CN102502791B - Method for preparing flower-cluster-shaped tin sulfide (SnS) nanometer particles by microwave hydrothermal method - Google Patents

Method for preparing flower-cluster-shaped tin sulfide (SnS) nanometer particles by microwave hydrothermal method Download PDF

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CN102502791B
CN102502791B CN 201110375499 CN201110375499A CN102502791B CN 102502791 B CN102502791 B CN 102502791B CN 201110375499 CN201110375499 CN 201110375499 CN 201110375499 A CN201110375499 A CN 201110375499A CN 102502791 B CN102502791 B CN 102502791B
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CN102502791A (en
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黄剑锋
张培培
齐慧
曹丽云
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Jiujingri Crucible (Jiangsu) New Material Technology Co.,Ltd.
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Shaanxi University of Science and Technology
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Abstract

The invention relates to a method for preparing flower-cluster-shaped tin sulfide (SnS) nanometer particles by a microwave hydrothermal method. The method comprises the steps that: SnCl2.2H2O is dissolved by concentrated hydrochloric acid, and then, de-ionized water is added to obtain solution A; thioacetamide is added into de-ionized water to obtain solution B; cetyl trimethyl ammonium bromide is added into the solution A to obtain solution C; the solution B is dripped into the solution C to obtain precursor solution D; the solution D is poured into a hydrothermal reaction kettle, and the hydrothermal reaction kettle is put into a temperature and pressure dual-control microwave hydrothermal reaction instrument; and a temperature control mode is selected for hydrothermal reaction, products are centrifugally collected after reaction completion, and then, the products are dried in an electric heating blowing drying box to obtain final products of flower-cluster-shaped SnS nanometer particles. The microwave hydrothermal method is adopted, the flower-cluster-shaped SnS particles with uniform size are fast prepared, and the reaction is completed in one step in liquid phases, the later-period treatment is not needed, in addition, the process equipment is simple, and the reaction period is short.

