CN104085915A - Preparation method for hexagonal CdS nanosheet with high-energy crystal face (001) exposed - Google Patents
Preparation method for hexagonal CdS nanosheet with high-energy crystal face (001) exposed Download PDFInfo
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- dodecyl mercaptan
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Abstract
The invention discloses a preparation method for hexagonal CdS nanosheets with high-energy crystal face (001) exposed. Small size hexagonal CdS nanosheets with the high-energy crystal face (001) exposed is prepared by adopting a simple refluxing method. A diagonal size of the CdS nanosheets is 5-50 nm and the thickness of the CdS nanosheets is 0.59-10 nm. The preparation method is simple in operations, low in cost and good in repeatability. The prepared hexagonal CdS nanosheets with high-energy crystal face (001) exposed is hopeful to show enhanced photoelectric properties in applications of photocatalysis, solar cells, superionic conductors, lithium ion batteries and supercapacitors.
Description
Technical field
The invention belongs to low dimensional structures Semiconductor Optoeletronic Materials technical field, be specifically related to a kind of preparation method who exposes high energy (001) crystal face six side's phase CdS nanometer sheet.
Background technology
As everyone knows, the physical and chemical performance of semiconductor nano material depends on its size and pattern strongly.Particularly it is found that recently that exposure high energy crystal face can effectively improve catalysis and the sensing capabilities of material, therefore, the preparation that exposes high energy active face semiconductor nano material has very important scientific meaning and huge using value.But the high energy crystal face speed of growth is very fast in crystal growing process, be difficult for coming out, the crystal face conventionally exposing is the crystal face of SA low surface energy.Therefore, the preparation of exposure high reactivity crystal face semiconductor material remains a huge challenge.
CdS is II-VI family direct band-gap semicondictor material, has two kinds of crystalline structure of cubic zinc blende and hexagonal wurtzite.Due to its unique optics, electricity and catalysis characteristics, make CdS there is potential using value widely in fields such as solar cell, nano generator, photodiode, laser apparatus and catalysis.We know that six side's phase CdS (001) crystal faces are high energy crystal faces, and its surface can be than the height of low energy crystal face [J.Am.Chem.Soc.2013,135,10411-10417].Up to the present, people have adopted hydrothermal method to synthesize the CdS nanotrees impeller structure [J.Mater.Chem. of exposure (001) crystal face, 2012,22,23815-23820] and flower-like structure [Materials Research Bulletin, 2012,47 of the sheet composition of thickness approximately 0.06～0.07 μ m, 3070-3077], find that they have the performance of photocatalytic hydrogen production by water decomposition and the degradation of organic dyes of enhancing.But the above-mentioned flower-like structure thickness being made up of sheet is thicker, approximately 0.06～0.07 μ m, high energy (001) the face ratio of exposure is less, affects its catalytic performance.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method that exposes the undersized six side's phase CdS nanometer sheet of high energy (001) crystal face of preparing by simple circumfluence method.
Solving the problems of the technologies described above adopted technical scheme is: by CdCl
22.5H
2o, Dodecyl Mercaptan add in oleyl amine, stir, and are warming up to 220～350 DEG C under inert atmosphere, constant temperature stirring and refluxing 1～10 hour, or first by CdCl
22.5H
2o adds in oleyl amine, stirs, and is warming up to 220～350 DEG C, then adds Dodecyl Mercaptan, constant temperature stirring and refluxing 1～10 hour, described CdCl under inert atmosphere
22.5H
2the mol ratio of O and Dodecyl Mercaptan is 1:5～200, and the volume ratio of oleyl amine and Dodecyl Mercaptan is 1～10:1, is prepared into and exposes high energy (001) crystal face six side's phase CdS nanometer sheet.
The preferred CdCl of the present invention
22.5H
2the mol ratio of O and Dodecyl Mercaptan is 1:80～105, and the volume ratio of oleyl amine and Dodecyl Mercaptan is 5～9:1.
The present invention is 250～300 DEG C of stirring and refluxing 2～5 hours under inert atmosphere preferably, best under inert atmosphere 270 DEG C of stirring and refluxing 3 hours.
The present invention adopts simple circumfluence method to be prepared into CdS nanometer sheet, and it has hexagonal wurtzite structure, exposes high energy (001) crystal face, and the Diagonal Dimension of CdS nanometer sheet is that 5～50nm, thickness are 0.59～10nm.The present invention is simple to operate, cost is low, reproducible, six side's phase CdS nanometer sheet of prepared exposure high energy (001) crystal face are expected to embody the photoelectric properties that strengthen in the application such as photochemical catalysis, solar cell, superionic conductor(s), lithium ion battery and ultracapacitor.
