifuge is 10000r/min, the centrifugation time is 5min each time, and drying in a vacuum drying oven at 60 ℃ to obtain the graphene-simple substance silicon composite aerogel. The characterization shows that: the specific surface area of the prepared graphene-elemental silicon composite aerogel is 382.21m2The circulation efficiency is kept at 86.03 percent after the circulation for 400 times under the current density of 200 mA/g.
Example 4
1mol of tetraethyl orthosilicate, 15mol of deionized water and 8mol of absolute ethyl alcohol are uniformly stirred for 6min, then 0.05mol of 10mg/ml graphene oxide aqueous solution is added into the mixed solution, and ultrasonic dispersion is carried out for 35 min. Then 1mol/L hydrochloric acid ethanol solution is added, the pH value of the solution is measured by a pH measuring instrument to reach 3, and the solution is stirred for 25 min. And finally adding 0.5mol/L ammonia water ethanol solution, measuring the pH value of the solution to 7.2 by a pH meter, stirring for 6min, pouring into a mold, and waiting for gelation at 40 ℃. And replacing impurity ions in the wet gel with anhydrous ethanol as aging solution for 7 times, each time for 11 h. Then the composite wet gel is put into a high-temperature high-pressure kettle, and CO is utilized2Drying the sample by supercritical drying method, wherein the CO2The pressure is controlled at 11MPa, the temperature is controlled at 45 ℃, and the supercritical drying time is 18 h. And then heating the sample to 500 ℃ at a heating rate of 3 ℃/min under the protection of argon atmosphere, keeping the temperature for 3 hours, and cooling to room temperature to obtain the graphene-silicon dioxide composite aerogel. 1mol of graphene-silicon dioxide composite aerogel and 2.2mol of magnesium powder are mixed in a vacuum glove box in an argon environment and sealed in a stainless steel reaction vessel. Heating the stainless steel reaction vessel to 700 ℃ at the heating rate of 4 ℃/min under the protection of argon atmosphere, carrying out heat treatment for 2.5h, naturally cooling to room temperature, and taking out the product in the vessel. Most preferablyAnd then, soaking the product in an excessive 1mol/L hydrochloric acid ethanol solution for 20 hours, then repeatedly centrifuging and cleaning the product for 8 times by using ethanol and deionized water, wherein the rotating speed of a centrifuge is 9000r/min, the centrifuging time of each time is 5min, and placing the product in a vacuum drying oven at 50 ℃ for drying to obtain the graphene-simple substance silicon composite aerogel. The characterization shows that: the specific surface area of the prepared graphene-elemental silicon composite aerogel is 323.16m2The circulation efficiency is kept at 85.24 percent after the circulation for 400 times under the current density of 200 mA/g.
The invention provides a graphene-elemental silicon composite aerogel and a preparation method thereof, and a plurality of methods and ways for specifically implementing the technical scheme, and the above description is only a preferred embodiment of the invention, and it should be noted that, for those skilled in the art, a plurality of improvements and decorations can be made without departing from the principle of the invention, and these improvements and decorations should also be regarded as the protection scope of the invention. All the components not specified in the present embodiment can be realized by the prior art.
