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Method for preparing black phosphorus nanosheets

A technology for nanosheets and black phosphorus, applied in the field of preparing black phosphorus nanosheets, can solve the problems of difficulty in controlling thickness and size, uneven size and size of phosphorene, affecting the purity of black phosphorus sheets, etc. Efficiency, cost saving effect

Inactive Publication Date: 2018-12-18
深圳市中科墨磷科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process is difficult to control, the yield is low, and the size and size of the phosphorene obtained are not uniform. If phosphorene of a certain size needs to be used, further screening is required.
Although CN104779380A shows that its method can be customized in size and thickness, it can be seen from the numerical values ​​of its examples that the size and thickness of phosphorene prepared are a range value, so this expression is controversial, because the method adopts a simple The one-step constant current and constant voltage method is used for stripping, so it is difficult to achieve the effect of controlling the thickness and size, and the device does not isolate the two electrodes, and the other level of product is likely to affect or pollute the stripped black phosphorus electrode, affecting the black phosphorus obtained. Purity of slices

Method used

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  • Method for preparing black phosphorus nanosheets
  • Method for preparing black phosphorus nanosheets
  • Method for preparing black phosphorus nanosheets

Examples

Experimental program
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Effect test

Embodiment 1

[0046] A method for preparing black phosphorus nanosheets, comprising the steps of:

[0047] (1) Take the two electrode holders and wrap them with an electrical insulating film, respectively clamp 0.01g of black phosphorus crystals as the cathode and anode, and use N,N-dimethylformamide dissolved in tetrabutylammonium bromide as the electrolytic solution, the concentration of which is 0.5M, and assembled into an H-type electrolytic cell; using chronopotentiometry, the black phosphorus crystals are intercalated for 30 minutes under the condition of a current of 1mA; after the intercalation is completed, continue to use Current-time curve, under the condition of voltage 10V, the black phosphorus after intercalation is expanded for 10 minutes, and after the expansion is completed, black phosphorus with rough surface and doubled volume is obtained;

[0048] (2) Adopt 400 mesh filter screens to filter the expanded black phosphorus, then use N-methylpyrrolidone to wash the expanded ...

Embodiment 2

[0066] A method for preparing black phosphorus nanosheets, comprising the steps of:

[0067] (1) After taking two electrode holders and wrapping them with an electrical insulating film, respectively clamp 0.01g of black phosphorus crystals as cathode and anode, and use N,N-dimethylformamide dissolved with tetra-n-octyl ammonium bromide as Electrolyte solution with a concentration of 1.0M was assembled into an H-type electrolytic cell; cyclic voltammetry was used to cycle 10 times in the potential range of 0-3V at a scan rate of 5mV / s, and the black phosphorus crystal was intercalated for 60min ; After the intercalation is completed, continue to expand the intercalated black phosphorus for 34 minutes in the electrolyte by using linear sweep voltammetry, with a scanning potential range of -5 to 15V and a scanning speed of 5mV / s;

[0068] (2) Use a 400-mesh filter screen to filter the expanded black phosphorus, then wash the expanded black phosphorus with ethanol for 3 times, and...

Embodiment 3

[0085] A method for preparing black phosphorus nanosheets, comprising the steps of:

[0086] (1) Take two electrode clips and wrap them with an electrical insulating film, respectively clamp 0.01g of black phosphorus crystals as the working electrode and auxiliary electrode, and use the Ag / AgCl electrode as the reference electrode to dissolve tetrabutylamine hexafluorophosphate N,N-dimethylformamide was used as the electrolyte with a concentration of 0.5M, and an H-type electrolytic cell was assembled; using the current-time curve, the black phosphorus crystal was intercalated at a potential of -3V for 1h; the intercalation After completion, continue to use the same method in the electrolyte, and carry out expansion treatment on the black phosphorus after intercalation at a potential of -10V for 20 minutes;

[0087] (2) Use a 400-mesh filter to filter the expanded black phosphorus. After filtering, wash the expanded black phosphorus with tetrahydrofuran for 3 times. After wash...

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Abstract

The invention discloses a method for preparing black phosphorus nanosheets. The method comprises the following steps: (1) assembling black phosphorus used as an electrode and an organic solvent containing an intercalating agent, used as an electrolyte, in order to form an H-shaped electrolytic cell; (2) applying a current or voltage between the electrodes to intercalate and expand the black phosphorus; (3) filtering and washing the treated black phosphorus obtained in step (2), and carrying out ultrasonic vibration treatment on the treated black phosphorus in an organic solvent; and (4) centrifuging the obtained solution, and collecting the obtained supernatant to obtain a uniform-size black phosphorus nanosheet dispersion. The black phosphorus nanosheets stripped by the method have a thickness of 2-100 nm and a lateral dimension of 10 nm to 50 [mu]m. The method solves the problem of difficult control of the thickness and the lateral dimension of the black phosphorus nanosheets duringthe preparation of the black phosphorus nanosheets in the prior art, also solves the problem of too long time in traditional black phosphorus nanosheet preparation methods, and has the advantages of simple preparation process, low energy consumption, low cost, and realization of large-scale production.

Description

technical field [0001] The invention belongs to the preparation technology of inorganic nanometer materials, in particular to a method for preparing black phosphorus nanosheets. Background technique [0002] Black phosphorus is a crystal with metallic luster, which is black and has a flaky structure, especially black phosphorus with a wrinkled layered structure is the most attractive one among the allotropes of elemental phosphorus. Due to its excellent semiconductor properties, black phosphorus has become one of the most potential two-dimensional semiconductors after graphene and transition metal chalcogenides. Black phosphorus has a tunable direct band gap, and when the number and size of layers are appropriate, it has a high carrier mobility (up to 6.5×10 4 cm 2 / V.s), extremely large switching ratio characteristics (10 4 ~10 5 ) and obvious anisotropy; in addition, it also has good thermal conductivity, thermoelectric properties, photovoltaic effect, polarized light ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/02B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01B25/02
Inventor 喻学锋刘丹妮王佳宏黄浩
Owner 深圳市中科墨磷科技有限公司
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