CN102392306A - Microwave hydro-thermal method for preparing SnS film - Google Patents
Microwave hydro-thermal method for preparing SnS film Download PDFInfo
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- CN102392306A CN102392306A CN2011103759547A CN201110375954A CN102392306A CN 102392306 A CN102392306 A CN 102392306A CN 2011103759547 A CN2011103759547 A CN 2011103759547A CN 201110375954 A CN201110375954 A CN 201110375954A CN 102392306 A CN102392306 A CN 102392306A
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- deionized water
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Abstract
A microwave hydro-thermal method for preparing a SnS film. The method comprises steps of: dissolving part of SnCl2.2H2O in concentrated hydrochloric acid; adding deionized water to obtain a solution A; adding (HN4)2S solution into deionized water to obtain a solution B; adding the solution A into the solution B with magnetic stirring to form a predecessor solution C; pouring the solution C into a hydro-thermal reaction kettle; putting glass substrate activated by concentrated nitric acid into the reaction kettle bottom, putting the reaction kettle into a temperature and pressure double control microwave hydrothermal reactor for a hydrothermal reaction and cooling to room temperature naturally after the reaction; then washing the glass substrate respectively with deionized water and waterless ethanol, drying in a vacuum drying box to obtain an end product SnS film on the glass substrate. The invention employs a microwave hydrothermal method to rapidly prepare SnS nano crystal with uniform particle size; as the reactions are completed in a liquid phase at one time, post treatment is not required; technical equipment is simple, and a reaction period is short.
Description
Technical field:
The present invention relates to a kind of SnS preparation methods, be specifically related to the method that a kind of microwave hydrothermal prepares the SnS film.
Background technology
SnS is that IV～VI family has the semiconductor material of stratiform orthorhombic crystalline structure, and unit cell is crossed over two-layer, and folded along crystalline c uranium pile, the direct energy gap Eg=1.3eV of its optics is near the best energy gap 1.5eV of solar cell; Its photoelectric transformation efficiency is than higher (about 25%) in theory; Big (α＞10 of uptake factor
-4Cm
-1), but filmization is few as the consumptive material of solar cell material; The Sn element and the S element earth content that constitute SnS in addition are abundant, cheap, nontoxic, and good Environmental compatibility is arranged.Therefore, SnS has unique advantages as a kind of novel photoelectric transition material with potential application foreground, as thin-film solar cells, because the relative silicon solar cell of its cost comes lowly, becomes the developing direction of solar cell from now on.
The method for preparing at present the SnS film has electrodip process [Subramanian B, Sanjeeviraja C, Jayachandan M.Materials Chemistry and Physics, 71 (2001) 40-46.]; Chemical vapour deposition [L.S.Price, I.P.Parkin, T.G.hibbert; Et al.Chem.Vapor Depos.4 (1998) 222.], molecular beam epitaxy [K.W.Nnebesny, G.E.Collins; P.A.Lee, et al.Chem.Mater, 3 (1991) 829.]; Spray heating decomposition [A.Ortiz, S.Lopez, Semicond.Sci.Technol; 9 (1994) 2130.], vacuum thermal evaporation plating method [Abou Shana A, Zeyada H M.Solar Energy Materials and Solar Cells.24 (2003) 555-561.]; Two-step approach [Ramakrishna Reddy K T, Purandhara Reddy P.Material Letters, 56 (2002) 108-111.] etc.These methods or higher to equipment requirements, otherwise raw material availability is lower, otherwise complex process, poor repeatability.In order to reach the purpose of practicality scale operation, necessary Development and Production technology is simple, and raw material availability is high, the SnS thin film preparation process that preparation cycle 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, and cost is low, does not need the microwave hydrothermal of anneal to prepare the method for SnS film.Film by preparation method of the present invention prepares is even, and purity is higher, no visible defects, and visual appearance is higher.
