CN108147376B - Method for synthesizing tin selenide powder at room temperature - Google Patents
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- MFIWAIVSOUGHLI-UHFFFAOYSA-N selenium;tin Chemical compound [Sn]=[Se] MFIWAIVSOUGHLI-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 239000000843 powder Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 23
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 88
- 239000012153 distilled water Substances 0.000 claims abstract description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 45
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 39
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 39
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000011975 tartaric acid Substances 0.000 claims abstract description 27
- 235000002906 tartaric acid Nutrition 0.000 claims abstract description 23
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 17
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 58
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 53
- 229910018162 SeO2 Inorganic materials 0.000 claims description 29
- 238000001035 drying Methods 0.000 claims description 24
- JPJALAQPGMAKDF-UHFFFAOYSA-N selenium dioxide Chemical compound O=[Se]=O JPJALAQPGMAKDF-UHFFFAOYSA-N 0.000 abstract description 20
- 238000001556 precipitation Methods 0.000 abstract description 2
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 description 16
- 238000001816 cooling Methods 0.000 description 15
- 239000000126 substance Substances 0.000 description 12
- 235000011150 stannous chloride Nutrition 0.000 description 9
- 239000011669 selenium Substances 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 6
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000003638 chemical reducing agent Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910052711 selenium Inorganic materials 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000012876 topography Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 231100000086 high toxicity Toxicity 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000004729 solvothermal method Methods 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- -1 stannum selenide Chemical class 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
A precipitation method for synthesizing tin selenide powder at room temperature is characterized in that tartaric acid, EDTA or citric acid are dissolved in distilled water, tin selenide is added and stirred to be dissolved to prepare a solution A, then selenium dioxide, sodium hydroxide and sodium borohydride are sequentially added into the distilled water to prepare a solution B, the solution A is slowly added into the solution B, the solution B is stirred for 10-20 minutes, a sample is centrifugally separated and collected, then the solution A is placed into an oven to be dried, and then the solution is naturally cooled to room temperature and dried to obtain black tin selenide powder.
Description
Technical Field
The invention relates to the technical field of room temperature synthesis of two-dimensional materials, in particular to a method for synthesizing tin selenide powder at room temperature.
Background
Tin selenide (SnSe) is a very important P-type semiconductor material having a two-dimensional layered structure, and the layers are connected by weak van der waals force. The stannum selenide has rich and nontoxic earth elements, stable chemical properties, narrow band gap (1.0-1.5eV) and excellent electronic and photoelectric properties. The range of potential applications of SnSe is very wide, as in photovoltaics (Li L, Chen Z, Hu Y, et al, Single-layer single-crystalline SnSe nanosheets [ J ]. Journal of the American Chemical Society,2013,135(4):1213-6.), thermoelectric (Feng D, Ge Z H, Wu D, et al. enhanced thermal properties of SnSe polycrystalline via texture control [ J ]. Physical Chemistry Chemical Physics,2016,18(46):31821.) and Energy storage (Yuan S, Zhu Y H, Li W, et al. surface-Free Aqueous Synthesis of Pure Single-Crystalline, SnSe nanoshiet Cluster as for High Energy and Power-Density Sodium-Ion Batteries [ J ]. Advanced Materials,2016,29(4).) aspects, memory switching devices, infrared light devices, solar cells, negative electrode Materials for lithium Batteries, and the like.
At present, the synthesis methods of tin selenide are many, mainly include a solvothermal method, a hydrothermal method and the like, some methods need special instruments in the preparation process, and some methods involve using hydrazine hydrate and other strong reducing agents with high toxicity to reduce a selenium source (SeO) in the synthesis process2)(Feng D,Ge Z H,Wu D,et al.Enhanced thermoelectric properties of SnSe polycrystals via texture control[J]Physical Chemistry Chemical Physics,2016,18(46):31821.) results in environmental pollution of the manufacturing process and adverse operator health; in addition, the solvothermal method, the hydrothermal method and other methods need to be heated to about 120-260 ℃, and a surfactant needs to be added, so that the process is complex and the time is long. In the existing technology for synthesizing SnSe at room temperature, Se powder is used as a selenium source, but the Se powder is not easy to dissolve and can be dissolved by means of NaOH dissolution and heat release to about 80 ℃. Therefore, the method for preparing the tin selenide material at room temperature has important significance.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a method for synthesizing tin selenide powder at room temperature, which adopts tin dichloride (SnCl)2) And selenium dioxide (SeO)2) The tin source and the selenium source are respectively adopted, the raw materials and the generated solution in the whole process are easy to process and have no pollution, the preparation cost is low, the operation process is simple, the repeatability is high, and the high-purity tin selenide powder can be quickly obtained through room-temperature precipitation.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for synthesizing tin selenide powder at room temperature comprises the following steps:
the method comprises the following steps: adding tartaric acid, citric acid or ethylenediamine tetraacetic acid into distilled water, stirring, and adding SnCl2Stirring until SnCl2Dissolving to obtain a solution A;
will be SeO2NaOH and NaBH4Adding into distilled water, and stirring to obtain transparent solution B;
step two: and adding the solution A into the transparent solution B, uniformly stirring, centrifugally separating, collecting a sample, and drying to obtain black tin selenide powder.