Description

A kind of microwave hydrothermal prepares the method for flowers shape SnS nanoparticle
Technical field
The present invention relates to a kind of method for preparing flowers shape SnS nanoparticle, be specifically related to a kind of method that microwave hydrothermal prepares flowers shape SnS nanoparticle.
Background technology
SnS is that IV～VI family has the semiconductor material of stratiform orthorhombic crystalline structure, its optics direct band gap and indirect band gap are respectively 1.3～1.5eV and 1.0～1.1eV, with the visible ray in solar radiation, good Spectral matching is arranged, 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, environmental protection of potential application foreground, has been subject to gradually in recent years people and has greatly paid close attention to.Up to now, under specific reaction conditions, success has prepared SnS nano wire [Yingkai Liu, Dedong Hou, Guanghou Wang.Chemical Physics Letters, 379 (2003) 67-73.], nanometer rod [H.L.Su, Y.Xie, Y.J.Xiong, P.Gao, Y.T.Qian, J.Solid State Chem.161 (2001) 190-196.], nano belt [C.H.An, K.B.Tang, G.Z.Shen, C.R.Wang, Q.Yang, B.Hai, Y.T.Qian, J.Crystal Growth 244 (2002) 333-338.], soccerballene [S.Y.Hong, R.Popovitz-Biro, Y.Prior, R.Tenne, J.Am.Chem.Soc.125 (2005) 10470-10474.], nanometer sheet [Guozhen Shen, Di Chen, Kaibin Tang, Liying Huang, et al.Inorganic Chemistry Communications.6 (2003) 178-180.] etc. there is the powder of special appearance.The novel unique powder of the synthetic pattern of above bibliographical information, but it is less to relate to the nano-powder self-assembly.Microwave-hydrothermal method has high reaction efficiency, and working method is simple, without the protection of rare gas element, and simple and repeated advantages of higher.In view of some unique advantages of microwave hydrothermal and the effect of tensio-active agent morphology control, both are combined and there is not yet report in the research aspect preparation self-assembly flowers shape SnS powder.Therefore, this experiment attempts adopting microwave-hydrothermal method, under Surfactant CTAB is auxiliary, by SnCl 22H 2o and CH 3cSNH 2synthesizing blossom SnS microballoon, these flowers shape microballoons are formed by the nanometer sheet self-assembly.
Summary of the invention
The object of the invention is to provide a kind of equipment simple, easy handling, and preparation time is short, and the microwave hydrothermal that cost is low prepares the method for flowers shape SnS nanoparticle.
For achieving the above object, the technical solution used in the present invention is:
1) by analytically pure SnCl 22H 2after O dissolves with concentrated hydrochloric acid, then add deionized water to be mixed with Sn 2+the clear solution A that concentration is 0.01mol/L～1.0mol/L;
2) analytically pure thioacetamide (TAA) is added in deionized water and is mixed with S 2-the clear solution B that concentration is 0.02mol/L～2.0mol/L;
3) analytically pure cetyl trimethylammonium bromide (CTAB) is added in solution A, be mixed with the clear solution that cetyl trimethylammonium bromide concentration is 0.0025mol/L～0.125mol/L, gained solution is designated as C;
4) drip solution B in C solution under magnetic agitation, finally make Sn 2+: S 2-mol ratio is 1: (1～10) forms precursor solution D;
5) solution D is poured in hydrothermal reaction kettle, compactedness is controlled at 40%～80%; The sealing hydrothermal reaction kettle, put it in the warm-pressing double-control microwave hydrothermal reaction; Select temperature controlling mode to be reacted, hydrothermal temperature is controlled at 100 ℃～180 ℃, and pressure is 1～3.0MPa, and the reaction times is controlled at 10min～120min, and reaction naturally cools to room temperature after finishing;
6) open hydrothermal reaction kettle, product, by centrifugal collection, then adopts respectively deionized water and dehydrated alcohol or washed with isopropyl alcohol 1～3 time, then is placed in electric drying oven with forced convection dry final product flowers shape SnS nanoparticle that obtains under 40 ℃～70 ℃.
The present invention adopts microwave-hydrothermal method, prepares fast even particle size flowers shape SnS particle, because reaction once completes in liquid phase, do not need post-processed, and processing unit is simple, and reaction time is short.
The accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the prepared flowers shape SnS nanoparticle of the embodiment of the present invention 1;
Fig. 2 is the TEM photo of the prepared flowers shape SnS nanoparticle 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 2after O dissolves with concentrated hydrochloric acid, then add deionized water to be mixed with Sn 2+the clear solution A that concentration is 0.05mol/L;
2) analytically pure thioacetamide (TAA) is added in deionized water and is mixed with S 2-the clear solution B that concentration is 0.1mol/L;
3) analytically pure cetyl trimethylammonium bromide (CTAB) is added in solution A, be mixed with the clear solution that cetyl trimethylammonium bromide concentration is 0.01mol/L, gained solution is designated as C;
4) drip solution B in C solution under magnetic agitation, finally make Sn 2+: S 2-mol ratio is 1: 2, forms precursor solution D;
5) solution D is poured in hydrothermal reaction kettle, compactedness is controlled at 70%; The sealing hydrothermal reaction kettle, put it in the warm-pressing double-control microwave hydrothermal reaction; Select temperature controlling mode to be reacted, hydrothermal temperature is controlled at 100 ℃, and pressure is 1.5MPa, and the reaction times is controlled at 60min, and reaction naturally cools to room temperature after finishing;
6) open hydrothermal reaction kettle, product, by centrifugal collection, then adopts respectively deionized water and absolute ethanol washing 1～3 time, then is placed in electric drying oven with forced convection dry final product flowers shape SnS nanoparticle that obtains under 40 ℃.
The SnS nanocrystal of gained is analyzed with Rigaku D/max2000PC x-ray diffractometer, at 2 θ, it is 26.009 °, 30.473 °, 31.531 °, 39.045 ° edge (120), (101), (111), the growth of (131) crystal face respectively, the rhombic system SnS (Fig. 1) that product is JCPDS numbering 39-0354.This JSM-6390A type scanning electronic microscope that for sample, Jeol Ltd. (JEOL) produces is observed to (Fig. 2), can find out that from photo prepared SnS particle has special floriform appearance, size evenly, can find out that from its partial enlarged drawing the standby flowers shape SnS particle of this legal system may be formed through assembling by the SnS particle of lamellar growth.
Embodiment 2:
1) by analytically pure SnCl 22H 2after O dissolves with concentrated hydrochloric acid, then add deionized water to be mixed with Sn 2+the clear solution A that concentration is 0.1mol/L;
