CN111268722B - Method for preparing stannic disulfide with vertical array structure at normal temperature in situ - Google Patents
Method for preparing stannic disulfide with vertical array structure at normal temperature in situ Download PDFInfo
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- CN111268722B CN111268722B CN202010129129.8A CN202010129129A CN111268722B CN 111268722 B CN111268722 B CN 111268722B CN 202010129129 A CN202010129129 A CN 202010129129A CN 111268722 B CN111268722 B CN 111268722B
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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 stannic 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 by using a tungsten needle tip for rubbing lithium metal in a transmission electron microscope, and applying voltage; and irradiating the sample by the convergent electron beam to obtain the tin disulfide with a vertical array structure. The method does not need to use 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 stannic 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 in order to ensure stable and continuous development of economy and science and technology under the big background of increasingly shortage of non-renewable resources, the full utilization of natural materials with large reserves and environmental friendliness to replace materials with limited reserves and serious pollution has become a great trend. In the transition metal sulfide, tin disulfide is an n-type semiconductor material with a band gap width of 2.2-2.5eV, each layer of Sn atoms is connected with S atoms through a strong Sn-S covalent bond, and the layers are connected through weak Van der Waals force. Sn is located in the octahedral center composed of six sulfur atoms. The method has the advantages of abundant reserves, low price, high photocatalysis efficiency, large energy storage capacity and the like, and has wide application prospect in the fields of photoelectric detection, solar cells, energy storage and the like. Tin disulfide with a vertical array morphology has great potential in energy conversion and storage due to the high density of more electrochemical reaction exposed edge sites.
The current methods for preparing transition metal sulfides with vertical array morphology mainly include hydrothermal method and CVD method. The main problem faced in preparing transition metal sulfide with vertical array morphology by adopting a hydrothermal method is that the hydrothermal reaction temperature is usually above 160 ℃, the raw materials are complex and the reaction time is long, and meanwhile, the prepared sample has serious agglomeration and poor dispersibility. The product obtained by the hydrothermal reaction is further cleaned to produce wastewater. The CVD process is too energy consuming, typically with reaction temperatures above 500 c, which results in significant energy consumption.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for preparing the stannic disulfide with the vertical array structure at normal temperature in situ. The method does not need to use high temperature and other toxic and harmful chemical reagents, thereby simplifying the process and reducing the production cost.
In order to achieve the above purpose, the invention is realized by the following technical scheme:
a method for preparing stannic 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 by using a tungsten needle tip for rubbing lithium metal in a transmission electron microscope, and applying voltage; and irradiating the sample by the convergent electron beam 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 electron beam current density at the time of irradiation is in the range of 1.0X10 4 A/m 2 - 1.0×10 6 A/ m 2 。
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 stannic disulfide reactant with the vertical array structure is complex and high in energy consumption, and the method uses few chemical reagents, so that samples are not required to be heated in the reaction process, and the stannic disulfide with the vertical array structure can be prepared according to requirements only under the condition of normal temperature, thereby greatly reducing the energy consumption caused by high temperature, being 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 is contacted with tin disulfide, lithium ions are inserted between tin disulfide layers, so that covalent bonds between the tin disulfide layers are more easily broken, and the tin disulfide with a vertical array structure can be grown only by using electron beam irradiation. The method has simple raw materials and environmental protection, is favorable for fully playing each potential of the stannic disulfide with the vertical array structure, expands a novel method for preparing the stannic disulfide with the vertical array structure, and expands a novel approach for energy conversion and storage research.
Drawings
FIG. 1 is a transmission electron microscopic view of tin disulfide of a vertical array structure obtained in example 1 of the present invention.
Detailed Description
The method for preparing the stannic disulfide with the vertical array structure at normal temperature in situ is further described in detail below with reference to the accompanying figure 1 and the specific embodiment.
Example 1
Pouring the common layered tin disulfide 10 mg into 10 ml 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 which are dispersed by ultrasonic on a semi-carbon film by using a dropper, and naturally airing;
after a tungsten needle point is scratched on lithium metal, the tungsten needle point and a semi-carbon film are arranged on an electric pole;
contacting layered tin disulfide at the edge of the semi-carbon film with a tungsten tip with lithium metal in a transmission electron microscope, and applying a voltage of-0.1V;
converging the electron beam to achieve a beam current density of 1.0X10 4 A/m 2 The contacted samples were irradiated for 20 minutes.
The results are shown in FIG. 1: the tin disulfide changed from a layered structure to a vertical array structure, and the lattice fringe spacing in fig. 1 was 0.59nm, which is consistent with the tin disulfide 001 interplanar spacing. This shows that the original layered tin disulfide is irradiated by electron beam to form a large piece of tin disulfide with a compact vertical arrangement structure.
Example 2
Pouring the common layered tin disulfide 10 mg into 20 ml 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 which are dispersed by ultrasonic on a semi-carbon film by using a dropper, and naturally airing;
after a tungsten needle point is scratched on lithium metal, the tungsten needle point and a semi-carbon film are arranged on an electric pole;
contacting layered tin disulfide at the edge of the semi-carbon film with a tungsten tip with lithium metal in a transmission electron microscope, and applying a voltage of-5V;
converging the electron beam to achieve a beam current density of 5.0X10 4 A/m 2 The contacted samples were irradiated for 10 minutes.
The results obtained were similar to those of example 1.
Example 3
Pouring the common layered tin disulfide 20 and mg into 10 and ml 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 which are dispersed by ultrasonic on a semi-carbon film by using a dropper, and naturally airing;
after a tungsten needle point is scratched on lithium metal, the tungsten needle point and a semi-carbon film are arranged on an electric pole;
contacting layered tin disulfide at the edge of the semi-carbon film with a tungsten tip with lithium metal in a transmission electron microscope, and applying a voltage of-5V;
converging the electron beam to achieve a beam current density of 8.0X10 4 A/m 2 The contacted samples were irradiated for 5 minutes.
The results obtained were similar to those of example 1.
Example 4
Pouring the common layered tin disulfide 20 and mg into 10 and ml 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 which are dispersed by ultrasonic on a semi-carbon film by using a dropper, and naturally airing;
after a tungsten needle point is scratched on lithium metal, the tungsten needle point and a semi-carbon film are arranged on an electric pole;
contacting layered tin disulfide at the edge of the semi-carbon film with a tungsten tip with lithium metal in a transmission electron microscope, and applying a voltage of-0.1V;
converging the electron beam to achieve a beam current density of 1.0X10 6 A/m 2 The contacted samples were irradiated for 1 minute.
The results obtained were similar to those of example 1.
While the foregoing is directed to embodiments of the present invention, other and further details of the invention may be had by the present invention, it should be understood that the foregoing description is merely illustrative of the present invention and that no limitations are intended to the scope of the invention, except insofar as modifications, equivalents, improvements or modifications are within the spirit and principles of the invention.
Claims (1)
1. The method for preparing the stannic disulfide with the vertical array structure at 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 by using a tungsten needle tip for rubbing lithium metal in a transmission electron microscope, and applying voltage; irradiating the sample by converging electron beams to obtain tin disulfide with a vertical array structure;
the ultrasonic dispersion time is 10-30 minutes;
the voltage is (-0.1 to-5) V;
the electron beam density range during irradiation is 1.0X10 4 A/m 2 -1.0×10 6 A/m 2 ；
The irradiation time is 1-20 minutes.
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Citations (7)
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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 |
| 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20160093491A1 (en) * | 2014-09-29 | 2016-03-31 | University Of North Texas | LARGE SCALE AND THICKNESS-MODULATED MoS2 NANOSHEETS |
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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 |
| 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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