In a further development of the invention, the SnCl2Tartaric acid, SeO2NaOH and NaBH4The mass ratio of (1): (8-12): 1: (10-20): 2 or SnCl2Tartaric acid, SeO2NaOH and NaBH4The mass ratio of (2): (14-16): 1: 20: 2.
in a further development of the invention, the SnCl2Ethylenediaminetetraacetic acid, SeO2NaOH and NaBH4The mass ratio of (1): (6-8): 1: 20: 2 or SnCl2Ethylenediaminetetraacetic acid, SeO2NaOH and NaBH4The mass ratio of (2): 12: 1: 20: 2.
in a further development of the invention, the SnCl2Citric acid, SeO2NaOH and NaBH4The mass ratio of (1): (6-8): 1: 20: 2 or SnCl2Citric acid, SeO2NaOH and NaBH4The mass ratio of (2): 12: 1: 20: 2.
the invention further improves that in the solution A, the ratio of tartaric acid to distilled water is (1.2-2.4) g: 20mL, the ratio of citric acid to distilled water is (1.75-3.51) g: 20mL, the ratio of the ethylenediamine tetraacetic acid to the distilled water is (1.15-2.31) g: 20 mL.
A further development of the invention is that in solution B, NaBH is added4Ratio to distilled water 2 mmol: 15 mL.
The further improvement of the invention is that the drying temperature is 60-70 ℃ and the drying time is 1-5 hours.
Compared with the prior art, the invention has the beneficial effects that: SeO in the invention2Becomes SeO in the environment of strong base NaOH2 3-，NaBH4Added as a reducing agent to be further reduced into Se2-Ions thereby to Sn2+And carrying out ion reaction to further generate the tin selenide. The preparation method can realize the preparation of pure-phase tin selenide powder at room temperature, the required reagents and solvents are conventional chemicals, complex organic reagents are not required, the preparation method is non-toxic and harmless, a surfactant is not required to be added, the whole related technical process is convenient and simple to operate, the distilled water is used as the solvent for reaction, special instruments are not required in the preparation process, a strong reducing agent with high toxicity is not used for reducing a selenium source in the synthesis process, the preparation cost is low, no pollution is caused, heating is not required, the time of the whole experimental process is short, the tin selenide powder can be quickly obtained at room temperature, and the repeatability is high.
Drawings
Figure 1 is the XRD pattern of example 1.
FIG. 2 is an SEM photograph of example 1.
Figure 3 is the XRD pattern of example 2.
FIG. 4 is an SEM photograph of example 2.
Figure 5 is the XRD pattern of example 3.
FIG. 6 is an SEM photograph of example 3.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings.
In the invention, the mass of tartaric acid is about 1.2g to 2.4g, the mass of EDTA is about 1.75g to 3.51g, the mass of citric acid is about 1.15g to 2.31g, and the volume of distilled water is 20 mL.
SeO2Becomes SeO in the environment of strong base NaOH2 3-，NaBH4Added as a reducing agent to be further reduced into Se2-Ions thereby to Sn2+And carrying out ion reaction to further generate the tin selenide.
Example 1
2.4g of tartaric acid is weighed and dissolved in 20mL of distilled water, stirred until the tartaric acid is dissolved to obtain a clear and transparent solution, then 2mmol of tin dichloride is added, and stirred until the solution is clear and transparent to obtain a solution A.
