CN111268722A - Method for preparing tin disulfide with vertical array structure at normal temperature in situ - Google Patents
Method for preparing tin disulfide with vertical array structure at normal temperature in situ Download PDFInfo
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- CN111268722A CN111268722A CN202010129129.8A CN202010129129A CN111268722A CN 111268722 A CN111268722 A CN 111268722A CN 202010129129 A CN202010129129 A CN 202010129129A CN 111268722 A CN111268722 A CN 111268722A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/78—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by stacking-plane distances or stacking sequences
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- 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
Abstract
The invention belongs to the field of nano material manufacturing, and particularly relates to a method for preparing tin disulfide with a vertical array structure at normal temperature in situ. The method comprises the following steps: dispersing common layered tin disulfide on a semi-carbon film by ultrasonic, touching the tin disulfide with a tungsten needle tip scraped with lithium metal in a transmission electron microscope, and applying voltage; and converging the electron beams to irradiate the sample to obtain the tin disulfide with a vertical array structure. The method does not need high temperature and other toxic and harmful chemical reagents, thereby simplifying the process and reducing the production cost.
Description
Technical Field
The invention belongs to the field of nano material manufacturing, and particularly relates to a method for preparing tin disulfide with a vertical array structure at normal temperature in situ.
Background
With the rapid development of society, the problem of environmental pollution is increasingly prominent, and under the large background that non-renewable resources are increasingly in short supply, in order to ensure that economy and science and technology can be stably and continuously developed, the full utilization of materials with large natural reserves and environmental friendliness to replace materials with limited reserves and serious pollution becomes a great trend. In the transition metal sulfide, tin disulfide is an n-type semiconductor material with the band gap width of 2.2-2.5eV, each layer of Sn atoms is connected with S atoms through stronger Sn-S covalent bonds, and the layers are connected through weaker Van der Waals force. Sn is located in the center of an octahedron composed of six sulfur atoms. The photocatalyst has the advantages of rich reserves, low price, high photocatalytic efficiency, large energy storage capacity and the like, and has wide application prospects in the fields of photoelectric detection, solar cells, energy storage and the like. Tin disulfide with vertical array morphology shows huge potential in energy conversion and storage due to high density of electrochemical reaction exposed edge sites.
At present, the methods for preparing the transition metal sulfide with the vertical array morphology mainly comprise a hydrothermal method and a CVD method. The hydrothermal method for preparing the transition metal sulfide with the vertical array morphology has the main problems that the hydrothermal reaction temperature is usually over 160 ℃, the raw materials are complex, the reaction time is long, and the prepared sample is serious in agglomeration and poor in dispersibility. The product obtained by the hydrothermal reaction needs to be further cleaned, and waste water is generated. The energy consumption of the CVD method is too high, and the reaction temperature is usually over 500 ℃, which causes great energy consumption.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for preparing tin disulfide with a vertical array structure at normal temperature in situ. The method does not need high temperature and other toxic and harmful chemical reagents, thereby simplifying the process and reducing the production cost.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a method for preparing tin disulfide with a vertical array structure at normal temperature in situ comprises the following steps: dispersing common layered tin disulfide on a semi-carbon film by ultrasonic, touching the tin disulfide with a tungsten needle tip scraped with lithium metal in a transmission electron microscope, and applying voltage; and converging the electron beams to irradiate the sample to obtain the tin disulfide with a vertical array structure.
Preferably, the ultrasonic dispersion time is 10 to 30 minutes.
Preferably, the voltage is (-0.1-5) V.
Preferably, the beam current density range of the electron beam during irradiation is 1.0 x 104A/m2- 1.0×106A/ m2。
Preferably, the irradiation time is 1 to 20 minutes.
Compared with the prior art, the invention has the following beneficial effects:
(1) the traditional method for preparing the tin disulfide with the vertical array structure has complex reactants and high energy consumption, the used chemical reagents are few in types, the sample is not required to be heated in the reaction process, the tin disulfide with the vertical array structure can be prepared according to the requirements only under the condition of normal temperature, the energy consumption caused by high temperature is greatly reduced, and the method is green, environment-friendly and low in energy consumption.