Brief description of the drawings
Fig. 1 is the X-ray diffractogram of the CdS nanometer sheet prepared of embodiment 1.
Fig. 2 is the transmission electron microscope picture of the CdS nanometer sheet prepared of embodiment 1.
Fig. 3 is the high explanation in the part transmission electron microscope photo of Fig. 2.
Fig. 4 is the high explanation in the part transmission electron microscope photo of Fig. 3.
Fig. 5 is the Fast Fourier Transform (FFT) figure of the CdS nanometer sheet prepared of embodiment 1.
Fig. 6 is the atomic force microscope figure of the CdS nanometer sheet prepared of embodiment 1.
Fig. 7 is the thickness curve of the interior sample of AB linear extent in Fig. 6.
Fig. 8 is the transmission electron microscope picture of the CdS nanometer sheet prepared of embodiment 2.
Fig. 9 is the transmission electron microscope picture of the CdS nanometer sheet prepared of embodiment 3.
Figure 10 is the transmission electron microscope picture of the CdS nanometer sheet prepared of embodiment 4.
Figure 11 is the transmission electron microscope picture of the CdS nanometer sheet prepared of embodiment 5.
Figure 12 is the transmission electron microscope picture of the CdS nanometer sheet prepared of embodiment 6.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in more detail, but protection scope of the present invention is not limited only to these embodiment.
Embodiment 1
Under room temperature, by 0.0091g (0.04mmol) CdCl
22.5H
2o, 1mL (4.2mmol) Dodecyl Mercaptan, 9mL oleyl amine add in 50mL round-bottomed flask, CdCl
22.5H
2the mol ratio of O and Dodecyl Mercaptan is 1:105; the volume ratio of oleyl amine and Dodecyl Mercaptan is 9:1; round-bottomed flask is placed in to sand-bath; under argon gas atmosphere protection, be warming up to 270 DEG C, constant temperature stirring and refluxing 3 hours, naturally cools to room temperature; centrifugal; by product absolute ethanol washing 3 times, drying at room temperature, is prepared into and exposes high energy (001) crystal face six side's phase CdS nanometer sheet.
From Fig. 1～7, prepared single CdS nanometer sheet is single-chip, has hexagonal wurtzite structure, and exposes high energy (001) crystal face, and CdS nanometer sheet Diagonal Dimension is 13nm, the about 0.59nm of thickness.
Embodiment 2
Under room temperature, by 0.0114g (0.05mmol) CdCl
22.5H
2o, 1mL (4.2mmol) Dodecyl Mercaptan, 5mL oleyl amine add in 50mL round-bottomed flask, CdCl
22.5H
2the mol ratio of O and Dodecyl Mercaptan is 1:84; the volume ratio of oleyl amine and Dodecyl Mercaptan is 5:1; round-bottomed flask is placed in to sand-bath, stirs, under argon gas atmosphere protection, be warming up to 300 DEG C; constant temperature stirring and refluxing 5 hours; naturally cool to room temperature, centrifugal, by product absolute ethanol washing 3 times; drying at room temperature, is prepared into and exposes high energy (001) crystal face six side's phase CdS nanometer sheet.As seen from Figure 8, prepared CdS nanometer sheet diagonal lines mean sizes is about 40～50nm, the about 8nm of thickness.
Embodiment 3
Under room temperature, by 0.1911g (0.84mmol) CdCl
22.5H
2o, 1mL (4.2mmol) Dodecyl Mercaptan, 1mL oleyl amine add in 50mL round-bottomed flask, CdCl
22.5H
2the mol ratio of O and Dodecyl Mercaptan is 1:5; the volume ratio of oleyl amine and Dodecyl Mercaptan is 1:1; round-bottomed flask is placed in to sand-bath, stirs, under argon gas atmosphere protection, be warming up to 220 DEG C; constant temperature stirring and refluxing 10 hours; naturally cool to room temperature, centrifugal, by product absolute ethanol washing 3 times; drying at room temperature, is prepared into and exposes high energy (001) crystal face six side's phase CdS nanometer sheet.As seen from Figure 9, prepared CdS nanometer sheet diagonal lines mean sizes is about 30～40nm, the about 7.6nm of thickness.
