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Unstratified metal sulfide nanosheet and preparation method thereof

A technology of metal sulfides and nanosheets, applied in the preparation of sulfides/polysulfides, chemical instruments and methods, lead sulfide, etc., can solve problems such as difficult kinetic factor regulation, difficult formation of synthesis methods, unfavorable nanocrystals, etc. , to achieve good application prospects, easy preparation, and simple raw materials

Active Publication Date: 2019-06-25
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The thermal synthesis of traditional non-layered metal sulfides is limited by the high reaction temperature, and it is difficult to effectively control the kinetic factors of the reaction, which is not conducive to the construction of nanocrystals with anisotropic structure.
In addition, the thermal synthesis process involves many reaction conditions, requiring a large number of experimental experiments, and the conditions required for different metal sulfides are different, so it is difficult to form a universal and effective synthesis method

Method used

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  • Unstratified metal sulfide nanosheet and preparation method thereof
  • Unstratified metal sulfide nanosheet and preparation method thereof
  • Unstratified metal sulfide nanosheet and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] A preparation method of non-layered lead sulfide nanosheets, comprising the steps of:

[0054] 1) Weigh 0.2 mmol of lead acetate and 0.4 mmol of n-dodecanethiol into a quartz flask, add 5 mL of oleylamine and 5 mL of oleic acid, and stir magnetically until a cloudy and uniform yellow solution is obtained.

[0055] 2) The above solution was heated in an oil bath at 75° C. for 30 min to obtain a clear and transparent yellow solution.

[0056] 3) Introduce argon gas into the clear and transparent yellow solution, and while heating at 75°C in an oil bath, select a 500W high-pressure mercury lamp as the light source for 4 hours of light, and then cool down to room temperature naturally to obtain a black turbid solution.

[0057] 4) Add toluene to the above black turbid solution and mix well, centrifuge at 6000 rpm for 5 minutes, repeat this process 5 times, and dry at 60-80°C for 12-24h to obtain non-layered PbS nanosheets .

[0058] figure 1 The middle curve is the XRD s...

Embodiment 2

[0063] Repeat Example 1, the difference is only that the metal salt is changed from lead acetate to cadmium chloride, oleic acid is changed to octadecene, and the heating temperature is changed from 75°C to 120°C.

[0064] Figure 4 The middle curve is the XRD spectrum of the CdS nanosheets prepared in Example 1.

[0065] Figure 5 The transmission electron microscope image of the CdS nanosheets prepared in Example 2.

[0066] Figure 6 High-resolution transmission electron microscope image of the CdS nanosheets prepared in Example 2.

[0067] Depend on Figure 4 It can be seen that only the peak of CdS crystal appears in the XRD spectrum of the synthesized CdS nanosheets, indicating that the synthesized product is a pure phase of CdS. Depend on Figure 5 It can be seen that only flaky products are observed in the TEM images of the synthesized CdS nanosheets, which also shows that the synthesized CdS is nanosheets. Depend on Figure 6 It can be seen that the synthesize...

Embodiment 3-4

[0069] Repeat Example 1, its difference is only to change mercaptan into octyl mercaptan or n-octyl mercaptan. The obtained PbS has a non-layered nanosheet structure.

[0070] Figure 7 , 8 Shown are the transmission electron micrographs of the PbS nanosheets synthesized in Examples 3 and 4. In the figure, the PbS products synthesized by using two kinds of alkyl chain thiols have only non-layered nanosheet structure, and no nanoparticles or other morphological products appear.

[0071] The experiment of the present invention proves that the length of the straight-chain alkylthiol under investigation has no obvious influence on the formation of sulfide nanosheets.

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Abstract

The invention discloses a preparation method of a unstratified metal sulfide nanosheet. The preparation method of the unstratified metal sulfide nanosheet comprises the following steps: dissolving metal salt and a sulfur source in an organic solvent, and uniformly mixing for reacting to obtain a first muddy solution; heating till the first muddy solution is clear and transparent, introducing inertia gas, performing an illumination reaction, and then cooling to room temperature to obtain a second muddy solution; washing, centrifugally separating and drying to obtain the unstratified metal sulfide nanosheet. The preparation method provided by the invention has the advantages of few raw material kinds, simple process, mild conditions, universality and controllable nanosheet appearance. Moreover, the unstratified metal sulfide nanosheet prepared by the method is small in thickness, being 1.2 to 9 nm, and has high anisotropy and crystallinity, and good application prospects.

Description

technical field [0001] The present invention relates to the field of metal sulfide synthesis. More specifically, it relates to a non-layered metal sulfide nanosheet and a preparation method thereof. Background technique [0002] Metal sulfides are a common class of semiconductors. Many common metal sulfides have wide band gaps, such as PbS, Cu 2 S, CdS, etc., therefore have good light absorption in the visible region or near ultraviolet region, and the appropriate band edge position makes these metal sulfides have excellent and efficient photoresponsive activity. When the metal sulfide in the bulk phase is made into a nanosheet structure, due to the quantum size effect, the electronic band structure of the metal sulfide changes significantly. All have great application value. [0003] For MoS 2 , SnS 2 And other partial sulfides, whose bulk phase is a layered material, and the layers are connected by relatively weak van der Waals force, so physical exfoliation can be u...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/20C01G11/02C01G19/00C01G21/21B82Y40/00
Inventor 张铁锐郭家昊曹溢涛
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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