CN106744727B - The preparation method of screw dislocation driving growth spiral type stratiform stannic selenide nanometer sheet - Google Patents
The preparation method of screw dislocation driving growth spiral type stratiform stannic selenide nanometer sheet Download PDFInfo
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- CN106744727B CN106744727B CN201611062238.2A CN201611062238A CN106744727B CN 106744727 B CN106744727 B CN 106744727B CN 201611062238 A CN201611062238 A CN 201611062238A CN 106744727 B CN106744727 B CN 106744727B
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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- 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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/22—Particle morphology extending in two dimensions, e.g. plate-like with a polygonal circumferential shape
Abstract
The invention discloses a kind of preparation methods of screw dislocation driving growth spiral type stratiform stannic selenide nanometer sheet, screw type stratiform stannic selenide nanometer sheet is prepared using the technology path of solvent method, stannic selenide nanometer sheet is controlled by controlling the concentration of precursor liquid and is driven with screw dislocation grows, this method is easy to operate, at low cost, and obtained screw type stratiform stannic selenide nanometer sheet has the helical periodicity of atomic-level thickness.
Description
Technical field
The present invention relates to stannic selenide nanometer sheet preparation field, especially a kind of screw dislocation drives growth spiral type stratiform selenium
Change the preparation method of tin nanometer sheet.
Background technique
The two-dimensional material of atomic-level thickness include graphene, boron nitride and transient metal sulfide etc. all show with
The different new features of its block materials, make its electronic device, in terms of there are good application prospects.So
And the controllable two-dimensional material such as exact growth thickness, size, structure, symmetry and ingredient still has important choose at present
War.The p-type semiconductor material for the narrow band gap that stannic selenide is abundant as a kind of storage, toxicity is low, chemical stability is good, in solar energy
There is good application prospect in battery, photodetector and near infrared light electric equipment.So far, by chemical method by selenizing
A series of stannic selenide nanostructures such as tin nanoflower, nanometer sheet and nano wire have all been synthesized；However, some unique
The screw type stratiform stannic selenide nanometer sheet of nanostructure such as atomic-level thickness is but seldom studied.
Summary of the invention
In order to solve the deficiencies in the prior art, the present invention for two-dimensional material thickness, size, structure, symmetry and at
Divide the status for being difficult to regulate and control, a kind of reliable effective, simple screw dislocation driving growth spiral type stratiform stannic selenide of regulation is provided
The preparation method of nanometer sheet.
In order to realize above-mentioned technical purpose, the technical solution of the present invention is as follows:
The preparation method of screw dislocation driving growth spiral type stratiform stannic selenide nanometer sheet comprising following steps:
1) stannous chloride that at room temperature, configuration concentration is 0.4~1.0mmol/L, concentration are 0.4~1.0mmol/
The selenium dioxide and concentration of L is the benzyl alcohol solution of the polyvinylpyrrolidone of 160~400g/L, and is uniformly mixed；
2) solution after mixing is transferred in three neck round bottom and is sealed and stirs, and be slowly introducing protection
Gas；
3) in protective gas atmosphere, solution is heated to 190~210 DEG C, and constant temperature keeps 12~18h；
4) by after solution cooled to room temperature, 8~12min of centrifugation, gained are carried out under the revolving speed of 900~1100rpm
It is centrifuged product and carries out washing filtering with dehydrated alcohol, and be stored in ethanol solution, obtain screw dislocation driving growth
Screw type stratiform stannic selenide nanometer sheet.
Further, the concentration of stannous chloride is 0.8mmol/L in the step 1), and the concentration of selenium dioxide is 0.8mmol/
L, the concentration of polyvinylpyrrolidone are 320g/L.
Further, stannous chloride, selenium dioxide and polyvinylpyrrolidone press 1mmol/L:1 in the step 1)
The ratio of mmol/L:400g/L is uniformly mixed.
Further, the protective gas of the step 2 and step 3) is nitrogen, helium or argon gas.
Further, for the step 3) in protective gas atmosphere, solution is heated to 200 DEG C.
Further, the driving of screw dislocation made from step 4) growth spiral type stratiform stannic selenide nanometer sheet has atom
The helical periodicity of grade thickness.