For achieving the above object, the technical scheme that the present invention adopts is:
1) with analytically pure SnCl
22H
2O is dissolved in the concentrated hydrochloric acid, adds deionized water again and is mixed with Sn
2+Concentration is the clear solution A of 0.001mol/L～0.5mol/L;
2) with analytically pure (NH
4)
2S solution adds deionized water and is mixed with S
2-Concentration is the yellow solution B of 0.001mol/L～1.0mol/L;
3) under magnetic agitation, the A drips of solution is added to formation precursor solution C in the B solution;
Sn wherein
2+/ S
2-Mol ratio be 1: 2～5: 1;
4) solution C is poured in the hydrothermal reaction kettle, compactedness is controlled at 30%～80%; To adopt the glass substrate of concentrated nitric acid activation treatment to put into the hydrothermal reaction kettle bottom then, 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, and the reaction times is controlled at 60min～180min, and reaction naturally cools to room temperature after finishing;
5) open hydrothermal reaction kettle, take out glass substrate, adopt deionized water and absolute ethyl alcohol to wash respectively then respectively 1～3 time, in vacuum drying oven,, promptly on glass substrate, obtain final product SnS film at 40 ℃～70 ℃ following dry 10min～60min.
Described analytically pure (NH
4)
2The S of S solution
2-Concentration>=8%.
Described glass substrate is placed on earlier and filled in the beaker that concentration is 35% hydrochloric acid ultrasonic cleaning 30 minutes, uses washed with de-ionized water then; Washed with de-ionized water is used in ultrasonic cleaning 30 minutes in filling the beaker of acetone more then; Then in filling the beaker of aqueous ethanolic solution, cleaned 30 minutes, wherein ethanol in the aqueous ethanolic solution: the volume ratio of water is 1: 1, uses washed with de-ionized water then; Cleaned 30 minutes in deionized water for ultrasonic at last, be put in the thermostatic drying chamber rapidly then and dry.
The present invention adopts microwave-hydrothermal method, prepares even particle size SnS nanocrystal fast, once accomplishes owing to be reflected in the liquid phase, do not need post-processed, and processing unit is simple, and reaction time is short.
Description of drawings
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the prepared SnS film 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 dissolved in the concentrated hydrochloric acid, adds deionized water again and is mixed with Sn
2+Concentration is the clear solution A of 0.001mol/L;
2) with analytically pure S
2-(the NH of concentration>=8%
4)
2S solution adds deionized water and is mixed with S
2-Concentration is the yellow solution B of 0.001mol/L;
3) under magnetic agitation, the A drips of solution is added to formation precursor solution C in the B solution;
Sn wherein
2+/ S
2-Mol ratio be 1: 1;
4) glass substrate is placed on filled in the beaker that concentration is 35% hydrochloric acid ultrasonic cleaning 30 minutes earlier, use washed with de-ionized water then; Washed with de-ionized water is used in ultrasonic cleaning 30 minutes in filling the beaker of acetone more then; Then in filling the beaker of aqueous ethanolic solution, cleaned 30 minutes, wherein ethanol in the aqueous ethanolic solution: the volume ratio of water is 1: 1, uses washed with de-ionized water then; Cleaned 30 minutes in deionized water for ultrasonic at last, be put in the thermostatic drying chamber rapidly then and dry, the glass substrate after the oven dry is used the concentrated nitric acid activation treatment;
5) solution C is poured in the hydrothermal reaction kettle, compactedness is controlled at 35%; Then glass substrate after the activation is put into the hydrothermal reaction kettle bottom, 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, and the reaction times is controlled at 60min, and reaction naturally cools to room temperature after finishing;
6) open hydrothermal reaction kettle, take out glass substrate, adopt deionized water and absolute ethyl alcohol to wash respectively then respectively 1～3 time, in vacuum drying oven,, promptly on glass substrate, obtain final product SnS film at 50 ℃ of following dry 30min.
The SnS film of gained is analyzed with Japanese D/max2000PC x-ray diffractometer of science, and the discovery product is rhombic form (Fig. 1), is 30.478 ° at 2 θ; 31.579 °; 31.903 °, locate diffraction peak for 39.059 °, the crystal face of corresponding SnS is (101), (111), (040), (131).
