CN106219596B - A kind of synthetic method of the SnS crystal with letter C shape - Google Patents
A kind of synthetic method of the SnS crystal with letter C shape Download PDFInfo
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- CN106219596B CN106219596B CN201610568208.2A CN201610568208A CN106219596B CN 106219596 B CN106219596 B CN 106219596B CN 201610568208 A CN201610568208 A CN 201610568208A CN 106219596 B CN106219596 B CN 106219596B
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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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- 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
- C01P2002/72—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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- 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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The invention discloses a kind of synthetic method of the SnS crystal with letter C shape, comprise the following steps：Step 1: by stanniferous presoma, sulfur-bearing presoma and surfactant obtained solution soluble in water, described surfactant is polypyrrole alkanone；Step 2: obtained solution in step 1 to be transferred in reactor and heat, after reaction completely, centrifugation, with water and ethanol wash sample, the SnS crystal with letter C shape is made.The advantage of the invention is that：Technique is simple, and production cost is low, and the obtained SnS crystal morphologies with letter C shape are homogeneous, suitable for directly preparing electrode material of lithium battery and solar cell, and easily carry out popularization and application.
Description
Technical field
The present invention relates to technical field of nano material, a kind of especially synthesis side of the SnS crystal with letter C shape
Method.
Background technology
SnS is due to the energy gap near ideal, Sn the and S reserves enriched in addition on the earth, has cheap, high
Effect, nontoxic three big feature, turn into the preferred material of solar energy conversion.
It is one of most important study frontier in material science to prepare ultra-thin semiconductor nano piece using solwution method, domestic
Substantial amounts of research has been carried out to this outside.But the method used at present is mostly oil phase method, so generally requiring to use much has
The organic solvent of poison.Hydro-thermal method, as a kind of method using water as reaction medium, applied to a variety of inorganic semiconductor nanometers of synthesis
Material, so far, many SnS Nano/microns crystal with special appearance structure have all been synthesized by domestic and international scientist
Out, but still without document on the report with letter C shape SnS crystal.
The content of the invention
It is simple the technical problem to be solved by the invention for the present situation of prior art is to provide technique, prepare convenient, peace
Entirely, the synthetic method of a kind of SnS crystal with letter C shape easy to utilize.
Technical scheme is used by the present invention solves above-mentioned technical problem：
A kind of synthetic method of the SnS crystal with letter C shape, comprises the following steps：
Step 1: by stanniferous presoma, sulfur-bearing presoma and surfactant obtained solution soluble in water, described surface
Activating agent is polypyrrole alkanone；
Step 2: obtained solution in step 1 to be transferred in reactor and heat, after reaction completely, centrifugation, water is used
With ethanol wash sample, the SnS crystal with letter C shape is made.
The technical measures of optimization also include：
In above-mentioned step one, stanniferous presoma is stannous chloride, butter of tin or stannous sulfate.
In above-mentioned step one, sulfur-bearing presoma is thiocarbamide, thioacetamide, vulcanized sodium, cysteine or reduction paddy Guang
Sweet peptide.
In above-mentioned step one, the mol ratio of stanniferous presoma and sulfur-bearing presoma is 1：1 to 1：12.
In above-mentioned step one, the mol ratio of stanniferous presoma and surfactant is 1：0.1 to 1：2.
In above-mentioned step two, reaction temperature is 150 DEG C to 220 DEG C.
In above-mentioned step two, the reaction time is 1h to 18h.
A kind of synthetic method of the SnS crystal with letter C shape of the present invention, technique is simple, and production cost is low, obtained
The SnS crystal morphologies with letter C shape it is homogeneous, suitable for directly preparing electrode material of lithium battery and solar cell, and hold
Easily carry out popularization and application.
Brief description of the drawings
Fig. 1 is the electron-microscope scanning figure for the SnS crystal that the present invention has letter C shape；
Fig. 2 is the energy spectrum diagram for the SnS crystal that the present invention has letter C shape；
Fig. 3 is the XRD for the SnS crystal that the present invention has letter C shape.
Embodiment
The present invention is described in further detail below in conjunction with accompanying drawing embodiment.
A kind of synthetic method of the SnS crystal with letter C shape, comprises the following steps：
Step 1: by stanniferous presoma, sulfur-bearing presoma and surfactant obtained solution soluble in water, described surface
Activating agent is polypyrrole alkanone (PVP)；
Step 2: obtained solution in step 1 to be transferred in reactor and heat, after reaction completely, centrifugation, water is used
With ethanol wash sample, the SnS crystal with letter C shape is made.
Wherein, in step 1, stanniferous presoma is stannous chloride, butter of tin or stannous sulfate；Sulfur-bearing presoma is sulphur
Urea, thioacetamide, vulcanized sodium, cysteine or reduced glutathione.
The mol ratio of stanniferous presoma and sulfur-bearing presoma is 1：1 to 1：12；Stanniferous presoma and surfactant rub
You are than being 1：0.1 to 1：2.
In step 2, reaction temperature is 150 DEG C to 220 DEG C；Reaction time is 1h to 18h.