Further, the conveyor screw of screw dislocation driving growth spiral type stratiform stannic selenide nanometer sheet is by more than one
Rectangle stannic selenide nanometer sheet composition interconnected, the rectangle stannic selenide nanometer sheet area interconnected sequentially successively decrease.
By using above-mentioned technical solution, the invention has the benefit that being prepared using the technology path of solvent method
Screw type stratiform stannic selenide nanometer sheet controls stannic selenide nanometer sheet by controlling the concentration of precursor liquid with screw dislocation and drives life
Long, this method is easy to operate, at low cost, and obtained screw type stratiform stannic selenide nanometer sheet has the spiral week of atomic-level thickness
Phase property.
Detailed description of the invention
The present invention is further elaborated with reference to the accompanying drawings and detailed description:
Fig. 1 is the low power scanning electron microscope (SEM) photograph of screw type stratiform stannic selenide nanometer sheet of the present invention；
Fig. 2 is scanning electron microscope (SEM) photograph of the place (b) after magnification at high multiple in Fig. 1；
Fig. 3 is the atomic force microscope shape appearance figure of the place (b) screw type stratiform stannic selenide nanometer sheet in Fig. 1；
Fig. 4 is the cross sectional view in Fig. 3 at dotted line, and internal small figure is the structural representation of screw type stratiform stannic selenide nanometer sheet
Figure；
Fig. 5 is the X-ray diffractogram of screw type stratiform stannic selenide nanometer sheet of the present invention；
Fig. 6 is the transmission electron microscope picture of screw type stratiform stannic selenide nanometer sheet of the present invention；
Fig. 7 is tin element image corresponding in Fig. 6；
Fig. 8 is selenium element image corresponding in Fig. 6；
Fig. 9 is the electronic capability dispersion map of screw type stratiform stannic selenide nanometer sheet；
Figure 10 is the high resolution transmission electron microscope figure of screw type stratiform stannic selenide nanometer sheet；
Figure 11 is the electron diffraction diagram of screw type stratiform stannic selenide nanometer sheet；
Figure 12 is the transmission electron microscope picture at screw type stratiform stannic selenide nanometer sheet center in Fig. 6；
Figure 13 is the abosrption spectrogram of screw type stratiform stannic selenide nanometer sheet；
Figure 14 is the Raman spectrogram of screw type stratiform stannic selenide nanometer sheet.
Specific embodiment
The preparation method of screw dislocation driving growth spiral type stratiform stannic selenide nanometer sheet comprising following steps:
1) stannous chloride that at room temperature, configuration concentration is 0.4~1.0mmol/L, concentration are 0.4~1.0mmol/
The selenium dioxide and concentration of L is the benzyl alcohol solution of the polyvinylpyrrolidone of 160~400g/L, and is uniformly mixed；
2) solution after mixing is transferred in three neck round bottom and is sealed and stirs, and be slowly introducing protection
Gas；
3) in protective gas atmosphere, solution is heated to 190~210 DEG C, and constant temperature keeps 12~18h；
4) by after solution cooled to room temperature, 12~18min of centrifugation, gained are carried out under the revolving speed of 900~1100rpm
It is centrifuged product and carries out washing filtering with dehydrated alcohol, and be stored in ethanol solution, obtain screw dislocation driving growth
Screw type stratiform stannic selenide nanometer sheet.
Further, the concentration of stannous chloride is 0.8mmol/L in the step 1), and the concentration of selenium dioxide is 0.8mmol/
L, the concentration of polyvinylpyrrolidone are 320g/L.
Further, stannous chloride, selenium dioxide and polyvinylpyrrolidone press 1mmol/L:1 in the step 1)
The ratio of mmol/L:400g/L is uniformly mixed.
Further, the protective gas of the step 2 and step 3) is nitrogen, helium or argon gas.
Further, for the step 3) in protective gas atmosphere, solution is heated to 200 DEG C.
Further, the driving of screw dislocation made from step 4) growth spiral type stratiform stannic selenide nanometer sheet has atom
The helical periodicity of grade thickness.
