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Preparation method of transition metal disulfide quantum chip

A technology of transition metals and transition metal elements, which is applied in the field of preparation of transition metal dichalcogenide quantum chips, can solve the problems of complicated process, difficult to meet large-scale production, and difficult operation, so as to achieve simple and easy operation of the process and realize large-scale The effect of large-scale production and a wide range of sources

Inactive Publication Date: 2017-03-08
THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN105129748A adopts a "bottom-up" strategy to prepare transition metal dichalcogenide quantum dots. Although it has good versatility, its reaction conditions are relatively harsh, requiring a strict inert gas environment and 280-350 ° C. The reaction temperature is high, and at the same time, more toxic raw materials are used, such as trioctylphosphine oxide and metal carbonyl compounds, etc.
The use of hydrogen peroxide makes the product complicated, and the deep ultraviolet LED lamp will bring additional costs, which is not suitable for mass production
[0005] So far, the preparation methods of transition metal dichalcogenide quantum dots reported in the literature and patents all have the following common problems: such as high cost, complicated process, high toxicity of raw materials, difficult operation, etc., and low yield , it is difficult to meet the needs of mass production

Method used

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  • Preparation method of transition metal disulfide quantum chip
  • Preparation method of transition metal disulfide quantum chip
  • Preparation method of transition metal disulfide quantum chip

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] 1 g of MoS with an average size of 5 μm 2 , 1g of sodium chloride and 10g of agate balls with a diameter of 0.5mm are mixed, and ball milled for 0.5h. The agate balls were then separated, and the resulting sample was washed with water several times until the sodium chloride was completely washed out. After drying, N-methylpyrrolidone (NMP) was added, and ultrasonic power of 50 W was used for 120 h. The ultrasonic sample was first centrifuged at 500r / min for 120min, then vacuum filtered, and passed through a filter membrane with a pore size of 0.02μm to obtain MoS 2 NMP dispersion of quantum flakes.

[0056] The resulting MoS 2 The NMP dispersion of the quantum sheet was dried, and the obtained powder had a mass of 0.198g, and the calculated MoS 2 The final yield of quantum flakes was 19.8%.

[0057] figure 1 MoS in Example 1 2 Scanning electron micrographs of raw materials. Depend on figure 1 It can be seen that the size thereof is 1-10 μm, and the average size...

Embodiment 2

[0061] 0.1 g of WS with an average size of 2 μm 2 , 10g of potassium sulfate and 10g of stainless steel balls with a diameter of 20mm were mixed, and ball milled for 120h. Then the stainless steel balls were separated, and the obtained samples were washed with water several times until the potassium sulfate was completely washed out. After drying, NMP was added, and ultrasonic power of 1000W was used for 0.5h. The ultrasonic sample is first centrifuged at 10000r / min for 1min, then vacuum filtered, and passed through a filter membrane with a pore size of 0.02μm to obtain WS 2 NMP dispersion of quantum flakes.

[0062] The resulting WS 2 The NMP dispersion of the quantum sheet is dried, and the powder mass obtained is 0.0211g, and the calculated WS 2 The final yield of quantum flakes was 21.1%.

[0063] Figure 4 WS in Example 2 2 Scanning electron micrographs of raw materials. Depend on Figure 4 It can be seen that the size thereof is 1-10 μm, and the average size is ...

Embodiment 3

[0065] 0.01 g of MoSe with an average size of 100 μm 2, 0.1g of calcium carbonate and 5g of zirconia balls with a diameter of 6mm were mixed, and ball milled for 20 hours. Then the zirconia balls were separated, and the obtained sample was washed with hydrochloric acid for many times until the calcium carbonate was completely washed away, and then washed with water for many times to completely wash away the residual hydrochloric acid. After drying, dimethyl sulfoxide (DMSO) was added and ultrasonicated at 200 W for 5 h. The ultrasonic sample was first centrifuged at 5000r / min for 20min, then vacuum filtered, and passed through a filter membrane with a pore size of 0.02μm to obtain MoSe 2 DMSO dispersion of quantum flakes.

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Abstract

The invention relates to a preparation method of a transition metal disulfide quantum chip. The preparation method includes: mixing transition metal disulfide raw materials, auxiliary inorganic matter and ball milling balls, performing ball milling, removing the ball milling balls and the inorganic matter, and performing ultrasonic dispersing on the product to obtain the even and stable dispersing liquid of the transition metal disulfide quantum chip. Compared with the prior art, the preparation method has the advantages that the method is rich in raw material source, efficient, environmentally friendly, simple to operate and the like, and the prepared transition metal disulfide quantum chip keeps intrinsic characteristics, extremely few in defects, extremely high in yield and suitable for being prepared in a large-scale manner.

Description

technical field [0001] The invention relates to the technical field of preparation of inorganic nanometer materials, in particular to a preparation method of transition metal dichalcogenide quantum sheets. Background technique [0002] Transition metal dichalcogenides (TMDs) refer to compounds of the X-M-X structure formed by transition metal elements (M) and chalcogen nonmetal elements (X), where transition metal elements mainly refer to IVB, VB, VIB in the periodic table of elements , VIIB, VIII transition metals, chalcogen non-metallic elements mainly refer to S, Se, Te and other elements. Transition metal dichalcogenides have a layered structure similar to graphite, in which the transition metal atoms and chalcogen atoms in the layers are combined by chemical bonds, while the interlayers are combined by weak van der Waals forces. Typical transition metal dichalcogenides include MoS 2 、MoSe 2 、MoTe 2 、WS 2 、WSe 2 、TiS 2 、TaS 2 , VS 2 , FeS 2 Wait. [0003] Tran...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/06C01G41/00C01B19/04B82Y30/00B82Y40/00
CPCC01G39/06B82Y30/00B82Y40/00C01B19/04C01G41/00C01P2004/03C01P2004/04C01P2004/64
Inventor 张勇韩春春徐元清
Owner THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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