Claims (9)
1. The preparation method of the graphene-elemental silicon composite aerogel is characterized by comprising the following steps:
(1) uniformly mixing a silicon source, deionized water and absolute ethyl alcohol to obtain a mixed solution A;
(2) adding a graphene oxide aqueous solution into the mixed solution A obtained in the step (1), and performing ultrasonic dispersion uniformly to obtain a mixed solution B;
(3) adding an ethanol hydrochloride solution into the mixed solution B obtained in the step (2), uniformly stirring, and adjusting the pH value of the mixed solution to 2-3;
(4) adding an ammonia water ethanol solution into the mixed solution obtained in the step (3), uniformly stirring, adjusting the pH value of the mixed solution to 6.5-7.8, and waiting for gelation at the temperature of 20-70 ℃;
(5) adding the gel obtained in the step (4) into absolute ethyl alcohol for solvent replacement to obtain a composite wet gel;
(6) subjecting the composite wet gel obtained in the step (5) to CO2Performing supercritical drying treatment to obtain the composite aerogel;
(7) performing high-temperature reduction on the composite aerogel obtained in the step (6), and naturally cooling to room temperature to obtain graphene-silicon dioxide composite aerogel;
(8) mixing the graphene-silicon dioxide composite aerogel obtained in the step (7) with magnesium powder, carrying out heat treatment under the protection of inert gas, naturally cooling to room temperature after the treatment is finished, soaking the product in an excessive hydrochloric acid ethanol solution, repeatedly washing with ethanol and deionized water, and drying in a vacuum drying oven to obtain the graphene-silicon dioxide composite aerogel;
in the step (7), the reducing atmosphere of the high-temperature reduction is nitrogen or argon, the reducing temperature is 400-500 ℃, the heating rate is 2-4 ℃/min, and the reducing time is 2-3 h;
in the step (8), the heat treatment is carried out at a heating rate of 2-4 ℃/min until the temperature is 650-700 ℃, and the heat is preserved for 2-3 h.
2. The preparation method of the graphene-elemental silicon composite aerogel according to claim 1, wherein in the step (1), the silicon source is one of tetraethyl orthosilicate, tetramethyl orthosilicate or 3-aminopropyltriethoxysilane; and mixing a silicon source, deionized water and absolute ethyl alcohol according to a molar ratio of 1 (10-20) to 5-10.
3. The preparation method of the graphene-elemental silicon composite aerogel according to claim 1, wherein in the step (2), the concentration of the graphene oxide aqueous solution is 5-15 mg/ml, and the molar ratio of the silicon source to the graphene oxide is 1 (0.02-0.12).
4. The preparation method of the graphene-elemental silicon composite aerogel according to claim 1, wherein in the step (3) and the step (8), the solubility of the ethanol hydrochloride solution is 0.5-1.5 mol/L.
5. The preparation method of the graphene-elemental silicon composite aerogel according to claim 1, wherein in the step (4), the solubility of the ammonia water ethanol solution is 0.5-1 mol/L.
6. The preparation method of the graphene-elemental silicon composite aerogel according to claim 1, wherein in the step (5), the absolute ethyl alcohol is replaced every 10-12 hours for 6-8 times.
7. The method for preparing the graphene-elemental silicon composite aerogel according to claim 1, wherein in the step (6), the CO is added2The supercritical drying treatment is carried out under the condition of adopting CO2And (3) under the protection of gas, controlling the reaction temperature to be 45-50 ℃, the pressure of the high-pressure reaction kettle to be 10-12 MPa, and the reaction time to be 12-24 h.
8. The preparation method of the graphene-elemental silicon composite aerogel according to claim 1, wherein in the step (8), the molar ratio of the graphene-silica composite aerogel to the magnesium powder is 1 (2-2.5); soaking the product in an excessive ethanol hydrochloride solution for 18-24 hours; the drying temperature is 50-70 ℃.
9. The graphene-elemental silicon composite aerogel prepared by the preparation method of any one of claims 1 to 8.
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| CN112934211B (en) * | 2021-01-29 | 2022-01-25 | 广西交科集团有限公司 | Preparation method of silica aerogel with photocatalytic activity |
| CN114023941A (en) * | 2021-11-09 | 2022-02-08 | 江苏科技大学 | Rice hull-based silicon oxide/graphene aerogel composite negative electrode material and preparation method and application thereof |
| CN115490524A (en) * | 2022-05-27 | 2022-12-20 | 南京工业大学 | Preparation method of enhanced high-temperature-resistant silicon-based ceramic aerogel |
| CN115181489B (en) * | 2022-08-02 | 2023-07-21 | 亚士漆(上海)有限公司 | Sound-absorbing coating and preparation method and application thereof |
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