Embodiment 4
Under room temperature, by 0.0114g (0.05mmol) CdCl
22.5H
2o, 1mL oleyl amine add in 50mL round-bottomed flask, and round-bottomed flask is placed in to sand-bath, stir, and under argon gas atmosphere protection, are warming up to 270 DEG C, then add 1mL (4.2mmol) Dodecyl Mercaptan, CdCl
22.5H
2the mol ratio of O and Dodecyl Mercaptan is 1:84, and the volume ratio of oleyl amine and Dodecyl Mercaptan is 1:1, constant temperature stirring and refluxing 3 hours, naturally cool to room temperature, centrifugal, by product absolute ethanol washing 3 times, drying at room temperature, is prepared into and exposes high energy (001) crystal face six side's phase CdS nanometer sheet.As seen from Figure 10, prepared CdS nanometer sheet Diagonal Dimension is about 8nm, the about 1.6nm of thickness.
Embodiment 5
Under room temperature, by 0.0114g (0.05mmol) CdCl
22.5H
2o, 1mL oleyl amine add in 50mL round-bottomed flask, and round-bottomed flask is placed in to sand-bath, stir, and under argon gas atmosphere protection, are warming up to 250 DEG C, then add 1mL (4.2mmol) Dodecyl Mercaptan, CdCl
22.5H
2the mol ratio of O and Dodecyl Mercaptan is 1:84, and the volume ratio of oleyl amine and Dodecyl Mercaptan is 1:1, constant temperature stirring and refluxing 3 hours, naturally cool to room temperature, centrifugal, by product absolute ethanol washing 3 times, drying at room temperature, obtains exposing high energy (001) crystal face six side's phase CdS nanometer sheet.As seen from Figure 11, prepared CdS nanometer sheet diagonal lines mean sizes is 8～12nm, the about 2nm of thickness.
Embodiment 6
Under room temperature, by 0.0114g (0.05mmol) CdCl
22.5H
2o, 1mL oleyl amine add in 50mL round-bottomed flask, and round-bottomed flask is placed in to sand-bath, stir, and under argon gas atmosphere protection, are warming up to 250 DEG C, then add 1mL (4.2mmol) Dodecyl Mercaptan, CdCl
22.5H
2the mol ratio of O and Dodecyl Mercaptan is 1:84, and the volume ratio of oleyl amine and Dodecyl Mercaptan is 1:1, constant temperature stirring and refluxing 3 hours, naturally cool to room temperature, centrifugal, by product absolute ethanol washing 3 times, drying at room temperature, obtains exposing high energy (001) crystal face six side's phase CdS nanometer sheet.As seen from Figure 12, prepared CdS nanometer sheet diagonal lines mean sizes is 7.4～17.6nm, the about 1.7nm of thickness.
Embodiment 7
Under room temperature, by 0.0048g (0.021mmol) CdCl
22.5H
2o, 1mL (4.2mmol) Dodecyl Mercaptan, 10mL oleyl amine add in 50mL round-bottomed flask, CdCl
22.5H
2the mol ratio of O and Dodecyl Mercaptan is 1:200; the volume ratio of oleyl amine and Dodecyl Mercaptan is 1:10; round-bottomed flask is placed in to sand-bath, stirs, under argon gas atmosphere protection, be warming up to 350 DEG C; constant temperature stirring and refluxing 2 hours; naturally cool to room temperature, centrifugal, by product absolute ethanol washing 3 times; drying at room temperature, is prepared into and exposes high energy (001) crystal face six side's phase CdS nanometer sheet.
Claims (8)
1. a preparation method who exposes high energy (001) crystal face six side's phase CdS nanometer sheet, is characterized in that: by CdCl
22.5H
2o, Dodecyl Mercaptan add in oleyl amine, stir, and are warming up to 220～350 DEG C, constant temperature stirring and refluxing 1～10 hour, described CdCl under inert atmosphere
22.5H
2the mol ratio of O and Dodecyl Mercaptan is 1:5～200, and the volume ratio of oleyl amine and Dodecyl Mercaptan is 1～10:1, is prepared into and exposes high energy (001) crystal face six side's phase CdS nanometer sheet.
2. the preparation method of exposure high energy according to claim 1 (001) crystal face six side's phase CdS nanometer sheet, is characterized in that: described CdCl
22.5H
2the mol ratio of O and Dodecyl Mercaptan is 1:80～105, and the volume ratio of oleyl amine and Dodecyl Mercaptan is 5～9:1.
3. the preparation method of exposure high energy according to claim 1 and 2 (001) crystal face six side's phase CdS nanometer sheet, is characterized in that: 250～300 DEG C of stirring and refluxing 2～5 hours under inert atmosphere.