2) analytically pure thioacetamide (TAA) is added in deionized water and is mixed with S 2-the clear solution B that concentration is 0.5mol/L;
3) analytically pure cetyl trimethylammonium bromide (CTAB) is added in solution A, be mixed with the clear solution that cetyl trimethylammonium bromide concentration is 0.1mol/L, gained solution is designated as C;
4) drip solution B in C solution under magnetic agitation, finally make Sn 2+: S 2-mol ratio is 1: 1, forms precursor solution D;
5) solution D is poured in hydrothermal reaction kettle, compactedness is controlled at 60%; The sealing hydrothermal reaction kettle, put it in the warm-pressing double-control microwave hydrothermal reaction; Select temperature controlling mode to be reacted, hydrothermal temperature is controlled at 120 ℃, and pressure is 1.5MPa, and the reaction times is controlled at 50min, and reaction naturally cools to room temperature after finishing;
6) open hydrothermal reaction kettle, product, by centrifugal collection, then adopts respectively deionized water and washed with isopropyl alcohol 1～3 time, then is placed in electric drying oven with forced convection dry final product flowers shape SnS nanoparticle that obtains under 60 ℃.
Embodiment 3:
1) by analytically pure SnCl 22H 2after O dissolves with concentrated hydrochloric acid, then add deionized water to be mixed with Sn 2+the clear solution A that concentration is 0.2mol/L;
2) analytically pure thioacetamide (TAA) is added in deionized water and is mixed with S 2-the clear solution B that concentration is 1.2mol/L;
3) analytically pure cetyl trimethylammonium bromide (CTAB) is added in solution A, be mixed with the clear solution that cetyl trimethylammonium bromide concentration is 0.05mol/L, gained solution is designated as C;
4) drip solution B in C solution under magnetic agitation, finally make Sn 2+: S 2-mol ratio is 1: 6, forms precursor solution D;
5) solution D is poured in hydrothermal reaction kettle, compactedness is controlled at 50%; The sealing hydrothermal reaction kettle, put it in the warm-pressing double-control microwave hydrothermal reaction; Select temperature controlling mode to be reacted, hydrothermal temperature is controlled at 140 ℃, and pressure is 2MPa, and the reaction times is controlled at 40min, and reaction naturally cools to room temperature after finishing;
6) open hydrothermal reaction kettle, product, by centrifugal collection, then adopts respectively deionized water and absolute ethanol washing 1～3 time, then is placed in electric drying oven with forced convection dry final product flowers shape SnS nanoparticle that obtains under 45 ℃.
Embodiment 4:
1) by analytically pure SnCl 22H 2after O dissolves with concentrated hydrochloric acid, then add deionized water to be mixed with Sn 2+the clear solution A that concentration is 0.5mol/L;
2) analytically pure thioacetamide (TAA) is added in deionized water and is mixed with S 2-the clear solution B that concentration is 1.5mol/L;
3) analytically pure cetyl trimethylammonium bromide (CTAB) is added in solution A, be mixed with the clear solution that cetyl trimethylammonium bromide concentration is 0.08mol/L, gained solution is designated as C;
4) drip solution B in C solution under magnetic agitation, finally make Sn 2+: S 2-mol ratio is 1: 3, forms precursor solution D;
5) solution D is poured in hydrothermal reaction kettle, compactedness is controlled at 80%; The sealing hydrothermal reaction kettle, put it in the warm-pressing double-control microwave hydrothermal reaction; Select temperature controlling mode to be reacted, hydrothermal temperature is controlled at 160 ℃, and pressure is 3MPa, and the reaction times is controlled at 10min, and reaction naturally cools to room temperature after finishing;
6) open hydrothermal reaction kettle, product, by centrifugal collection, then adopts respectively deionized water and washed with isopropyl alcohol 1～3 time, then is placed in electric drying oven with forced convection dry final product flowers shape SnS nanoparticle that obtains under 55 ℃.
Embodiment 5:
1) by analytically pure SnCl 22H 2after O dissolves with concentrated hydrochloric acid, then add deionized water to be mixed with Sn 2+the clear solution A that concentration is 1.0mol/L;
2) analytically pure thioacetamide (TAA) is added in deionized water and is mixed with S 2-the clear solution B that concentration is 2.0mol/L;
3) analytically pure cetyl trimethylammonium bromide (CTAB) is added in solution A, be mixed with the clear solution that cetyl trimethylammonium bromide concentration is 0.125mol/L, gained solution is designated as C;
4) drip solution B in C solution under magnetic agitation, finally make Sn 2+: S 2-mol ratio is 1: 8, forms precursor solution D;
5) solution D is poured in hydrothermal reaction kettle, compactedness is controlled at 80%; The sealing hydrothermal reaction kettle, put it in the warm-pressing double-control microwave hydrothermal reaction; Select temperature controlling mode to be reacted, hydrothermal temperature is controlled at 180 ℃, and pressure is 3MPa, and the reaction times is controlled at 100min, and reaction naturally cools to room temperature after finishing;
6) open hydrothermal reaction kettle, product, by centrifugal collection, then adopts respectively deionized water and absolute ethanol washing 1～3 time, then is placed in electric drying oven with forced convection dry final product flowers shape SnS nanoparticle that obtains under 70 ℃.
Embodiment 6:
1) by analytically pure SnCl 22H 2after O dissolves with concentrated hydrochloric acid, then add deionized water to be mixed with Sn 2+the clear solution A that concentration is 0.01mol/L;
2) analytically pure thioacetamide (TAA) is added in deionized water and is mixed with S 2-the clear solution B that concentration is 0.02mol/L;
3) analytically pure cetyl trimethylammonium bromide (CTAB) is added in solution A, be mixed with the clear solution that cetyl trimethylammonium bromide concentration is 0.0025mol/L, gained solution is designated as C;
4) drip solution B in C solution under magnetic agitation, finally make Sn 2+: S 2-mol ratio is 1: 10, forms precursor solution D;
5) solution D is poured in hydrothermal reaction kettle, compactedness is controlled at 40%; The sealing hydrothermal reaction kettle, put it in the warm-pressing double-control microwave hydrothermal reaction; Select temperature controlling mode to be reacted, hydrothermal temperature is controlled at 150 ℃, and pressure is 2MPa, and the reaction times is controlled at 120min, and reaction naturally cools to room temperature after finishing;
6) open hydrothermal reaction kettle, product, by centrifugal collection, then adopts respectively deionized water and washed with isopropyl alcohol 1～3 time, then is placed in electric drying oven with forced convection dry final product flowers shape SnS nanoparticle that obtains under 50 ℃.