Sequentially adding 1mmol of selenium dioxide, 0.8g of sodium hydroxide and 2mmol of sodium borohydride into 15mL of distilled water, and uniformly stirring to obtain a transparent solution B.
And slowly adding the solution A into the transparent solution B, stirring for 15 minutes at room temperature, centrifugally separating to collect a sample, then putting the sample into an oven for drying for 3 hours at 60 ℃, and naturally cooling to room temperature to obtain black tin selenide powder.
Figure 1 is the XRD pattern of the product, with no impurity peaks present, indicating that the product is pure tin selenide.
Fig. 2 is an SEM topography photograph of the product. As can be seen from fig. 2, SnSe is present as particulate agglomerates.
Example 2
2.34g of EDTA was dissolved in 20mL of distilled water, and after stirring to dissolve it, 1mmol of tin dichloride was added to prepare a solution A.
Sequentially adding 1mmol of selenium dioxide, 0.8g of sodium hydroxide and 2mmol of sodium borohydride into 15mL of distilled water, and uniformly stirring to obtain a transparent solution B.
And slowly adding the solution A into the transparent solution B, stirring for 15 minutes at room temperature, centrifugally separating to collect a sample, then putting the sample into an oven for drying for 3 hours at 65 ℃, and naturally cooling to room temperature to obtain black tin selenide powder.
Figure 3 is an XRD pattern of the product with no impurity peaks present, indicating that the product is pure tin selenide.
Fig. 4 is an SEM topography photograph of the product. As can be seen from fig. 4, lamellar SnSe was formed.
Example 3
Weighing 2.31g of citric acid, dissolving the citric acid in 20mL of distilled water, stirring until the citric acid is dissolved to obtain a clear and transparent solution, then adding 2mmol of tin dichloride, and stirring until the solution is clear and transparent to obtain a solution A.
Sequentially adding 1mmol of selenium dioxide, 0.8g of sodium hydroxide and 2mmol of sodium borohydride into 15mL of distilled water, and uniformly stirring to obtain a transparent solution B.
And slowly adding the solution A into the transparent solution B, stirring for 15 minutes at room temperature, centrifugally separating to collect a sample, then putting the sample into an oven for drying at 70 ℃ for 2 hours, and naturally cooling to room temperature to obtain black tin selenide powder.
Figure 5 is an XRD pattern of the product with no impurity peaks present, indicating that the product is pure tin selenide.
Fig. 6 is an SEM topography photograph of the product. As can be seen from fig. 6, SnSe is granular.
Example 4
Weighing 1.2g of tartaric acid, dissolving the tartaric acid in 20mL of distilled water, stirring the solution until the tartaric acid is dissolved to obtain a clear and transparent solution, then adding 1mmol of tin dichloride, and stirring the solution until the solution is clear and transparent to obtain a solution A.
Sequentially adding 1mmol of selenium dioxide, 0.8g of sodium hydroxide and 2mmol of sodium borohydride into 15mL of distilled water, and uniformly stirring to obtain a transparent solution B.
And slowly adding the solution A into the transparent solution B, stirring for 15 minutes at room temperature, centrifugally separating to collect a sample, then putting the sample into an oven for drying at 60 ℃ for 1 hour, and naturally cooling to room temperature to obtain black tin selenide powder.
Example 5
1.2g of tartaric acid is weighed and dissolved in 20mL of distilled water, stirred until dissolved, then 1mmol of tin dichloride is added, and stirred until the solution is clear and transparent, thus obtaining solution A.
And sequentially adding 1mmol of selenium dioxide, 0.4g of sodium hydroxide and 2mmol of sodium borohydride into 15mL of distilled water, and stirring to obtain a solution B.
Slowly pouring the solution A into the solution B, stirring for 15min at room temperature, centrifugally separating and collecting a sample, then putting the sample into an oven at 70 ℃ for drying for 2h, and naturally cooling to room temperature to obtain black tin selenide powder.
Example 6
Dissolving 1.8g of tartaric acid in 20mL of distilled water, stirring until the tartaric acid is dissolved, adding 1mmol of tin dichloride, and stirring until the solution is clear and transparent to obtain a solution A.
1mmol of selenium dioxide, 0.8g of sodium hydroxide and 2mmol of sodium borohydride are sequentially added into 15mL of distilled water and stirred to obtain a solution B.
