CN102502793B - Preparation method of rod-shaped SnS nanocrystals - Google Patents
Preparation method of rod-shaped SnS nanocrystals Download PDFInfo
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- CN102502793B CN102502793B CN201110375888.3A CN201110375888A CN102502793B CN 102502793 B CN102502793 B CN 102502793B CN 201110375888 A CN201110375888 A CN 201110375888A CN 102502793 B CN102502793 B CN 102502793B
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Abstract
The invention relates to a preparation method of rod-shaped SnS nanocrystals. The preparation method comprises the steps of: dissolving SnCl2 2H2O with ethylene glycol to obtain a solution A; adding a (NH4)2S solution to ethylene glycol to obtain a solution B; adding the solution A to the solution B, and stirring with a magnetic stirrer to form a precursor solution C; pouring the solution C to a hydrothermal reaction kettle, reacting under a temperature controlled mode, and naturally cooling to room temperature; and opening the hydrothermal reaction kettle, centrifuging and collecting the product, then respectively washing with deionized water and isopropanol, and then drying in a vacuum drying oven to obtain the final product rod-shaped SnS nanocrystals. According to the invention, SnS nanocrystals with uniform particle size are quickly prepared by adopting a microwave solvothermal method, the reaction is finished in the liquid phase at one time, post-treatment is not needed, the process equipment is simple and the reaction period is short.
Description
Technical field
The present invention relates to a kind of preparation method of SnS nano-powder, be specifically related to the nanocrystalline method of the bar-shaped SnS of a kind of microwave solvent hot preparation.
Background technology
SnSShiIV～VI family has the semiconductor material of stratiform orthorhombic crystalline structure, and its spacer is
lattice parameter is: a=0.4329nm, b=1.1193nm, c=0.3984nm.SnS is p-type under normal conditions, and when Sn is imbued with, its conduction type will transfer N-shaped to by p-type.Its optics direct band gap and indirect band gap are respectively 1.3～1.5eV and 1.0～1.1eV, there is good Spectral matching with the visible ray in solar radiation, photoelectric transformation efficiency reaches 25%, be suitable as very much the light absorbing zone in solar cell, also can be used as near infrared detector and the photovoltage equipment of electroluminescent display.Form in addition Sn element and the S element earth rich content of SnS, and nontoxic, therefore, SnS, as a kind of novel photoelectric transition material with nontoxic, the environmental protection of potential application foreground, has been subject to gradually in recent years people and has greatly paid close attention to.
The method of preparing at present SnS split has hydrothermal synthesis method [Rao.M.H, Jayalakshmi.M, Reddy.R.S.Chemistry Letters, 8 (2004) 1044-1045.], TGA assisting alcohol-hydrothermal method [Zhu H L, Yang D R, Zhang H.Mater.Lett., 60 (2006), 2686-2689.], microwave assisting method [Chen D, Shen G, Tang K, et al.J.Cryst.Growth, 260 (2004) 469-474.], ultrasonic liquid-phase auxiliary law [Li H S, Lei TM, Feng Q, et al.J.Synth.Cryst., 34,200519-322.] etc.These methods or complex process, or apparatus expensive, or the shortcoming such as poor repeatability, and product occurs that reunion situation is serious, the phenomenon such as pattern is inhomogeneous, affects the photoelectric properties of SnS.
Summary of the invention
The object of the invention is to provide a kind of equipment simple, easy handling, preparation time is short, the nanocrystalline method of the bar-shaped SnS of employing microwave solvent hot preparation that cost is low, by preparation method of the present invention, can prepare the rod-shaped powder that particle diameter of nanometer powder is 100～300nm, be uniformly dispersed and purity higher.