Claims (1)

1. a microwave hydrothermal prepares the method for flowers shape SnS nanoparticle, it is characterized in that:
1) by analytically pure SnCl 22H 2after O dissolves with concentrated hydrochloric acid, then add deionized water to be mixed with Sn 2+the clear solution A that concentration is 0.01mol/L～1.0mol/L;
2) analytically pure thioacetamide is added in deionized water and is mixed with S 2-the clear solution B that concentration is 0.02mol/L～2.0mol/L;
3) analytically pure cetyl trimethylammonium bromide (CTAB) is added in solution A, be mixed with the clear solution that cetyl trimethylammonium bromide concentration is 0.0025mol/L～0.125mol/L, gained solution is designated as C;
4) drip solution B in C solution under magnetic agitation, finally make Sn 2+: S 2-mol ratio is 1:(1～10), form precursor solution D;
5) solution D is poured in hydrothermal reaction kettle, compactedness is controlled at 40%～80%; The sealing hydrothermal reaction kettle, put it in the warm-pressing double-control microwave hydrothermal reaction; Select temperature controlling mode to be reacted, hydrothermal temperature is controlled at 100 ℃～180 ℃, and pressure is 1～3.0MPa, and the reaction times is controlled at 10min～120min, and reaction naturally cools to room temperature after finishing;
6) open hydrothermal reaction kettle, product, by centrifugal collection, then adopts respectively deionized water and dehydrated alcohol or washed with isopropyl alcohol 1～3 time, then is placed in electric drying oven with forced convection dry final product flowers shape SnS nanoparticle that obtains under 40 ℃～70 ℃.
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CN107032390B (en) * 2016-11-02 2018-06-22 陕西科技大学 A kind of cube shaped frame SnS2The preparation method of anode material of lithium-ion battery
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