Embodiment 2:
1) with analytically pure SnCl
22H
2O is dissolved in the concentrated hydrochloric acid, adds deionized water again and is mixed with Sn
2+Concentration is the clear solution A of 0.05mol/L;
2) with analytically pure S
2-(the NH of concentration>=8%
4)
2S solution adds deionized water and is mixed with S
2-Concentration is the yellow solution B of 0.15mol/L;
3) under magnetic agitation, the A drips of solution is added to formation precursor solution C in the B solution;
Sn wherein
2+/ S
2-Mol ratio be 1: 3;
4) glass substrate is placed on filled in the beaker that concentration is 35% hydrochloric acid ultrasonic cleaning 30 minutes earlier, use washed with de-ionized water then; Washed with de-ionized water is used in ultrasonic cleaning 30 minutes in filling the beaker of acetone more then; Then in filling the beaker of aqueous ethanolic solution, cleaned 30 minutes, wherein ethanol in the aqueous ethanolic solution: the volume ratio of water is 1: 1, uses washed with de-ionized water then; Cleaned 30 minutes in deionized water for ultrasonic at last, be put in the thermostatic drying chamber rapidly then and dry, the glass substrate after the oven dry is used the concentrated nitric acid activation treatment;
5) solution C is poured in the hydrothermal reaction kettle, compactedness is controlled at 60%; Then glass substrate after the activation is put into the hydrothermal reaction kettle bottom, 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, and the reaction times is controlled at 80min, and reaction naturally cools to room temperature after finishing;
6) open hydrothermal reaction kettle, take out glass substrate, adopt deionized water and absolute ethyl alcohol to wash respectively then respectively 1～3 time, in vacuum drying oven,, promptly on glass substrate, obtain final product SnS film at 60 ℃ of following dry 20min.
Embodiment 3:
1) with analytically pure SnCl
22H
2O is dissolved in the concentrated hydrochloric acid, adds deionized water again and is mixed with Sn
2+Concentration is the clear solution A of 0.2mol/L;
2) with analytically pure S
2-(the NH of concentration>=8%
4)
2S solution adds deionized water and is mixed with S
2-Concentration is the yellow solution B of 0.1mol/L;
3) under magnetic agitation, the A drips of solution is added to formation precursor solution C in the B solution;
Sn wherein
2+/ S
2-Mol ratio be 2: 1;
4) glass substrate is placed on filled in the beaker that concentration is 35% hydrochloric acid ultrasonic cleaning 30 minutes earlier, use washed with de-ionized water then; Washed with de-ionized water is used in ultrasonic cleaning 30 minutes in filling the beaker of acetone more then; Then in filling the beaker of aqueous ethanolic solution, cleaned 30 minutes, wherein ethanol in the aqueous ethanolic solution: the volume ratio of water is 1: 1, uses washed with de-ionized water then; Cleaned 30 minutes in deionized water for ultrasonic at last, be put in the thermostatic drying chamber rapidly then and dry, the glass substrate after the oven dry is used the concentrated nitric acid activation treatment;
5) solution C is poured in the hydrothermal reaction kettle, compactedness is controlled at 70%; Then glass substrate after the activation is put into the hydrothermal reaction kettle bottom, 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 140 ℃, and pressure is less than 2.0MPa, and the reaction times is controlled at 100min, and reaction naturally cools to room temperature after finishing;
6) open hydrothermal reaction kettle, take out glass substrate, adopt deionized water and absolute ethyl alcohol to wash respectively then respectively 1～3 time, in vacuum drying oven,, promptly on glass substrate, obtain final product SnS film at 40 ℃ of following dry 60min.