For achieving the above object, the technical solution used in the present invention is:
1) by analytically pure SnCl
22H
2o spent glycol dissolves makes Sn
2+concentration is the clear solution A of 0.01mol/L～1.0mol/L;
2) by analytically pure (NH
4)
2s solution spent glycol is mixed with S
2-concentration is the solution B of 0.01mol/L～2.0mol/L;
3) A solution is joined in B solution and form precursor solution C by magnetic stirrer;
Sn wherein
2+: S
2-mol ratio be 1: 2～10: 1;
4) solution C is poured in hydrothermal reaction kettle, compactedness is controlled at 40%～60%; Sealing hydrothermal reaction kettle, puts it in warm-pressing double-control microwave hydrothermal reaction; Select temperature controlling mode to react, temperature is controlled at 100 ℃～150 ℃, and pressure is less than 3.0MPa, after reaction 10min～120min, naturally cools to room temperature;
5) open hydrothermal reaction kettle, product, by centrifugal collection, then adopts respectively deionized water and washed with isopropyl alcohol 1～3 time, then it is dry at 40 ℃～70 ℃ to be placed in vacuum drying oven, obtains the bar-shaped SnS nanocrystal of final product.
Described analytically pure (NH
4)
2the S of S solution
2-concentration>=8%.
The present invention adopts the hot method of microwave solvent, prepares fast even particle size SnS nanocrystal, because reaction once completes in liquid phase, do not need post-processed, and processing unit is simple, and reaction time is short.
Accompanying drawing explanation
Fig. 1 is nanocrystalline X-ray diffraction (XRD) collection of illustrative plates of the prepared bar-shaped SnS of the embodiment of the present invention 1;
Fig. 2 is the nanocrystalline TEM photo of the prepared bar-shaped SnS of the embodiment of the present invention 1.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Embodiment 1:
1) by analytically pure SnCl
22H
2o spent glycol dissolves makes Sn
2+concentration is the clear solution A of 0.05mol/L;
2) by analytically pure (NH
4)
2s solution spent glycol is mixed with S
2-concentration is the solution B of 0.1mol/L;
3) A solution is joined in B solution and form precursor solution C, wherein Sn by magnetic stirrer
2+: S
2-mol ratio be 1: 2;
4) solution C is poured in hydrothermal reaction kettle, compactedness is controlled at 50%; Sealing hydrothermal reaction kettle, puts it in warm-pressing double-control microwave hydrothermal reaction; Select temperature controlling mode to react, temperature is controlled at 100 ℃, and pressure is 2.0MPa, after reaction 60min, naturally cools to room temperature;
5) open hydrothermal reaction kettle, product, by centrifugal collection, then adopts respectively deionized water and washed with isopropyl alcohol 1～3 time, is placed in vacuum drying oven dry at 40 ℃, the bar-shaped SnS nanocrystal of final product.
The bar-shaped SnS nanocrystal of gained is analyzed with Rigaku D/max2000PC x-ray diffractometer, discovery product is rhombic form (Fig. 1), at 2 θ, it is 31.519 °, 31.880 °, 30.460 °, 27.440 ° of growth characteristics respectively with (111), (400), (011), (210) crystal face.The TEM-3010 of sample Yong Yong Jeol Ltd. (JEOL) type transmission electron microscope is observed to (Fig. 2), from photo, can find out that prepared SnS nano crystal particles is approximately 200～500nm.
Embodiment 2:
1) by analytically pure SnCl
22H
2o spent glycol dissolves makes Sn
2+concentration is the clear solution A of 0.5mol/L;
2) by analytically pure (NH
4)
2s solution spent glycol is mixed with S
2-concentration is the solution B of 0.5mol/L;
3) A solution is joined in B solution and form precursor solution C, wherein Sn by magnetic stirrer
2+: S
2-mol ratio be 1: 1;
4) solution C is poured in hydrothermal reaction kettle, compactedness is controlled at 60%; Sealing hydrothermal reaction kettle, puts it in warm-pressing double-control microwave hydrothermal reaction; Select temperature controlling mode to react, temperature is controlled at 120 ℃, and pressure is less than 3.0MPa, after reaction 50min, naturally cools to room temperature;
5) open hydrothermal reaction kettle, product, by centrifugal collection, then adopts respectively deionized water and washed with isopropyl alcohol 1～3 time, is placed in vacuum drying oven dry at 40 ℃, the bar-shaped SnS nanocrystal of final product.