Slowly pouring the A into the solution B, stirring for 15min at room temperature, centrifugally separating to collect a sample, then putting the sample into an oven for drying for 5h at 60 ℃, naturally cooling to room temperature, and drying to obtain black tin selenide powder.
Example 7
Dissolving 1.2g of tartaric acid in 20mL of distilled water, stirring until the tartaric acid is dissolved, adding 2mmol of tin dichloride, and stirring until the solution is clear and transparent to obtain a solution A.
1mmol of selenium dioxide, 0.8g of sodium hydroxide and 2mmol of sodium borohydride are sequentially added into 15mL of distilled water and stirred to obtain a solution B.
And slowly adding the solution A into the solution B, stirring for 15 minutes at room temperature, centrifugally separating to collect a sample, then putting the sample into an oven for drying for 3 hours at 65 ℃, naturally cooling to room temperature, and drying to obtain black tin selenide powder.
Example 8
Dissolving 2.4g of tartaric acid in 20mL of distilled water, stirring until the tartaric acid is dissolved, adding 2mmol of tin dichloride, and stirring until the solution is clear and transparent to obtain a solution A.
1mmol of selenium dioxide, 0.8g of sodium hydroxide and 2mmol of sodium borohydride are sequentially added into 15mL of distilled water and stirred to obtain a solution B.
And slowly adding the solution A into the solution B, stirring for 15 minutes at room temperature, centrifugally separating to collect a sample, then putting the sample into an oven for drying at 70 ℃ for 2 hours, naturally cooling to room temperature, and drying to obtain black tin selenide powder.
Example 9
Adding EDTA into distilled water, stirring, and adding SnCl2Stirring until SnCl2Dissolving to obtain a solution A; wherein, EDTA and SnCl2The mass ratio of (a) to (b) is 6: 1.
will be SeO2NaOH and NaBH4Adding into distilled water, and stirring to obtain transparent solution B; wherein, SnCl2、SeO2NaOH and NaBH4The ratio of the amounts of substances (1): 1: 20: 2.
and adding the solution A into the transparent solution B, stirring for 20 minutes, centrifugally separating and collecting a sample, drying at 65 ℃ for 3 hours, and naturally cooling to room temperature to obtain black tin selenide powder.
Example 10
Adding citric acid into distilled water, stirring uniformly, and then adding SnCl2Stirring until SnCl2Dissolving to obtain a solution A; wherein tartaric acid and SnCl2The mass ratio of (a) to (b) is 8: 1.
Will be SeO2NaOH and NaBH4Adding into distilled water, and stirring to obtain transparent solution B; wherein, SnCl2、SeO2NaOH and NaBH4The ratio of the amounts of substances (1): 1: 20: 2.
and adding the solution A into the transparent solution B, stirring for 10 minutes, centrifugally separating and collecting a sample, drying at 70 ℃ for 1 hour, and naturally cooling to room temperature to obtain black tin selenide powder.
Example 11
Adding tartaric acid intoStirring the mixture evenly in distilled water, and then adding SnCl2Stirring until SnCl2Dissolving to obtain a solution A; wherein tartaric acid and SnCl2The mass ratio of (a) to (b) is 14: 1.
will be SeO2NaOH and NaBH4Adding into distilled water, and stirring to obtain transparent solution B; wherein, SnCl2、SeO2NaOH and NaBH4The ratio of the amounts of substances (1): 1: 20: 2.
and adding the solution A into the transparent solution B, stirring for 20 minutes, centrifugally separating and collecting a sample, drying at 65 ℃ for 3 hours, and naturally cooling to room temperature to obtain black tin selenide powder.
Example 12
Adding EDTA into distilled water, stirring, and adding SnCl2Stirring until SnCl2Dissolving to obtain a solution A; wherein, EDTA and SnCl2The mass ratio of (a) to (b) is 8: 1.
will be SeO2NaOH and NaBH4Adding into distilled water, and stirring to obtain transparent solution B; wherein, SnCl2、SeO2NaOH and NaBH4The ratio of the amounts of substances (1): 1: 20: 2.
and adding the solution A into the transparent solution B, stirring for 20 minutes, centrifugally separating and collecting a sample, drying at 65 ℃ for 3 hours, and naturally cooling to room temperature to obtain black tin selenide powder.
