CN102502790A - Method for preparing SnS powder through microwave hydrothermal-ultrasonic chemistry method - Google Patents
Method for preparing SnS powder through microwave hydrothermal-ultrasonic chemistry method Download PDFInfo
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- CN102502790A CN102502790A CN201110374930XA CN201110374930A CN102502790A CN 102502790 A CN102502790 A CN 102502790A CN 201110374930X A CN201110374930X A CN 201110374930XA CN 201110374930 A CN201110374930 A CN 201110374930A CN 102502790 A CN102502790 A CN 102502790A
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- 239000000843 powder Substances 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000001311 chemical methods and process Methods 0.000 title abstract 3
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 36
- 239000008367 deionised water Substances 0.000 claims abstract description 15
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 15
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000007789 sealing Methods 0.000 claims abstract description 8
- 238000001291 vacuum drying Methods 0.000 claims abstract description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 21
- 230000035484 reaction time Effects 0.000 claims description 16
- 239000000047 product Substances 0.000 claims description 10
- 239000012467 final product Substances 0.000 claims description 7
- 239000002243 precursor Substances 0.000 claims description 7
- 239000002245 particle Substances 0.000 abstract description 4
- 229910021626 Tin(II) chloride Inorganic materials 0.000 abstract 1
- 238000005119 centrifugation Methods 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 235000011150 stannous chloride Nutrition 0.000 abstract 1
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 3
- 230000012010 growth Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- KGWDUNBJIMUFAP-KVVVOXFISA-N Ethanolamine Oleate Chemical compound NCCO.CCCCCCCC\C=C/CCCCCCCC(O)=O KGWDUNBJIMUFAP-KVVVOXFISA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000713 high-energy ball milling Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- DZXKSFDSPBRJPS-UHFFFAOYSA-N tin(2+);sulfide Chemical compound [S-2].[Sn+2] DZXKSFDSPBRJPS-UHFFFAOYSA-N 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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Abstract
A method for preparing SnS powder through a microwave hydrothermal-ultrasonic chemistry method comprises the following steps: dissolving SnCl2 2h2O into absolute ethyl alcohol to obtain a solution A; dissolving thioacetamide into deionized water to obtain a solution B; adding the solution A into the solution B to obtain a predecessor solution C; pouring the solution C into a hydro-thermal reaction kettle, sealing the hydro-thermal reaction kettle, putting the hydro-thermal reaction kettle into a temperature-pressure double control microwave hydro-thermal reaction instrument for hydro-thermal reaction, after the reaction, placing the hydro-thermal reaction kettle into a numerical control ultrasonic wave reaction instrument for ultrasonic wave reaction and then cooling to a room temperature naturally; opening the reaction kettle, collecting products through centrifugation, then placing the products into a vacuum drying box for drying, and finally obtaining SNS powder. In the invention, hydrothermal-ultrasonic chemistry method is adopted for preparing the SnS powder which is excellent in particle dispersivity, is controllable in appearance, and excellent in repetitiveness, the processing equipment is simple, and the reaction period is short. Therefore, the method has a wide development prospect.
Description
Technical field
The present invention relates to a kind of preparation method of SnS powder, be specifically related to the method that a kind of microwave hydrothermal-sonochemical method prepares the SnS powder.
Background technology
At present, in numerous solar cells, silicon solar cell is because its technology maturation has occupied the principal market.Thin-film solar cells because the relative silicon solar cell of its cost comes lowly, and becomes the developing direction of solar cell from now on, and in recent years, the stannous sulfide of rhombic system (SnS) is as a kind of novel solar cell material.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 light in the solar radiation good Spectral matching is arranged; Photoelectric transformation efficiency reaches 25%, is suitable as very much the light absorbing zone in the solar cell, also can be used as the near infrared detector and the photovoltage equipment of electroluminescent display.The Sn element and the S element earth content that constitute SnS in addition are abundant, and nontoxic, and therefore, SnS receives investigator's extensive concern in recent years as a kind of novel photoelectric transition material with nontoxic, environmental protection of potential application foreground.
