CN111285397A - Method for hydro-thermal synthesis of ultrathin hexagonal tin disulfide nanosheets - Google Patents
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Abstract
The invention relates to a method for hydro-thermal synthesis of an ultrathin hexagonal tin disulfide nanosheet. The problem that the tin disulfide nanosheet produced in the prior art is serious in aggregation degree and thick in lamella and does not meet the requirements of the nanosheet is solved. The method comprises the following steps: 1) respectively weighing a tin source and a sulfur source, adding deionized water, stirring on a magnetic stirrer until the tin source and the sulfur source are completely dissolved to form a transparent solution, dropwise adding glacial acetic acid, and continuously stirring uniformly to obtain a mixed solution; 2) transferring the mixed solution into a polytetrafluoroethylene inner container with the capacity of 50ml, sealing the high-pressure reaction kettle, putting the reaction kettle into an oven, heating and reacting for a period of time, and standing until the temperature is cooled to room temperature after the reaction is finished; 3) the supernatant in the reaction kettle is discarded, and the yellow precipitate at the bottom is centrifugally cleaned for three times by using absolute ethyl alcohol and deionized water respectively to remove redundant reactants and impurities; 4) and after cleaning, putting the precipitate into an oven, and performing vacuum drying to obtain a tin disulfide sample.
Description
Technical Field
The invention relates to the technical field of nano material preparation, in particular to a method for hydro-thermally synthesizing an ultrathin hexagonal tin disulfide nanosheet.
Background
The two-dimensional material is a nano material with a layered structure, the layers of the two-dimensional material are combined through Van der Waals force, the two-dimensional material has a huge specific surface area compared with a bulk material, and the two-dimensional material becomes a research hotspot in recent years due to the special layered crystal structure and excellent chemical and physical properties due to the reduction of dimensionality.
The tin disulfide in a lamellar structure is bonded between layers by weak van der waals forces, which means that tin disulfide has the characteristics of a typical two-dimensional material. The lamellar tin disulfide can meet the requirements of the semiconductor characteristics and the dimensional characteristics at present, has excellent photoelectric performance, the photoelectric conversion efficiency of the lamellar tin disulfide is as high as 38.7%, and compared with the lamellar tin disulfide, the conversion efficiency of the lamellar tin disulfide of the bulk material is only 2.33%, which is far greater than that of other materials; meanwhile, the micro-nano electronic component is widely applied, so that the micro-nano electronic component is widely concerned by scientific research practitioners.
In the Chinese patent 'preparation method of hexagonal tin disulfide nanosheet' (CN101844799A), C is utilized14-C20The alkylamine surfactant is characterized in that a tin source and a sulfur source are directly added to form a reaction solution, and the molar ratio of the added alkylamine is controlled to enable the anisotropic growth of the hexagonal tin disulfide nanosheet to achieve a good growth effect, but the aggregation degree of the product obtained by the method is serious.
In a patent 'a method for preparing hexagonal nanosheets by a hydrothermal method' (CN107032391A), a tin disulfide nanosheet is prepared in an alkaline environment, the nanosheet prepared by the method is in a hexagonal structure with the side length of about 4 microns and the thickness of about 1 micron, and the nanosheet is thick and does not meet the requirements of nanosheet level.
Disclosure of Invention
In view of the above, the invention provides a method for hydrothermally synthesizing an ultrathin hexagonal tin disulfide nanosheet, which aims to solve the problems that the tin disulfide nanosheet produced in the prior art is serious in aggregation degree and thick in lamella, and does not meet the requirements of the nanosheet.
In order to solve the problems in the prior art, the technical scheme of the invention is as follows: a method for hydro-thermal synthesis of ultrathin hexagonal tin disulfide nanosheets is characterized by comprising the following steps: the method comprises the following steps:
1) respectively weighing 2-5 mmol of tin source and 6-13 mmol of sulfur source, adding 50mL of deionized water, stirring on a magnetic stirrer until the tin source and the sulfur source are completely dissolved to form a transparent solution, dropwise adding 1-3 mL of glacial acetic acid, and then continuously stirring uniformly to obtain a mixed solution;
2) transferring the mixed solution into a polytetrafluoroethylene inner container with the capacity of 50ml, sealing the high-pressure reaction kettle, putting the reaction kettle into an oven, heating and reacting for a period of time, and standing until the temperature is cooled to room temperature after the reaction is finished;
3) the supernatant in the reaction kettle is discarded, and the yellow precipitate at the bottom is centrifugally cleaned for three times by using absolute ethyl alcohol and deionized water respectively to remove redundant reactants and impurities;
4) and after cleaning, putting the precipitate into an oven, and performing vacuum drying to obtain a tin disulfide sample.