Embodiment 3:
1) by analytically pure SnCl
22H
2o spent glycol dissolves makes Sn
2+concentration is the clear solution A of 0.2mol/L;
2) by analytically pure (NH
4)
2s solution spent glycol is mixed with S
2-concentration is the solution B of 1.2mol/L;
3) A solution is joined in B solution and form precursor solution C, wherein Sn by magnetic stirrer
2+: S
2-mol ratio be 1: 6;
4) solution C is poured in hydrothermal reaction kettle, compactedness is controlled at 50%; Sealing hydrothermal reaction kettle, puts it in warm-pressing double-control microwave hydrothermal reaction; Select temperature controlling mode to react, temperature is controlled at 140 ℃, and pressure is less than 3.0MPa, after reaction 40min, naturally cools to room temperature;
5) open hydrothermal reaction kettle, product, by centrifugal collection, then adopts respectively deionized water and washed with isopropyl alcohol 1～3 time, is placed in vacuum drying oven dry at 40 ℃, the bar-shaped SnS nanocrystal of final product.
Embodiment 4:
1) by analytically pure SnCl
22H
2o spent glycol dissolves makes Sn
2+concentration is the clear solution A of 0.5mol/L;
2) by analytically pure (NH
4)
2s solution spent glycol is mixed with S
2-concentration is the solution B of 2.0mol/L;
3) A solution is joined in B solution and form precursor solution C, wherein Sn by magnetic stirrer
2+: S
2-mol ratio be 1: 4;
4) solution C is poured in hydrothermal reaction kettle, compactedness is controlled at 40%; Sealing hydrothermal reaction kettle, puts it in warm-pressing double-control microwave hydrothermal reaction; Select temperature controlling mode to react, temperature is controlled at 150 ℃, and pressure is less than 3.0MPa, after reaction 10min, naturally cools to room temperature;
5) open hydrothermal reaction kettle, product, by centrifugal collection, then adopts respectively deionized water and washed with isopropyl alcohol 1～3 time, is placed in vacuum drying oven dry at 50 ℃, the bar-shaped SnS nanocrystal of final product.
Embodiment 5:
1) by analytically pure SnCl
22H
2o spent glycol dissolves makes Sn
2+concentration is the clear solution A of 1.0mol/L;
2) by analytically pure (NH
4)
2s solution spent glycol is mixed with S
2-concentration is the solution B of 0.01mol/L;
3) A solution is joined in B solution and form precursor solution C, wherein Sn by magnetic stirrer
2+: S
2-mol ratio be 10: 1
4) solution C is poured in hydrothermal reaction kettle, compactedness is controlled at 55%; Sealing hydrothermal reaction kettle, puts it in warm-pressing double-control microwave hydrothermal reaction; Select temperature controlling mode to react, temperature is controlled at 110 ℃, and pressure is less than 3.0MPa, after reaction 120min, naturally cools to room temperature;
5) open hydrothermal reaction kettle, product, by centrifugal collection, then adopts respectively deionized water and washed with isopropyl alcohol 1～3 time, is placed in vacuum drying oven dry at 70 ℃, the bar-shaped SnS nanocrystal of final product.
Embodiment 6:
1) by analytically pure SnCl
22H
2o spent glycol dissolves makes Sn
2+concentration is the clear solution A of 0.01mol/L;
2) by analytically pure (NH
4)
2s solution spent glycol is mixed with S
2-concentration is the solution B of 0.05mol/L;
3) A solution is joined in B solution and form precursor solution C, wherein Sn by magnetic stirrer
2+: S
2-mol ratio be 1: 5;
4) solution C is poured in hydrothermal reaction kettle, compactedness is controlled at 45%; Sealing hydrothermal reaction kettle, puts it in warm-pressing double-control microwave hydrothermal reaction; Select temperature controlling mode to react, temperature is controlled at 130 ℃, and pressure is less than 3.0MPa, after reaction 100min, naturally cools to room temperature;
5) open hydrothermal reaction kettle, product, by centrifugal collection, then adopts respectively deionized water and washed with isopropyl alcohol 1～3 time, is placed in vacuum drying oven dry at 60 ℃, the bar-shaped SnS nanocrystal of final product.