Obtained material obtains energy spectrum diagram as shown in Figure 2 through analysis, and the material that can confirm to obtain from energy spectrum diagram is
SnS；Appearance structure figure as shown in Figure 1 is obtained by ESEM scanning, is clear that obtained SnS is brilliant from the figure
The letter-c-shaped shape of body, sample obtain the XRD of sample as shown in Figure 3 by X-ray diffraction analysis.
Embodiment one
Step 1: 1mmol stannous chloride, 1mmol thioacetamides, 0.1 mmol polypyrroles alkanone (PVP) are dissolved in
Obtained solution in 80ml water；
Step 2: by the solution prepared in step 1 and being transferred to reactor heating, controlling reaction temperature is 150 DEG C, instead
After answering 1h, centrifugation, sample is washed with water and alcohol, the SnS crystal with letter C shape is made.
Embodiment two
Step 1: 1mmol butters of tin, 10mmol cysteines, 0.5mmol polypyrroles alkanone (PVP) are dissolved in 80ml
Obtained solution in water；
Step 2: by the solution prepared in step 1 and being transferred to reactor heating, controlling reaction temperature is 180 DEG C, instead
After answering 6h, centrifugation, sample is washed with water and alcohol, the SnS crystal with letter C shape is made.
Embodiment three
Step 2: by 1mmol stannous sulfates, 5mmol thiocarbamides, 1mmol polypyrroles alkanone (PVP), which is dissolved in 80ml water, to be made
Obtain solution；
Step 3: by the solution prepared in step 1 and being transferred to reactor heating, controlling reaction temperature is 200 DEG C, instead
After answering 10h, centrifugation, sample is washed with water and alcohol, the SnS crystal with letter C shape is made.
Example IV
Step 1: 1mmol stannous chloride, 5mmol reduced glutathiones, 1.5mmol polypyrroles alkanone (PVP) are dissolved in
Obtained solution in 80ml water；
Step 2: by the solution prepared in step 1 and being transferred to reactor heating, controlling reaction temperature is 220 DEG C, instead
After answering 15h, centrifugation, sample is washed with water and alcohol, the SnS crystal with letter C shape is made.
Embodiment five
Step 1: by 1mmol butters of tin, 12mmol cysteines and 2mmol polypyrroles alkanone (PVP) are dissolved in 80ml water
Middle obtained solution；
Step 2: by the solution prepared in step 1 and being transferred to reactor heating, controlling reaction temperature is 220 DEG C, instead
After answering 18h, centrifugation, sample is washed with water and alcohol, the SnS crystal with letter C shape is made.
Highly preferred embodiment of the present invention has illustrated, and the various change or remodeling made by those of ordinary skill in the art are not
It can depart from the scope of the present invention.
Claims (1)
1. a kind of synthetic method of the SnS crystal with letter C shape, it is characterized in that：Comprise the following steps：
Step 1: by 1mmol stannous chloride, 5mmol reduced glutathiones, 1.5mmol polypyrrole alkanones, which are dissolved in 80ml water, to be made
Obtain solution；
Step 2: the solution prepared in step 1 is transferred into reactor heating, controlling reaction temperature is 220 DEG C, reacts 15h
Afterwards, centrifuge, sample is washed with water and alcohol, the SnS crystal with letter C shape is made；
The material that can confirm to obtain in the energy spectrum diagram that obtained material obtains through analysis is SnS；Scanned and obtained by ESEM
Appearance structure figure in can be clearly apparent the obtained letter-c-shaped shape of SnS crystal.
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| CN201610568208.2A CN106219596B (en) | 2016-07-19 | 2016-07-19 | A kind of synthetic method of the SnS crystal with letter C shape |
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| CN201610568208.2A CN106219596B (en) | 2016-07-19 | 2016-07-19 | A kind of synthetic method of the SnS crystal with letter C shape |
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| CN106219596A CN106219596A (en) | 2016-12-14 |
| CN106219596B true CN106219596B (en) | 2018-01-16 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107522223B (en) * | 2017-09-07 | 2019-12-31 | 昆明鼎邦科技股份有限公司 | Preparation method of stannous sulfide |
| CN108545769A (en) * | 2018-04-26 | 2018-09-18 | 南京邮电大学 | A kind of SnS nanocrystals and its preparation method and application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103588241A (en) * | 2013-11-25 | 2014-02-19 | 湛江师范学院 | Preparation method for synthetizing three-dimensional stannous sulfide micro-flowers through complexing agent with aid of quaternary ammonium salt |
| CN103915625A (en) * | 2014-04-09 | 2014-07-09 | 暨南大学 | Preparation method and application of spherical tin sulfide consisting of nanorods |
| CN104108747A (en) * | 2013-04-19 | 2014-10-22 | 李孝凤 | Method for synthesizing SnS powder by utilizing high-pressure solvothermal |
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- 2016-07-19 CN CN201610568208.2A patent/CN106219596B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104108747A (en) * | 2013-04-19 | 2014-10-22 | 李孝凤 | Method for synthesizing SnS powder by utilizing high-pressure solvothermal |
| CN103588241A (en) * | 2013-11-25 | 2014-02-19 | 湛江师范学院 | Preparation method for synthetizing three-dimensional stannous sulfide micro-flowers through complexing agent with aid of quaternary ammonium salt |
| CN103915625A (en) * | 2014-04-09 | 2014-07-09 | 暨南大学 | Preparation method and application of spherical tin sulfide consisting of nanorods |
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