In the step 1), the tin source is stannic chloride pentahydrate, and the sulfur source is thioacetamide.
The temperature of the oven in the step 2) is 150-200 ℃, and the reaction time is 6-24 h.
The centrifugal speed in the step 3) is 8000-10000 rpm; the centrifugation time is 5-15 min.
In the step 4), the drying temperature is 60-80 ℃, and the drying time is 6-12 h.
Compared with the prior art, the invention has the following advantages:
1) according to the invention, glacial acetic acid is used as a surfactant, so that a good guiding effect is provided for anisotropic growth of the hexagonal tin disulfide nanosheet, a good growth limiting effect is also achieved on the hexagonal tin disulfide nanosheet, the hexagonal tin disulfide nanosheet is enabled to have a small size, and the prepared tin disulfide nanosheet is smaller in thickness and about 10nm compared with the prior art.
2) The invention adopts a hydrothermal method, and the method has the advantages of low raw material cost, simple operation process and high preparation efficiency. The diameter of the prepared tin disulfide ultrathin hexagonal nanosheet is about 30-50 nm, and the thickness of the prepared tin disulfide ultrathin hexagonal nanosheet is about 10 nm; the hexagonal tin disulfide nanosheet can be self-assembled into a columnar nano superstructure, and can be widely applied to the fields of light detection, solar cells, energy storage, photocatalysis and the like.
Description of the drawings:
FIG. 1 is an X-ray diffraction pattern of flake tin disulfide obtained in accordance with embodiments 1-4 of the present invention;
fig. 2(a) is a transmission electron microscope image of the flake tin disulfide obtained in example 1 of the present invention, and (b) is a high resolution transmission electron microscope image of the flake tin disulfide obtained in example 1 of the present invention;
FIG. 3(a) is a logarithmic plot of current of a group change memory prepared from a hydrothermal tin disulfide nanosheet in example 1 of the present invention; (b) the distribution curve of the high and low resistance values of the group change memory prepared by the tin disulfide nanosheet prepared by the hydrothermal method in the embodiment 1 of the invention is shown.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1:
the method for hydro-thermally synthesizing the ultrathin hexagonal tin disulfide nanosheet comprises the following steps:
1) respectively weighing 2mmol of stannic chloride pentahydrate and 6mmol of thioacetamide, adding into a 200ml beaker, adding 50ml of deionized water, stirring on a magnetic stirrer until the deionized water is completely dissolved to form a transparent solution, dropwise adding 1ml of glacial acetic acid, and then continuing to stir uniformly by magnetic force to prepare a reaction solution of stannic sulfide;
2) transferring the reaction liquid of tin disulfide into a polytetrafluoroethylene inner container with the capacity of 50ml, sealing the high-pressure reaction kettle, putting the reaction kettle into an oven, maintaining the reaction kettle in a digital temperature control box at 150 ℃ for hydrothermal reaction for 20 hours, and standing until the reaction is cooled to room temperature after the reaction is finished;
3) discarding the supernatant in the reaction kettle, and centrifugally cleaning the yellow precipitate at the bottom three times by using absolute ethyl alcohol and deionized water respectively, wherein the centrifugal speed is 8000 rpm; centrifuging for 5min to remove excessive reactant and impurities;
4) and after the cleaning is finished, putting the obtained precipitate into an oven at 60 ℃ for vacuum drying for 6h to obtain a tin disulfide sample.