Example 13
Adding EDTA into distilled water, stirring, and adding SnCl2Stirring until SnCl2Dissolving to obtain a solution A; wherein, EDTA and SnCl2The mass ratio of (a) to (b) is 6: 1.
will be SeO2NaOH and NaBH4Adding into distilled water, and stirring to obtain transparent solution B; wherein, SnCl2、SeO2NaOH and NaBH4The ratio of the amounts of substances of (a) to (b) is 2: 1: 20: 2.
and adding the solution A into the transparent solution B, stirring for 20 minutes, centrifugally separating and collecting a sample, drying at 65 ℃ for 3 hours, and naturally cooling to room temperature to obtain black tin selenide powder.
Example 14
Adding citric acid into distilled water, stirring uniformly, and then adding SnCl2Stirring until SnCl2Dissolving to obtain a solution A; wherein tartaric acid and SnCl2The mass ratio of (a) to (b) is 6: 1.
Will be SeO2NaOH and NaBH4Adding into distilled water, and stirring to obtain transparent solution B; wherein, SnCl2、SeO2NaOH and NaBH4The ratio of the amounts of substances (1): 1: 20: 2.
and adding the solution A into the transparent solution B, stirring for 10 minutes, centrifugally separating and collecting a sample, drying at 70 ℃ for 1 hour, and naturally cooling to room temperature to obtain black tin selenide powder.
Example 15
Adding citric acid into distilled water, stirring uniformly, and then adding SnCl2Stirring until SnCl2Dissolving to obtain a solution A; wherein tartaric acid and SnCl2The mass ratio of (a) to (b) is 6: 1.
Will be SeO2NaOH and NaBH4Adding into distilled water, and stirring to obtain transparent solution B; wherein, SnCl2、SeO2NaOH and NaBH4The ratio of the amounts of substances of (a) to (b) is 2: 1: 20: 2.
and adding the solution A into the transparent solution B, stirring for 10 minutes, centrifugally separating and collecting a sample, drying at 70 ℃ for 1 hour, and naturally cooling to room temperature to obtain black tin selenide powder.
Claims (3)
1. A method for synthesizing tin selenide powder at room temperature is characterized by comprising the following steps:
the method comprises the following steps: adding tartaric acid, citric acid or ethylenediamine tetraacetic acid into distilled water, stirring, and adding SnCl2Stirring until SnCl2Dissolving to obtain a solution A; in the solution A, the ratio of tartaric acid to distilled water is (1.2-2.4) g: 20mL, the ratio of citric acid to distilled water is (1.75-3.51) g: 20mL, the ratio of the ethylenediamine tetraacetic acid to the distilled water is (1.15-2.31) g: 20 mL;
will be SeO2NaOH and NaBH4Adding into distilled waterStirring to prepare a transparent solution B;
step two: adding the solution A into the transparent solution B, uniformly stirring, centrifugally separating, collecting a sample, and drying to obtain black tin selenide powder;
wherein, SnCl2Tartaric acid, SeO2NaOH and NaBH4The mass ratio of (1): (8-12): 1: (10-20): 2 or SnCl2Tartaric acid, SeO2NaOH and NaBH4The mass ratio of (2): (14-16): 1: 20: 2;
SnCl2ethylenediaminetetraacetic acid, SeO2NaOH and NaBH4The mass ratio of (1): (6-8): 1: 20: 2 or SnCl2Ethylenediaminetetraacetic acid, SeO2NaOH and NaBH4The mass ratio of (2): 12: 1: 20: 2;
SnCl2citric acid, SeO2NaOH and NaBH4The mass ratio of (1): (6-8): 1: 20: 2 or SnCl2Citric acid, SeO2NaOH and NaBH4The mass ratio of (2): 12: 1: 20: 2.
2. the method for synthesizing tin selenide powder at room temperature as claimed in claim 1, wherein in the solution B, NaBH is added4Ratio to distilled water 2 mmol: 15 mL.
3. The method for synthesizing tin selenide powder at room temperature as claimed in claim 1, wherein the drying temperature is 60-70 ℃ and the drying time is 1-5 hours.
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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 |
| CN102897724B (en) * | 2012-09-06 | 2014-08-20 | 江苏大学 | Tin selenide nano-flowers and preparation method thereof |
| KR101644053B1 (en) * | 2012-12-07 | 2016-08-01 | 삼성전자 주식회사 | Processes for synthesizing nanocrystals and nanocrystal compositions |
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