Embodiment 4:
1) with analytically pure SnCl
22H
2O is dissolved in the concentrated hydrochloric acid, adds deionized water again and is mixed with Sn
2+Concentration is the clear solution A of 0.5mol/L;
2) with analytically pure S
2-(the NH of concentration>=8%
4)
2S solution adds deionized water and is mixed with S
2-Concentration is the yellow solution B of 0.1mol/L;
3) under magnetic agitation, the A drips of solution is added to formation precursor solution C in the B solution;
Sn wherein
2+/ S
2-Mol ratio be 5: 1;
4) glass substrate is placed on filled in the beaker that concentration is 35% hydrochloric acid ultrasonic cleaning 30 minutes earlier, use washed with de-ionized water then; Washed with de-ionized water is used in ultrasonic cleaning 30 minutes in filling the beaker of acetone more then; Then in filling the beaker of aqueous ethanolic solution, cleaned 30 minutes, wherein ethanol in the aqueous ethanolic solution: the volume ratio of water is 1: 1, uses washed with de-ionized water then; Cleaned 30 minutes in deionized water for ultrasonic at last, be put in the thermostatic drying chamber rapidly then and dry, the glass substrate after the oven dry is used the concentrated nitric acid activation treatment;
5) solution C is poured in the hydrothermal reaction kettle, compactedness is controlled at 45%; Then glass substrate after the activation is put into the hydrothermal reaction kettle bottom, 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, and the reaction times is controlled at 120min, and reaction naturally cools to room temperature after finishing;
6) open hydrothermal reaction kettle, take out glass substrate, adopt deionized water and absolute ethyl alcohol to wash respectively then respectively 1～3 time, in vacuum drying oven,, promptly on glass substrate, obtain final product SnS film at 55 ℃ of following dry 40min.
Embodiment 5:
1) with analytically pure SnCl
22H
2O is dissolved in the concentrated hydrochloric acid, adds deionized water again and is mixed with Sn
2+Concentration is the clear solution A of 0.25mol/L;
2) with analytically pure S
2-(the NH of concentration>=8%
4)
2S solution adds deionized water and is mixed with S
2-Concentration is the yellow solution B of 1.0mol/L;
3) under magnetic agitation, the A drips of solution is added to formation precursor solution C in the B solution;
Sn wherein
2+/ S
2-Mol ratio be 1: 4;
4) glass substrate is placed on filled in the beaker that concentration is 35% hydrochloric acid ultrasonic cleaning 30 minutes earlier, use washed with de-ionized water then; Washed with de-ionized water is used in ultrasonic cleaning 30 minutes in filling the beaker of acetone more then; Then in filling the beaker of aqueous ethanolic solution, cleaned 30 minutes, wherein ethanol in the aqueous ethanolic solution: the volume ratio of water is 1: 1, uses washed with de-ionized water then; Cleaned 30 minutes in deionized water for ultrasonic at last, be put in the thermostatic drying chamber rapidly then and dry, the glass substrate after the oven dry is used the concentrated nitric acid activation treatment;
5) solution C is poured in the hydrothermal reaction kettle, compactedness is controlled at 80%; Then glass substrate after the activation is put into the hydrothermal reaction kettle bottom, 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 130 ℃, and pressure is less than 2.0MPa, and the reaction times is controlled at 150min, and reaction naturally cools to room temperature after finishing;
6) open hydrothermal reaction kettle, take out glass substrate, adopt deionized water and absolute ethyl alcohol to wash respectively then respectively 1～3 time, in vacuum drying oven,, promptly on glass substrate, obtain final product SnS film at 60 ℃ of following dry 30min.
Embodiment 6:
1) with analytically pure SnCl
22H
2O is dissolved in the concentrated hydrochloric acid, adds deionized water again and is mixed with Sn
2+Concentration is the clear solution A of 0.5mol/L;
2) with analytically pure S
2-(the NH of concentration>=8%
4)
2S solution adds deionized water and is mixed with S
2-Concentration is the yellow solution B of 1.0mol/L;
3) under magnetic agitation, the A drips of solution is added to formation precursor solution C in the B solution;
Sn wherein
2+/ S
2-Mol ratio be 1: 2;
4) glass substrate is placed on filled in the beaker that concentration is 35% hydrochloric acid ultrasonic cleaning 30 minutes earlier, use washed with de-ionized water then; Washed with de-ionized water is used in ultrasonic cleaning 30 minutes in filling the beaker of acetone more then; Then in filling the beaker of aqueous ethanolic solution, cleaned 30 minutes, wherein ethanol in the aqueous ethanolic solution: the volume ratio of water is 1: 1, uses washed with de-ionized water then; Cleaned 30 minutes in deionized water for ultrasonic at last, be put in the thermostatic drying chamber rapidly then and dry, the glass substrate after the oven dry is used the concentrated nitric acid activation treatment;
5) solution C is poured in the hydrothermal reaction kettle, compactedness is controlled at 30%; Then glass substrate after the activation is put into the hydrothermal reaction kettle bottom, 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, and the reaction times is controlled at 180min, and reaction naturally cools to room temperature after finishing;
6) open hydrothermal reaction kettle, take out glass substrate, adopt deionized water and absolute ethyl alcohol to wash respectively then respectively 1～3 time, in vacuum drying oven,, promptly on glass substrate, obtain final product SnS film at 70 ℃ of following dry 10min.