The X-ray diffraction pattern of the obtained flaky tin disulfide is shown as a curve 1 in the attached figure 1. FIG. 2(a) is a transmission electron micrograph of the obtained flaky tin disulfide, which shows that the obtained flaky tin disulfide is a hexagonal flaky nano structure, and the diameter of the flaky tin disulfide is about 30-50 nm; FIG. 2(b) is a high resolution TEM image of the resulting tin disulfide layer, which shows a thickness of about 10 nm. FIG. 3(a) is a graph showing I-V curves in logarithmic coordinates of the current of a group change memory prepared from the obtained tin disulfide nanosheets; FIG. 3(b) is a graph showing the distribution of high and low resistance values of a group-change memory prepared from the obtained tin disulfide nanosheets, with an on-off ratio of about 103。
Example 2:
the method for hydro-thermally synthesizing the ultrathin hexagonal tin disulfide nanosheet comprises the following steps:
1) respectively weighing 3mmol of stannic chloride pentahydrate and 8mmol of thioacetamide, adding into a 200ml beaker, adding 50ml of deionized water, stirring on a magnetic stirrer until the deionized water is completely dissolved to form a transparent solution, dropwise adding 2ml of glacial acetic acid, and then continuing to stir uniformly by magnetic force to prepare a reaction solution of stannic sulfide;
2) transferring the reaction liquid of tin disulfide into a polytetrafluoroethylene inner container with the capacity of 50ml, sealing the high-pressure reaction kettle, putting the reaction kettle into an oven, maintaining the reaction kettle in a digital temperature control box at 160 ℃ for hydrothermal reaction for 21 hours, and standing until the reaction is cooled to room temperature after the reaction is finished;
3) discarding the supernatant in the reaction kettle, and centrifugally cleaning the yellow precipitate at the bottom three times by using absolute ethyl alcohol and deionized water respectively, wherein the centrifugal speed is 8500 rpm; centrifuging for 10min to remove excessive reactant and impurities;
4) and after the cleaning is finished, putting the obtained precipitate into an oven at 70 ℃ for vacuum drying for 7h to obtain a tin disulfide sample.
The X-ray diffraction pattern of the obtained flaky tin disulfide is shown as a curve 2 in the attached figure 1.
Example 3:
the method for hydro-thermally synthesizing the ultrathin hexagonal tin disulfide nanosheet comprises the following steps:
1) respectively weighing 4mmol of stannic chloride pentahydrate and 10mmol of thioacetamide, adding into a 200ml beaker, adding 50ml of deionized water, stirring on a magnetic stirrer until the deionized water is completely dissolved to form a transparent solution, dropwise adding 3ml of glacial acetic acid, and then continuing to stir uniformly by magnetic force to prepare a reaction solution of stannic sulfide;
2) transferring the reaction liquid of tin disulfide into a polytetrafluoroethylene inner container with the capacity of 50ml, sealing the high-pressure reaction kettle, putting the reaction kettle into an oven, maintaining the reaction kettle in a digital temperature control box at 180 ℃ for hydrothermal reaction for 23 hours, and standing until the reaction is cooled to room temperature after the reaction is finished;
3) the supernatant in the reaction kettle is discarded, and the yellow precipitate at the bottom is centrifugally cleaned for three times by absolute ethyl alcohol and deionized water respectively, wherein the centrifugal speed is 9000 rpm; centrifuging for 13min to remove excessive reactant and impurities;
4) and after the cleaning is finished, putting the obtained precipitate into an oven at 70 ℃ for vacuum drying for 10h to obtain a tin disulfide sample.
The X-ray diffraction pattern of the obtained flaky tin disulfide is shown as a curve 3 in the attached figure 1.
Example 4:
the method for hydro-thermally synthesizing the ultrathin hexagonal tin disulfide nanosheet comprises the following steps:
1) respectively weighing 5mmol of stannic chloride pentahydrate and 13mmol of thioacetamide, adding into a 200ml beaker, adding 50ml of deionized water, stirring on a magnetic stirrer until the deionized water is completely dissolved to form a transparent solution, dropwise adding 3ml of glacial acetic acid, and then continuing to stir uniformly by magnetic force to prepare a reaction solution of stannic sulfide;
2) transferring the reaction solution of tin disulfide into a polytetrafluoroethylene inner container with the capacity of 50ml, sealing the high-pressure reaction kettle, putting the reaction kettle into an oven, maintaining the reaction kettle in a digital temperature control box at 200 ℃ for hydrothermal reaction for 24 hours, and standing until the reaction is cooled to room temperature after the reaction is finished.
3) Discarding the supernatant in the reaction kettle, and centrifugally cleaning the yellow precipitate at the bottom three times by using absolute ethyl alcohol and deionized water respectively, wherein the centrifugal speed is 10000 rpm; centrifuging for 15min to remove excessive reactant and impurities;
4) and after the cleaning is finished, putting the obtained precipitate into an oven at 80 ℃ for vacuum drying for 12h to obtain a tin disulfide sample.
The X-ray diffraction pattern of the obtained flaky tin disulfide is shown as a curve 4 in the attached figure 1.
The above example 1 is the most preferred embodiment. Referring to fig. 1, it can be seen that under the conditions of example 1, the diffraction peak completely conforms to the hexagonal tin disulfide structure, and a diffraction peak is obvious on the (102) crystal face, indicating that the product is pure crystalline.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and it should be noted that those skilled in the art should make modifications and variations without departing from the principle of the present invention.