Claims (2)
1. the nanocrystalline preparation method of bar-shaped SnS, is characterized in that:
1) by analytically pure SnCl
22H
2o spent glycol dissolves makes Sn
2+concentration is the clear solution A of 0.01mol/L～1.0mol/L;
2) by analytically pure (NH
4)
2s solution spent glycol is mixed with S
2-concentration is the solution B of 0.01mol/L～2.0mol/L;
3) A solution is joined in B solution and form precursor solution C by magnetic stirrer;
Sn wherein
2+: S
2-mol ratio be 1: 2～10: 1;
4) solution C is poured in hydrothermal reaction kettle, compactedness is controlled at 40%～60%; Sealing hydrothermal reaction kettle, puts it in warm-pressing double-control microwave hydrothermal reaction; Select temperature controlling mode to react, temperature is controlled at 100 ℃～150 ℃, and pressure is less than 3.0MPa, after reaction 10min～120min, naturally cools to room temperature;
5) open hydrothermal reaction kettle, product, by centrifugal collection, then adopts respectively deionized water and washed with isopropyl alcohol 1～3 time, then it is dry at 40 ℃～70 ℃ to be placed in vacuum drying oven, obtains the bar-shaped SnS nanocrystal of final product.
2. the nanocrystalline preparation method of bar-shaped SnS according to claim 1, is characterized in that: described analytically pure (NH
4)
2the S of S solution
2-concentration>=8%.
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| CN102897821A (en) * | 2012-10-19 | 2013-01-30 | 陕西科技大学 | Preparation method for cubic-phase Sm2O3 nanorod semiconductor material |
| CN102897822A (en) * | 2012-10-19 | 2013-01-30 | 陕西科技大学 | Method for preparing monoclinic Sm2O3 nanocrystal through solvothermal method |
| CN102897818A (en) * | 2012-10-19 | 2013-01-30 | 陕西科技大学 | Method for preparing Sm2O3 semiconductor nanocrystals with hexagonal sheet structures |
| CN102897819A (en) * | 2012-10-19 | 2013-01-30 | 陕西科技大学 | Method for preparing cubic-phase Sm2O3 nanocrystals by solvothermal method |
| CN102897820A (en) * | 2012-10-19 | 2013-01-30 | 陕西科技大学 | Method for preparing spherical Sm2O3 semiconductor nanocrystals by means of complex hydrothermal method |
| CN105016378B (en) * | 2014-04-21 | 2016-08-17 | 渤海大学 | The preparation method of stannous sulfide nanometer sheet |
| CN108821332B (en) * | 2018-07-05 | 2020-08-07 | 苏州影睿光学科技有限公司 | Preparation method of near-infrared stannous sulfide nanoparticles |
| CN114380324A (en) * | 2021-12-11 | 2022-04-22 | 上海工程技术大学 | P-type SnS nano-particles, P-type SnS film, and preparation and application thereof |
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Effective date of registration: 20201124 Address after: 808, floor 8, building B, business center, gangzhilong science and Technology Park, No. 6, Qinglong Road, Qinghua community, Longhua street, Longhua District, Shenzhen City, Guangdong Province Patentee after: Shenzhen Pengbo Information Technology Co.,Ltd. Address before: 710021 Shaanxi province Xi'an Weiyang University Park No. 1 Patentee before: SHAANXI University OF SCIENCE & TECHNOLOGY Effective date of registration: 20201124 Address after: No.32, group 3, Fuzi village, Donghai Town, Qidong City, Nantong City, Jiangsu Province Patentee after: Qidong Shiji crop cooperatives Address before: 808, floor 8, building B, business center, gangzhilong science and Technology Park, No. 6, Qinglong Road, Qinghua community, Longhua street, Longhua District, Shenzhen City, Guangdong Province Patentee before: Shenzhen Pengbo Information Technology Co.,Ltd. |
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