(2) By utilizing the in-situ preparation method, the tin disulfide can be accurately constructed on a nano scale as required. After lithium contacts with tin disulfide, lithium ions are embedded between layers of tin disulfide, covalent bonds between layers of tin disulfide are damaged more easily, and tin disulfide with a vertical array structure can be grown only by using electron beam irradiation. The method has simple raw materials, is green and environment-friendly, is beneficial to fully exerting the various potential of the tin disulfide with the vertical array structure, expands a new method for preparing the tin disulfide with the vertical array structure, and widens a new way for energy conversion and storage research.
Drawings
FIG. 1 is a TEM image of a vertical array of Sn disulfide obtained in example 1 of the present invention.
Detailed Description
The method for preparing tin disulfide with a vertical array structure at normal temperature in situ according to the invention is further described in detail with reference to the attached figure 1 and specific examples in the specification.
Example 1
Pouring 10 mg of common layered tin disulfide into 10 ml of deionized water, and performing ultrasonic dispersion for 30 minutes;
cutting a common carbon film used in a transmission electron microscope by using a blade, dripping two drops of liquid dispersed by ultrasonic on the semi-carbon film by using a dropper, and naturally drying;
after scraping and rubbing the lithium metal by using a tungsten needle tip, mounting the tungsten needle tip and the semi-carbon film on an electric pole;
in a transmission electron microscope, a tungsten needle point with lithium metal is used for contacting the layered tin disulfide at the edge of the semi-carbon film, and a voltage of-0.1V is applied;
converging the electron beam to make the beam density of the electron beam reach 1.0 x 104A/m2The contacted sample was irradiated for 20 minutes.
The results are shown in FIG. 1: the tin disulfide changed from a layered structure to a vertical array structure with a lattice fringe spacing of 0.59nm in fig. 1, which is consistent with the tin disulfide 001 interplanar spacing. This shows that after the original layered tin disulfide is irradiated by electron beams, a large number of tin disulfide with a close and vertical arrangement structure is generated.
Example 2
Pouring 10 mg of common layered tin disulfide into 20 ml of deionized water, and performing ultrasonic dispersion for 30 minutes;
cutting a common carbon film used in a transmission electron microscope by using a blade, dripping two drops of liquid dispersed by ultrasonic on the semi-carbon film by using a dropper, and naturally drying;
after scraping and rubbing the lithium metal by using a tungsten needle tip, mounting the tungsten needle tip and the semi-carbon film on an electric pole;
in a transmission electron microscope, a tungsten needle point with lithium metal is used for contacting the layered tin disulfide at the edge of the semi-carbon film, and a voltage of-5V is applied;
converging the electron beam to make the beam density of the electron beam reach 5.0 x 104A/m2The contacted sample was irradiated for 10 minutes.
The results obtained are similar to those of example 1.
Example 3
Pouring 20 mg of common layered tin disulfide into 10 ml of deionized water, and performing ultrasonic dispersion for 10 minutes;
cutting a common carbon film used in a transmission electron microscope by using a blade, dripping two drops of liquid dispersed by ultrasonic on the semi-carbon film by using a dropper, and naturally drying;
after scraping and rubbing the lithium metal by using a tungsten needle tip, mounting the tungsten needle tip and the semi-carbon film on an electric pole;
in a transmission electron microscope, a tungsten needle point with lithium metal is used for contacting the layered tin disulfide at the edge of the semi-carbon film, and a voltage of-5V is applied;
converging electron beams to make the beam density of the electron beams reach 8.0 x 104A/m2The contacted sample was irradiated for 5 minutes.
The results obtained are similar to those of example 1.
Example 4
Pouring 20 mg of common layered tin disulfide into 10 ml of deionized water, and performing ultrasonic dispersion for 10 minutes;
cutting a common carbon film used in a transmission electron microscope by using a blade, dripping two drops of liquid dispersed by ultrasonic on the semi-carbon film by using a dropper, and naturally drying;
after scraping and rubbing the lithium metal by using a tungsten needle tip, mounting the tungsten needle tip and the semi-carbon film on an electric pole;
in a transmission electron microscope, a tungsten needle point with lithium metal is used for contacting the layered tin disulfide at the edge of the semi-carbon film, and a voltage of-0.1V is applied;
converging the electron beam to make the beam density of the electron beam reach 1.0 x 106A/m2The contacted sample was irradiated for 1 minute.