Further, the conveyor screw of screw dislocation driving growth spiral type stratiform stannic selenide nanometer sheet is by more than one
Rectangle stannic selenide nanometer sheet composition interconnected, the rectangle stannic selenide nanometer sheet area interconnected sequentially successively decrease.
Embodiment 1
A kind of preparation method of screw dislocation driving growth spiral type stratiform stannic selenide nanometer sheet comprising following steps:
1) titanium dioxide that stannous chloride that at room temperature, configuration concentration is 0.8mmol/L, concentration are 0.8mmol/L
Selenium, the polyvinylpyrrolidone that concentration is 320g/L, ratio are the benzyl alcohol solution of 1mmol/L:1 mmol/L:400g/L, and
It is uniformly mixed；
2) solution after mixing is transferred in three neck round bottom and is sealed and stirs, and be slowly introducing nitrogen
Gas；
3) in nitrogen atmosphere, solution is heated to 200 DEG C, and constant temperature keeps 12h；
4) centrifugation 10min after solution cooled to room temperature, will be carried out under the revolving speed of 1000rpm, gained is centrifuged product
Washing filtering is carried out with dehydrated alcohol, and is stored in ethanol solution, the spiralization cycle with atomic-level thickness is obtained
Property screw dislocation drive growth spiral type stratiform stannic selenide nanometer sheet, the screw type of the described screw dislocation growth driving growth
The conveyor screw of stratiform stannic selenide nanometer sheet is made of more than one rectangle stannic selenide nanometer sheet interconnected, wherein being connected with each other
The area of rectangle stannic selenide nanometer sheet sequentially successively decrease.
Embodiment 2
A kind of preparation method of screw dislocation driving growth spiral type stratiform stannic selenide nanometer sheet comprising following steps:
1) titanium dioxide that stannous chloride that at room temperature, configuration concentration is 0.4mmol/L, concentration are 0.4mmol/L
Selenium, the polyvinylpyrrolidone that concentration is 160g/L, ratio are the benzyl alcohol solution of 1mmol/L:1 mmol/L:400g/L, and
It is uniformly mixed；
2) solution after mixing is transferred in three neck round bottom and is sealed and stirs, and be slowly introducing argon
Gas；
3) in argon atmosphere, solution is heated to 210 DEG C, and constant temperature keeps 18h；
4) centrifugation 12min after solution cooled to room temperature, will be carried out under the revolving speed of 900rpm, gained is centrifuged product and uses
Dehydrated alcohol carries out washing filtering, and is stored in ethanol solution, obtains the helical periodicity with atomic-level thickness
Screw dislocation drive growth spiral type stratiform stannic selenide nanometer sheet, the screw type layer of the described screw dislocation growth driving growth
The conveyor screw of shape stannic selenide nanometer sheet is made of more than one rectangle stannic selenide nanometer sheet interconnected, wherein interconnected
The area of rectangle stannic selenide nanometer sheet sequentially successively decreases.
Embodiment 3
A kind of preparation method of screw dislocation driving growth spiral type stratiform stannic selenide nanometer sheet comprising following steps:
1) titanium dioxide that stannous chloride that at room temperature, configuration concentration is 1.0mmol/L, concentration are 1.0mmol/L
Selenium, the polyvinylpyrrolidone that concentration is 400g/L, ratio are the benzyl alcohol solution of 1mmol/L:1 mmol/L:400g/L, and
It is uniformly mixed；
2) solution after mixing is transferred in three neck round bottom and is sealed and stirs, and be slowly introducing helium
Gas；
3) in helium atmosphere, solution is heated to 190 DEG C, and constant temperature keeps 16h；
4) centrifugation 8min after solution cooled to room temperature, will be carried out under the revolving speed of 1100rpm, gained is centrifuged product and uses
Dehydrated alcohol carries out washing filtering, and is stored in ethanol solution, obtains the helical periodicity with atomic-level thickness
Screw dislocation drive growth spiral type stratiform stannic selenide nanometer sheet, the screw type layer of the described screw dislocation growth driving growth
The conveyor screw of shape stannic selenide nanometer sheet is made of more than one rectangle stannic selenide nanometer sheet interconnected, wherein interconnected
The area of rectangle stannic selenide nanometer sheet sequentially successively decreases.