4. the preparation method of exposure high energy according to claim 1 and 2 (001) crystal face six side's phase CdS nanometer sheet, is characterized in that: 270 DEG C of stirring and refluxing 3 hours under inert atmosphere.
5. a preparation method who exposes high energy (001) crystal face six side's phase CdS nanometer sheet, is characterized in that: by CdCl
22.5H
2o adds in oleyl amine, stirs, and is warming up to 220～350 DEG C, then adds Dodecyl Mercaptan, constant temperature stirring and refluxing 1～10 hour, described CdCl under inert atmosphere
22.5H
2the mol ratio of O and Dodecyl Mercaptan is 1:5～200, and the volume ratio of oleyl amine and Dodecyl Mercaptan is 1～10:1, is prepared into and exposes high energy (001) crystal face six side's phase CdS nanometer sheet.
6. the preparation method of exposure high energy according to claim 5 (001) crystal face six side's phase CdS nanometer sheet, is characterized in that: described CdCl
22.5H
2the mol ratio of O and Dodecyl Mercaptan is 1:80～105, and the volume ratio of oleyl amine and Dodecyl Mercaptan is 5～9:1.
7. according to the preparation method of exposure high energy (001) the crystal face six side's phase CdS nanometer sheet described in claim 5 or 6, it is characterized in that: 250～300 DEG C of stirring and refluxing 2～5 hours under inert atmosphere.
8. according to the preparation method of exposure high energy (001) the crystal face six side's phase CdS nanometer sheet described in claim 5 or 6, it is characterized in that: 270 DEG C of stirring and refluxing 3 hours under inert atmosphere.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105463580A (en) * | 2016-01-07 | 2016-04-06 | 中国科学院理化技术研究所 | Preparation method of cadmium selenide or cadmium sulfide two-dimensional monocrystal nanosheet |
| CN105632781A (en) * | 2016-03-03 | 2016-06-01 | 哈尔滨工程大学 | Preparation method of super capacitor electrode material containing cadmium sulfide |
| CN108048900A (en) * | 2017-12-17 | 2018-05-18 | 华中科技大学 | A kind of method and product for preparing non-laminar two-dimensional nano cadmium sulfide crystalline material |
| CN109928369A (en) * | 2019-04-18 | 2019-06-25 | 中国科学院理化技术研究所 | A kind of non-laminar nano metal sulfide piece and preparation method thereof |
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| CN103212426A (en) * | 2013-03-25 | 2013-07-24 | 温州大学 | Nano heterojunction and preparation method thereof |
| CN103359770A (en) * | 2012-03-28 | 2013-10-23 | 华东师范大学 | Synthesis method of metal sulfide nano-structure material |
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| CN103359770A (en) * | 2012-03-28 | 2013-10-23 | 华东师范大学 | Synthesis method of metal sulfide nano-structure material |
| CN103212426A (en) * | 2013-03-25 | 2013-07-24 | 温州大学 | Nano heterojunction and preparation method thereof |
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| ZHONGBIN ZHUANG ET AL.: "A Facile "Dispersion-Decomposition" Route to Metal Sulfide Nanocrystals", 《CHEM. EUR. J.》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105463580A (en) * | 2016-01-07 | 2016-04-06 | 中国科学院理化技术研究所 | Preparation method of cadmium selenide or cadmium sulfide two-dimensional monocrystal nanosheet |
| CN105463580B (en) * | 2016-01-07 | 2018-05-08 | 中国科学院理化技术研究所 | A kind of preparation method of cadmium selenide or cadmium sulfide two dimension single crystal nanoplate |
| CN105632781A (en) * | 2016-03-03 | 2016-06-01 | 哈尔滨工程大学 | Preparation method of super capacitor electrode material containing cadmium sulfide |
| CN105632781B (en) * | 2016-03-03 | 2018-07-24 | 哈尔滨工程大学 | A kind of preparation method of the electrode material for super capacitor containing cadmium sulfide |
| CN108048900A (en) * | 2017-12-17 | 2018-05-18 | 华中科技大学 | A kind of method and product for preparing non-laminar two-dimensional nano cadmium sulfide crystalline material |
| CN108048900B (en) * | 2017-12-17 | 2019-07-23 | 华中科技大学 | A kind of method and product preparing non-laminar two-dimensional nano cadmium sulfide crystalline material |
| CN109928369A (en) * | 2019-04-18 | 2019-06-25 | 中国科学院理化技术研究所 | A kind of non-laminar nano metal sulfide piece and preparation method thereof |
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