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Small-sized black phosphorus flakes and preparation method thereof

A technology of small-sized black phosphorus flakes, which is applied in the field of small-sized black phosphorus flakes and its preparation, can solve the problems of low yield of flake black phosphorus, large material size, and small amount of black phosphorus flakes, and achieve uniform size and large size. Controllable, good monodispersity effect

Active Publication Date: 2016-05-25
HUBEI MOPHOS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the yield of flaky black phosphorus prepared by mechanical exfoliation is low, which is not suitable for the production of commercially applicable materials, and the operation is cumbersome, time-consuming, and the size of the obtained materials is relatively large, mostly in the micron scale; while chemical vapor deposition The amount of black phosphorus flakes prepared by the method is very small, and it is not easy to repeat

Method used

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  • Small-sized black phosphorus flakes and preparation method thereof
  • Small-sized black phosphorus flakes and preparation method thereof
  • Small-sized black phosphorus flakes and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] A preparation method of small-sized black phosphorus sheet, comprising the steps of:

[0058] Weigh 25 mg of black phosphorus block in a nitrogen-filled glove box, grind it and disperse it into 25 mL of N-methylpyrrolidone, seal to obtain a 1 mg / ml dispersion; ultrasonicate for 3 hours at 1200 W probe ultrasonic power , and then 10 hours of ultrasonication in a water bath with a power of 300W. The entire ultrasonication process is controlled below 277K by an ice bath; then centrifuged at a speed of 7000 rpm for 20 minutes. Small size black phosphorus flakes in N-methylpyrrolidone.

[0059] The product obtained in present embodiment 1 is characterized, and the results are as follows Figure 1 ~ Figure 3 As shown, among them, figure 1 It is the ultraviolet-visible-near-infrared absorption spectrogram of small-sized black phosphorus sheet in N-methylpyrrolidone solution; figure 2 It is a low-magnification transmission electron microscope picture of a small-sized black ...

Embodiment 2

[0061] A preparation method of small-sized black phosphorus sheet, comprising the steps of:

[0062] Weigh 15 mg of black phosphorus block in a nitrogen-filled glove box, grind it and disperse it into 25 mL of N-methylpyrrolidone, seal it, and obtain a 0.6 mg / ml dispersion; Hours, and then followed by 400W power of water bath ultrasonic 8 hours, the whole ultrasonic process is controlled by ice bath to complete below 277K; then centrifuged at 5000 rpm speed, centrifugation time is 20 minutes, take the supernatant, Obtain small size black phosphorus flakes.

Embodiment 3

[0064] A preparation method of small-sized black phosphorus sheet, comprising the steps of:

[0065] Weigh 30 mg of black phosphorus block in a nitrogen-filled glove box, grind and disperse it into 25 mL of dimethyl sulfoxide, seal it to obtain a 1.2 mg / ml dispersion; ultrasonicate under 1000 W probe type ultrasonic power 4 hours, followed by 100W water bath ultrasonication for 12 hours, the entire ultrasonic process is controlled below 277K by ice bath; then centrifuged at 9000 rpm for 10 minutes, the supernatant was taken, Obtain small size black phosphorus flakes.

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Abstract

The invention provides a preparation method of small-sized black phosphorus flakes. The preparation method comprises the following steps: under the condition that air is isolated, grinding black phosphorus, and dispersing the ground black phosphorus into a first organic solvent to obtain a dispersion at the concentration of 0.6-1.2mg / mL; performing probe-type ultrasonic treatment to the dispersion for 2-4h under the power of 1000-1400W first and then performing water-bath ultrasonic treatment for 8-12h under the power of 200-400W; after the ultrasonic treatment, centrifuging and collecting a supernatant, namely the stripped small-sized black phosphorus flakes. The preparation method is simple in process, easy to operate, relatively high in yield, good in reproducibility, easy to realize low-cost industrial production of the small-sized black phosphorus flakes, and free of secondary pollution to the environment. The invention further provides the small-sized black phosphorus flakes.

Description

technical field [0001] The invention relates to the field of novel nanomaterials, in particular to a small-sized black phosphorus sheet and a preparation method thereof. Background technique [0002] Black phosphorus has a natural wrinkled structure similar to but different from the graphene sheet structure. This unique wrinkled structure leads to many unique physical properties of black phosphorus. For example, black phosphorus has semiconductor gaps that graphene does not have and is directly banded. Gap, that is, the bottom of the electronic conduction energy band (conduction band) and the top of the non-conduction energy band (valence band) are at the same position, to achieve conduction from non-conduction to conduction, the electronic value requires absorption capacity, which means that black phosphorus can be used as a tunable semiconductor , can be directly coupled with light, and the spectrum includes the entire visible light to the near-infrared region. Therefore,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/02B82Y30/00
CPCB82Y30/00C01B25/02C01P2004/04C01P2004/64
Inventor 喻学锋韩卫家谢寒寒孙正博
Owner HUBEI MOPHOS TECH CO LTD
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