Claims (3)
1. a microwave hydrothermal prepares the method for SnS film, it is characterized in that:
1) with analytically pure SnCl
22H
2O is dissolved in the concentrated hydrochloric acid, adds deionized water again and is mixed with Sn
2+Concentration is the clear solution A of 0.001mol/L～0.5mol/L;
2) with analytically pure (NH
4)
2S solution adds deionized water and is mixed with S
2-Concentration is the yellow solution B of 0.001mol/L～1.0mol/L;
3) under magnetic agitation, the A drips of solution is added to formation precursor solution C in the B solution;
Sn wherein
2+/ S
2-Mol ratio be 1: 2～5: 1;
4) solution C is poured in the hydrothermal reaction kettle, compactedness is controlled at 30%～80%; To adopt the glass substrate of concentrated nitric acid activation treatment to put into the hydrothermal reaction kettle bottom then, 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, and the reaction times is controlled at 60min～180min, and reaction naturally cools to room temperature after finishing;
5) open hydrothermal reaction kettle, take out glass substrate, adopt deionized water and absolute ethyl alcohol to wash respectively then respectively 1～3 time, in vacuum drying oven,, promptly on glass substrate, obtain final product SnS film at 40 ℃～70 ℃ following dry 10min～60min.
2. microwave hydrothermal according to claim 1 prepares the method for SnS film, it is characterized in that: described analytically pure (NH
4)
2The S of S solution
2-Concentration>=8%.
3. microwave hydrothermal according to claim 1 prepares the method for SnS film, it is characterized in that: described glass substrate is placed on earlier and filled in the beaker that concentration is 35% hydrochloric acid ultrasonic cleaning 30 minutes, uses washed with de-ionized water then; Washed with de-ionized water is used in ultrasonic cleaning 30 minutes in filling the beaker of acetone more then; Then in filling the beaker of aqueous ethanolic solution, cleaned 30 minutes, wherein ethanol in the aqueous ethanolic solution: the volume ratio of water is 1: 1, uses washed with de-ionized water then; Cleaned 30 minutes in deionized water for ultrasonic at last, be put in the thermostatic drying chamber rapidly then and dry.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108842184A (en) * | 2018-06-27 | 2018-11-20 | 北京航空航天大学 | A kind of p-type SnS monocrystal material and preparation method thereof |
| CN113295670A (en) * | 2021-05-21 | 2021-08-24 | 合肥工业大学 | Preparation method of micro-fluidic chip detection device based on SERS substrate |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101838155A (en) * | 2010-05-25 | 2010-09-22 | 陕西科技大学 | Method for preparing hexagonal flaky cadmium sulphide membrane in microwave hydrothermal mode |
-
2011
- 2011-11-23 CN CN2011103759547A patent/CN102392306A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101838155A (en) * | 2010-05-25 | 2010-09-22 | 陕西科技大学 | Method for preparing hexagonal flaky cadmium sulphide membrane in microwave hydrothermal mode |
Non-Patent Citations (1)
| Title |
|---|
| 李兵等: "SnS2/SnS 薄膜太阳能电池的制备与性能研究", 《合肥工业大学学报(自然科学版)》, vol. 32, no. 6, 30 June 2009 (2009-06-30) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108842184A (en) * | 2018-06-27 | 2018-11-20 | 北京航空航天大学 | A kind of p-type SnS monocrystal material and preparation method thereof |
| CN113295670A (en) * | 2021-05-21 | 2021-08-24 | 合肥工业大学 | Preparation method of micro-fluidic chip detection device based on SERS substrate |
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Application publication date: 20120328 |