At present; The novel SnS method of synthetic pattern has both at home and abroad: people such as Zhu [Zhu H L, Yang D R, Zhang H.Mater.Lett.; 60 (2006) 2686-2689] adopt hydrothermal method at the auxiliary down synthetic SnS nanometer flower of TGA, hydrothermal method needs the unsuitable mass production of specific experimental installation; People such as Reddy [Reddy N K, Devika M, Ahsanulhaq Q, Cryst.Growth Des., 10 (2010) 4769-4772.] are with the SnS powder of two-step approach through the synthetic quadrature box-shape of crystal seed, this method complicated steps, poor repeatability; People such as Xu [Xu Y, Al-Salim N, Bumby CW, et al.J.Am.Chem.Soc., 131 (2009) 15990-15991.] are synthetic SnS quantum dot in the thanomin system, the expensive raw materials of this reaction system; People [Aso K, Hayashi A, Tatsumisago M.Cryst.Growth Des., 11 (2011) 3900-3904] such as Keigo Aso adopt mixed solvent method synthetic needle-like and plate-like SnS nano-powder under hot conditions, and this method hot conditions is relatively harsher; People such as Liyang [Li Y, Xie H Q, Tu J P.ActaPhys.-Chim.Sin.25 (2009) 365-370.] prepare the SnS particle through methods such as high-energy ball millings, and it is more that the product of gained contains impurity.Therefore must develop a kind of suitable suitability for industrialized production, preparation technology is simple, and product purity is high, the method for preparing the SnS powder that reaction time is short.
Summary of the invention
The object of the invention is to provide a kind of equipment simple, easy handling, and preparation time is short,
Microwave hydrothermal-sonochemical method that cost is low prepares the method for SnS powder.
For achieving the above object, the technical scheme that the present invention adopts is:
1) with analytically pure SnCl
22H
2O is mixed with Sn with absolute ethyl alcohol
2+Concentration is the clear solution A of 0.001mol/L～0.01mol/L;
2) analytical pure thioacetamide (TAA) is added deionized water and be mixed with S
2-Concentration is the clear solution B of 0.01mol/L～0.1mol/L;
3) in solution A, add solution B, make Sn
2+: S
2-Mol ratio be 1: (1～10) forms precursor solution C;
4) solution C is poured in the hydrothermal reaction kettle, compactedness is controlled at 30%～80%; The sealing hydrothermal reaction kettle puts it in the two control of the temperature and pressure microwave hydrothermal reaction; Select temperature controlling mode to react, hydrothermal temperature is controlled at 80 ℃～150 ℃, and pressure is less than 2.0MPa; Reaction times is controlled at 10～60min, after reaction finishes, hydrothermal reaction kettle is inserted in the numerical control supersonic reaction appearance; Power is controlled at 200～500W; Temperature is controlled at 50～80 ℃, and the reaction times is controlled at 20～60min, and reaction naturally cools to room temperature after finishing;
5) open reaction kettle, product adopts deionized water and washed with isopropyl alcohol respectively 1～3 time then through centrifugal collection, places vacuum drying oven dry under 40 ℃～70 ℃ again, gets final product SnS powder.
The present invention adopts microwave hydrothermal-sonochemical method, and it is good to prepare the SnS particle dispersion-type, and pattern is controlled, good reproducibility, and processing unit is simple, and reaction time is short, therefore has vast potential for future development.
Description of drawings
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the prepared SnS powder of the embodiment of the invention 1;
Fig. 2 is the TEM photo of the prepared SnS powder of the embodiment of the invention 1.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is done further explain.
Embodiment 1:
1) with analytically pure SnCl
22H
2O is mixed with Sn with absolute ethyl alcohol
2+Concentration is the clear solution A of 0.005mol/L;
2) analytical pure thioacetamide (TAA) is added deionized water and be mixed with S
2-Concentration is the clear solution B of 0.01mol/L;
3) in solution A, add solution B, make Sn
2+: S
2-Mol ratio be 1: 2, form precursor solution C;
4) solution C is poured in the hydrothermal reaction kettle, compactedness is controlled at 50%; The sealing hydrothermal reaction kettle puts it in the two control of the temperature and pressure microwave hydrothermal reaction; Select temperature controlling mode to react, hydrothermal temperature is controlled at 90 ℃, and pressure is less than 2.0MPa; Reaction times is controlled at 10min, after reaction finishes, hydrothermal reaction kettle is inserted in the numerical control supersonic reaction appearance; Power is controlled at 200W; Temperature is controlled at 60 ℃, and the reaction times is controlled at 30min, and reaction naturally cools to room temperature after finishing;
5) open reaction kettle, product adopts deionized water and washed with isopropyl alcohol respectively 1～3 time then through centrifugal collection, places vacuum drying oven dry under 45 ℃ again, gets final product SnS powder.