The above is the embodiment of the present invention, for the ordinary skill in the art, religion according to the present invention
Lead, without departing from the principles and spirit of the present invention all equivalent changes done according to scope of the present invention patent, repair
Change, replacement and variant, is all covered by the present invention.
Claims (6)
1. a kind of preparation method of screw dislocation driving growth spiral type stratiform stannic selenide nanometer sheet, it is characterised in that: it includes
Following steps:
1) stannous chloride that at room temperature, configuration concentration is 0.4~1.0mmol/L, concentration are 0.4~1.0mmol/L's
The benzyl alcohol solution for the polyvinylpyrrolidone that selenium dioxide and concentration are 160~400g/L, and be uniformly mixed；
2) solution after mixing is transferred in three neck round bottom and is sealed and stirs, and be slowly introducing protection gas
Body；
3) in protective gas atmosphere, solution is heated to 190~210 DEG C, and constant temperature keeps 12~18h；
4) 8~12min of centrifugation, gained centrifugation after solution cooled to room temperature, will be carried out under the revolving speed of 900~1100rpm
Product carries out washing filtering with dehydrated alcohol, and is stored in ethanol solution, obtains screw dislocation driving growth spiral
Type stratiform stannic selenide nanometer sheet, the conveyor screw of the screw dislocation driving growth spiral type stratiform stannic selenide nanometer sheet is by one
The above rectangle stannic selenide nanometer sheet composition interconnected, the rectangle stannic selenide nanometer sheet area interconnected are sequentially passed
Subtract.
2. a kind of preparation side of screw dislocation driving growth spiral type stratiform stannic selenide nanometer sheet according to claim 1
Method, it is characterised in that: the concentration of stannous chloride is 0.8mmol/L in the step 1), and the concentration of selenium dioxide is 0.8mmol/
L, the concentration of polyvinylpyrrolidone are 320g/L.
3. a kind of preparation side of screw dislocation driving growth spiral type stratiform stannic selenide nanometer sheet according to claim 1
Method, it is characterised in that: stannous chloride, selenium dioxide and polyvinylpyrrolidone are by concentration ratio in the step 1)
The ratio of 1mmol/L:1 mmol/L:400g/L is uniformly mixed with benzyl alcohol solution.
4. a kind of preparation side of screw dislocation driving growth spiral type stratiform stannic selenide nanometer sheet according to claim 1
Method, it is characterised in that: the protective gas of the step 2 and step 3) is nitrogen, helium or argon gas.
5. a kind of preparation side of screw dislocation driving growth spiral type stratiform stannic selenide nanometer sheet according to claim 1
Method, it is characterised in that: for the step 3) in protective gas atmosphere, solution is heated to 200 DEG C.
6. a kind of preparation side of screw dislocation driving growth spiral type stratiform stannic selenide nanometer sheet according to claim 1
Method, it is characterised in that: screw dislocation made from the step 4) drives growth spiral type stratiform stannic selenide nanometer sheet to have atom
The helical periodicity of grade thickness.
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| CN110240126B (en) * | 2019-06-14 | 2021-01-19 | 西安交通大学 | Tin diselenide with nanoflower structure and preparation method thereof |
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| CN101412505B (en) * | 2008-09-05 | 2010-06-02 | 山东建筑大学 | Preparation of high-purity tin diselenide nano-plate |
| CN102603202A (en) * | 2012-03-12 | 2012-07-25 | 山东建筑大学 | Method for preparing tin selenide photoelectric thin film |
| CN102897724B (en) * | 2012-09-06 | 2014-08-20 | 江苏大学 | Tin selenide nano-flowers and preparation method thereof |
| CN104692343B (en) * | 2015-03-17 | 2017-01-25 | 福州大学 | Tin selenide nano material, preparation method and application thereof |
| CN104831362A (en) * | 2015-06-08 | 2015-08-12 | 广东工业大学 | Method for preparing tin selenide single-crystal nano-belt |
| CN105565284B (en) * | 2016-03-04 | 2018-01-16 | 山东科技大学 | A kind of orientationization sheet SnSe raw powder's production technologies |
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