Claims (5)
1. A method for hydro-thermal synthesis of ultrathin hexagonal tin disulfide nanosheets is characterized by comprising the following steps: the method comprises the following steps:
1) respectively weighing 2-5 mmol of tin source and 6-13 mmol of sulfur source, adding 50mL of deionized water, stirring on a magnetic stirrer until the tin source and the sulfur source are completely dissolved to form a transparent solution, dropwise adding 1-3 mL of glacial acetic acid, and then continuously stirring uniformly to obtain a mixed solution;
2) transferring the mixed solution into a polytetrafluoroethylene inner container with the capacity of 50ml, sealing the high-pressure reaction kettle, putting the reaction kettle into an oven, heating and reacting for a period of time, and standing until the temperature is cooled to room temperature after the reaction is finished;
3) the supernatant in the reaction kettle is discarded, and the yellow precipitate at the bottom is centrifugally cleaned for three times by using absolute ethyl alcohol and deionized water respectively to remove redundant reactants and impurities;
4) and after cleaning, putting the precipitate into an oven, and performing vacuum drying to obtain a tin disulfide sample.
2. The method for hydrothermally synthesizing the ultra-thin hexagonal tin disulfide nanosheet according to claim 1, wherein: in the step 1), the tin source is stannic chloride pentahydrate, and the sulfur source is thioacetamide.
3. The method for hydrothermally synthesizing the ultra-thin hexagonal tin disulfide nanosheet according to claim 1 or 2, wherein: in the step 2), the temperature of the oven is 150-200 ℃, and the reaction time is 6-24 h.
4. The method for hydrothermally synthesizing the ultra-thin hexagonal tin disulfide nanosheet according to claim 3, wherein: the centrifugal speed in the step 3) is 8000-10000 rpm; the centrifugation time is 5-15 min.
5. The method for hydrothermally synthesizing the ultra-thin hexagonal tin disulfide nanosheet according to claim 4, wherein: in the step 4), the drying temperature is 60-80 ℃, and the drying time is 6-12 h.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111777095A (en) * | 2020-07-20 | 2020-10-16 | 洛阳布鲁姆电子科技有限公司 | Synthesis method of tin disulfide microspheres |
CN111871431A (en) * | 2020-08-27 | 2020-11-03 | 东北师范大学 | Tin disulfide/gold composite catalyst and preparation method and application thereof |
CN112164787A (en) * | 2020-09-25 | 2021-01-01 | 贵港益乐科技发展有限公司 | Three-dimensional SnS2Lithium ion battery cathode material for modifying N-doped mesoporous carbon |
CN113200565A (en) * | 2021-05-08 | 2021-08-03 | 湖南工学院 | Flaky tin disulfide and preparation method and application thereof |
CN113753942A (en) * | 2021-08-25 | 2021-12-07 | 天津大学 | Transition metal doped stannic disulfide nanoflower and preparation method thereof |
CN114380325A (en) * | 2021-12-11 | 2022-04-22 | 上海工程技术大学 | Ultra-thin SnS2Nanosheet and SnS2Film, preparation and application thereof |
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111777095A (en) * | 2020-07-20 | 2020-10-16 | 洛阳布鲁姆电子科技有限公司 | Synthesis method of tin disulfide microspheres |
CN111777095B (en) * | 2020-07-20 | 2022-09-09 | 洛阳布鲁姆电子科技有限公司 | Synthesis method of tin disulfide microspheres |
CN111871431A (en) * | 2020-08-27 | 2020-11-03 | 东北师范大学 | Tin disulfide/gold composite catalyst and preparation method and application thereof |
CN111871431B (en) * | 2020-08-27 | 2022-09-20 | 东北师范大学 | Tin disulfide/gold composite catalyst, and preparation method and application thereof |
CN112164787A (en) * | 2020-09-25 | 2021-01-01 | 贵港益乐科技发展有限公司 | Three-dimensional SnS2Lithium ion battery cathode material for modifying N-doped mesoporous carbon |
CN113200565A (en) * | 2021-05-08 | 2021-08-03 | 湖南工学院 | Flaky tin disulfide and preparation method and application thereof |
CN113753942A (en) * | 2021-08-25 | 2021-12-07 | 天津大学 | Transition metal doped stannic disulfide nanoflower and preparation method thereof |
CN114380325A (en) * | 2021-12-11 | 2022-04-22 | 上海工程技术大学 | Ultra-thin SnS2Nanosheet and SnS2Film, preparation and application thereof |
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