The SnS powder of gained is analyzed with Japanese D/max2000PC x-ray diffractometer of science; At 2 θ is 26.009 °; 30.473 °; 31.531 °, 39.045 ° of edge (120), (101), (111), growths of (131) crystal face respectively, product is the rhombic system SnS (Fig. 1) of JCPDS numbering 39-0354.This sample is observed (Fig. 2) with the JSM-6460 type sem that Jeol Ltd. (JEOL) produces, can find out that from photo prepared SnS particle has special pattern.
Embodiment 2:
1) with analytically pure SnCl
22H
2O is mixed with Sn with absolute ethyl alcohol
2+Concentration is the clear solution A of 0.01mol/L;
2) analytical pure thioacetamide (TAA) is added deionized water and be mixed with S
2-Concentration is the clear solution B of 0.03mol/L;
3) in solution A, add solution B, make Sn
2+: S
2-Mol ratio be 1: 1, form precursor solution C;
4) solution C is poured in the hydrothermal reaction kettle, compactedness is controlled at 60%; The sealing hydrothermal reaction kettle puts it in the two control of the temperature and pressure microwave hydrothermal reaction; Select temperature controlling mode to react, hydrothermal temperature is controlled at 110 ℃, and pressure is less than 2.0MPa; Reaction times is controlled at 20min, after reaction finishes, hydrothermal reaction kettle is inserted in the numerical control supersonic reaction appearance; Power is controlled at 300W; Temperature is controlled at 60 ℃, and the reaction times is controlled at 25min, and reaction naturally cools to room temperature after finishing;
5) open reaction kettle, product adopts deionized water and washed with isopropyl alcohol respectively 1～3 time then through centrifugal collection, places vacuum drying oven dry under 40 ℃ again, gets final product SnS powder.
Embodiment 3:
1) with analytically pure SnCl
22H
2O is mixed with Sn with absolute ethyl alcohol
2+Concentration is the clear solution A of 0.008mol/L;
2) analytical pure thioacetamide (TAA) is added deionized water and be mixed with S
2-Concentration is the clear solution B of 0.04mol/L;
3) in solution A, add solution B, make Sn
2+: S
2-Mol ratio be 1: 5, form precursor solution C;
4) solution C is poured in the hydrothermal reaction kettle, compactedness is controlled at 70%; The sealing hydrothermal reaction kettle puts it in the two control of the temperature and pressure microwave hydrothermal reaction; Select temperature controlling mode to react, hydrothermal temperature is controlled at 120 ℃, and pressure is less than 2.0MPa; Reaction times is controlled at 30min, after reaction finishes, hydrothermal reaction kettle is inserted in the numerical control supersonic reaction appearance; Power is controlled at 350W; Temperature is controlled at 70 ℃, and the reaction times is controlled at 40min, and reaction naturally cools to room temperature after finishing;
5) open reaction kettle, product adopts deionized water and washed with isopropyl alcohol respectively 1～3 time then through centrifugal collection, places vacuum drying oven dry under 60 ℃ again, gets final product SnS powder.
Embodiment 4:
1) with analytically pure SnCl
22H
2O is mixed with Sn with absolute ethyl alcohol
2+Concentration is the clear solution A of 0.001mol/L;
2) analytical pure thioacetamide (TAA) is added deionized water and be mixed with S
2-Concentration is the clear solution B of 0.08mol/L;
3) in solution A, add solution B, make Sn
2+: S
2-Mol ratio be 1: 8, form precursor solution C;
4) solution C is poured in the hydrothermal reaction kettle, compactedness is controlled at 30%; The sealing hydrothermal reaction kettle puts it in the two control of the temperature and pressure microwave hydrothermal reaction; Select temperature controlling mode to react, hydrothermal temperature is controlled at 80 ℃, and pressure is less than 2.0MPa; Reaction times is controlled at 60min, after reaction finishes, hydrothermal reaction kettle is inserted in the numerical control supersonic reaction appearance; Power is controlled at 500W; Temperature is controlled at 50 ℃, and the reaction times is controlled at 60min, and reaction naturally cools to room temperature after finishing;
5) open reaction kettle, product adopts deionized water and washed with isopropyl alcohol respectively 1～3 time then through centrifugal collection, places vacuum drying oven dry under 50 ℃ again, gets final product SnS powder.