The results obtained are similar to those of example 1.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. The method for preparing the tin disulfide with the vertical array structure at the normal temperature in situ is characterized by comprising the following steps of: dispersing common layered tin disulfide on a semi-carbon film by ultrasonic, touching the tin disulfide with a tungsten needle tip scraped with lithium metal in a transmission electron microscope, and applying voltage; and converging the electron beams to irradiate the sample to obtain the tin disulfide with a vertical array structure.
2. The method for preparing the tin disulfide with the vertical array structure at normal temperature in situ according to claim 1, wherein the ultrasonic dispersion time is 10-30 minutes.
3. The method for preparing tin disulfide in a vertical array structure at normal temperature in situ according to claim 1, wherein the voltage is (-0.1 to-5) V.
4. The method for preparing tin disulfide with a vertical array structure at normal temperature in situ according to claim 1, wherein the beam current density range of the electron beam during irradiation is 1.0 x 104A/m2- 1.0×106A/ m2。
5. The method for preparing the tin disulfide with the vertical array structure at normal temperature in situ according to claim 1, wherein the irradiation time is 1-20 minutes.
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| CN202010129129.8A CN111268722B (en) | 2020-02-28 | 2020-02-28 | Method for preparing stannic disulfide with vertical array structure at normal temperature in situ |
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Citations (8)
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|---|---|---|---|---|
| CN1935631A (en) * | 2006-09-22 | 2007-03-28 | 北京大学 | Method for accurately cutting-connecting nano material and its use |
| CN103586590A (en) * | 2013-11-12 | 2014-02-19 | 温州大学 | Nanometer welding method based on joule heat |
| CN104998660A (en) * | 2015-06-11 | 2015-10-28 | 岭南师范学院 | Preparation method of stannic oxide nanocrystalline loaded tin disulfide nanosheet composite nanomaterial |
| US20160093491A1 (en) * | 2014-09-29 | 2016-03-31 | University Of North Texas | LARGE SCALE AND THICKNESS-MODULATED MoS2 NANOSHEETS |
| CN105899359A (en) * | 2013-02-27 | 2016-08-24 | 3M创新有限公司 | Lamination transfer films for forming embedded nanostructures |
| CN105916674A (en) * | 2014-01-20 | 2016-08-31 | 3M创新有限公司 | Lamination transfer films for forming reentrant structures |
| CN105977135A (en) * | 2016-05-19 | 2016-09-28 | 西安电子科技大学 | Gallium nitride growth method based on tin disulfide and magnetron sputtering aluminium nitride |
| CN106744675A (en) * | 2017-01-22 | 2017-05-31 | 郑州大学 | A kind of nano material cutting off processing method |
-
2020
- 2020-02-28 CN CN202010129129.8A patent/CN111268722B/en active Active
Patent Citations (8)
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|---|---|---|---|---|
| CN1935631A (en) * | 2006-09-22 | 2007-03-28 | 北京大学 | Method for accurately cutting-connecting nano material and its use |
| CN105899359A (en) * | 2013-02-27 | 2016-08-24 | 3M创新有限公司 | Lamination transfer films for forming embedded nanostructures |
| CN103586590A (en) * | 2013-11-12 | 2014-02-19 | 温州大学 | Nanometer welding method based on joule heat |
| CN105916674A (en) * | 2014-01-20 | 2016-08-31 | 3M创新有限公司 | Lamination transfer films for forming reentrant structures |
| US20160093491A1 (en) * | 2014-09-29 | 2016-03-31 | University Of North Texas | LARGE SCALE AND THICKNESS-MODULATED MoS2 NANOSHEETS |
| CN104998660A (en) * | 2015-06-11 | 2015-10-28 | 岭南师范学院 | Preparation method of stannic oxide nanocrystalline loaded tin disulfide nanosheet composite nanomaterial |
| CN105977135A (en) * | 2016-05-19 | 2016-09-28 | 西安电子科技大学 | Gallium nitride growth method based on tin disulfide and magnetron sputtering aluminium nitride |
| CN106744675A (en) * | 2017-01-22 | 2017-05-31 | 郑州大学 | A kind of nano material cutting off processing method |
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