Embodiment 5:
1) with analytically pure SnCl
22H
2O is mixed with Sn with absolute ethyl alcohol
2+Concentration is the clear solution A of 0.003mol/L;
2) analytical pure thioacetamide (TAA) is added deionized water and be mixed with S
2-Concentration is the clear solution B of 0.1mol/L;
3) in solution A, add solution B, make Sn
2+: S
2-Mol ratio be 1: 10, form precursor solution C;
4) solution C is poured in the hydrothermal reaction kettle, compactedness is controlled at 80%; The sealing hydrothermal reaction kettle puts it in the two control of the temperature and pressure microwave hydrothermal reaction; Select temperature controlling mode to react, hydrothermal temperature is controlled at 150 ℃, and pressure is less than 2.0MPa; Reaction times is controlled at 50min, after reaction finishes, hydrothermal reaction kettle is inserted in the numerical control supersonic reaction appearance; Power is controlled at 400W; Temperature is controlled at 80 ℃, and the reaction times is controlled at 20min, and reaction naturally cools to room temperature after finishing;
5) open reaction kettle, product adopts deionized water and washed with isopropyl alcohol respectively 1～3 time then through centrifugal collection, places vacuum drying oven dry under 70 ℃ again, gets final product SnS powder.
Claims (1)
1. microwave hydrothermal-sonochemical method prepares the method for SnS powder, it is characterized in that:
1) with analytically pure SnCl
22H
2O is mixed with Sn with absolute ethyl alcohol
2+Concentration is the clear solution A of 0.001mol/L～0.01mol/L;
2) analytical pure thioacetamide (TAA) is added deionized water and be mixed with S
2-Concentration is the clear solution B of 0.01mol/L～0.1mol/L;
3) in solution A, add solution B, make Sn
2+: S
2-Mol ratio be 1: (1～10) forms precursor solution C;
4) solution C is poured in the hydrothermal reaction kettle, compactedness is controlled at 30%～80%; The sealing hydrothermal reaction kettle puts it in the two control of the temperature and pressure microwave hydrothermal reaction; Select temperature controlling mode to react, hydrothermal temperature is controlled at 80 ℃～150 ℃, and pressure is less than 2.0MPa; Reaction times is controlled at 10～60min, after reaction finishes, hydrothermal reaction kettle is inserted in the numerical control supersonic reaction appearance; Power is controlled at 200～500W; Temperature is controlled at 50～80 ℃, and the reaction times is controlled at 20～60min, and reaction naturally cools to room temperature after finishing;
5) open reaction kettle, product adopts deionized water and washed with isopropyl alcohol respectively 1～3 time then through centrifugal collection, places vacuum drying oven dry under 40 ℃～70 ℃ again, gets final product SnS powder.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106887578A (en) * | 2017-04-01 | 2017-06-23 | 中南大学 | A kind of artificial gold/CNT composite Nano negative material and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101127375A (en) * | 2007-09-12 | 2008-02-20 | 上海大学 | Method for making low resistance TiS thin film used in solar battery |
| CN101609887A (en) * | 2009-07-16 | 2009-12-23 | 浙江大学 | A kind of lithium ion battery SnS 2The preparation method of nanometer sheet negative material |
| CN101609884A (en) * | 2009-07-20 | 2009-12-23 | 北京理工大学 | A kind of lithium ion battery negative material SnS 2The preparation method |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101127375A (en) * | 2007-09-12 | 2008-02-20 | 上海大学 | Method for making low resistance TiS thin film used in solar battery |
| CN101609887A (en) * | 2009-07-16 | 2009-12-23 | 浙江大学 | A kind of lithium ion battery SnS 2The preparation method of nanometer sheet negative material |
| CN101609884A (en) * | 2009-07-20 | 2009-12-23 | 北京理工大学 | A kind of lithium ion battery negative material SnS 2The preparation method |
Non-Patent Citations (3)
| Title |
|---|
| CHANGHUA AN ET AL.: "Shape-selected synthesis of nanocrystalline SnS in different alkaline media", 《JOURNAL OF CRYSTAL GROWTH》, vol. 252, 31 December 2003 (2003-12-31), pages 581 - 586 * |
| 李红生等: "超声辅助液相合成多晶SnS纳米粉", 《人工晶体学报》, vol. 34, no. 2, 30 April 2005 (2005-04-30), pages 319 - 322 * |
| 黎阳等: "不同形貌和尺寸的锂离子电池SnS负极材料", 《物理化学学报》, vol. 25, no. 2, 28 February 2009 (2009-02-28), pages 365 - 370 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106887578A (en) * | 2017-04-01 | 2017-06-23 | 中南大学 | A kind of artificial gold/CNT composite Nano negative material and preparation method thereof |
| CN106887578B (en) * | 2017-04-01 | 2020-02-21 | 中南大学 | Tin sulfide/carbon nano tube composite nano negative electrode material and preparation method thereof |
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