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Large-area thin-layer high-quality black phosphorus nano-sheet and electrochemical stripping preparation method thereof

A high-quality, large-area technology, applied in chemical instruments and methods, preparation of phosphorus, phosphorus compounds, etc., can solve the problems of small size of few-layer black phosphorus nanosheets, not satisfying larger sizes, and residues on the surface of the sheet, etc. Achieve high stripping efficiency, maintain integrity and size, and low cost

Inactive Publication Date: 2020-02-21
SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

Ultrasonic liquid phase exfoliation is a method that can be used for large-scale preparation of black phosphorus nanosheets compared with micromechanical exfoliation, but this method can only obtain black phosphorus nanosheets with thinner layers by prolonging the ultrasonic time and increasing the ultrasonic power. The black phosphorus nanosheets prepared by this method are often severely oxidized under the action of long-term and high-power ultrasound, and the size of the few-layer black phosphorus nanosheets is small, which seriously hinders its application in the field of physics.
The current universal electrochemical liquid phase stripping method needs to be combined with ultrasonic treatment. The sheet obtained by it meets the requirement of few layers, but does not meet the requirement of large size, and due to the strong polarity of the stripping electrolyte propylene carbonate (PC), resulting in PC Too much residue on the surface of the sheet will affect subsequent device processing

Method used

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  • Large-area thin-layer high-quality black phosphorus nano-sheet and electrochemical stripping preparation method thereof
  • Large-area thin-layer high-quality black phosphorus nano-sheet and electrochemical stripping preparation method thereof
  • Large-area thin-layer high-quality black phosphorus nano-sheet and electrochemical stripping preparation method thereof

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[0028] An aspect of the embodiments of the present invention provides a method for preparing large-area thin-layer high-quality black phosphorus nanosheets by electrochemical stripping, which includes:

[0029] Use black phosphorus as the working electrode, and at least construct an electrochemical reaction system together with the counter electrode and the electrolyte, wherein the electrolyte contains tetrabutylammonium ions (TBA + ) in acetonitrile;

[0030] The working electrode and the counter electrode are electrically connected to the negative pole and the positive pole of the power supply respectively, so that a selected voltage is applied between the working electrode and the counter electrode, and then peeled off from the black phosphorus to obtain a large-area thin layer of high-quality black phosphorus. Phosphorus nanosheets.

[0031] In some preferred solutions, the concentration of the acetonitrile solution containing tetrabutylammonium ions during the electroche...

Embodiment 1

[0057] Example 1 Electrochemical exfoliation of bulk BP crystals

[0058] Such as figure 1 As shown in the schematic diagram of the electrochemical stripping black phosphorus device in China, select a BP block with a size of cubic centimeters, wrap it with platinum wire and clamp it on the platinum electrode clip as the working electrode, and use a pure platinum electrode parallel to the working electrode as the counter electrode at the other end , the distance between the two electrodes can be adjusted according to the required voltage, and the distance is 1-2 cm, preferably 1.5 cm. First, prepare 0.5-2mol / L (preferably 1mol / L) acetonitrile solution of tetrabutylammonium bisulfate, soak the electrode and the block into the solution respectively, and connect the current flowing from the negative electrode of the workstation to the electrode connected to the BP block superior. After the black phosphorus block is completely soaked in the electrolyte, apply a voltage of 10V to ...

Embodiment 2

[0061] This example is basically the same as Example 1, except that tetrabutylammonium bisulfate is replaced by n-butylammonium tetrafluorophosphate. After testing, please refer to the SEM image of the black phosphorus nanosheets obtained in this embodiment image 3 .

[0062] It can be seen from Examples 1-2 that the innovation of the present invention lies in the discovery that the electrochemical stripping effect of the two-dimensional material is related to whether the ionic radius of the electrolyte in the electrolyte matches the interlayer distance of the two-dimensional material. In the process of stripping black phosphorus, the synergistic effect of n-butylammonium ion and acetonitrile is used. The influence of n-butyl ammonium ion on the stripping process, that is, high-efficiency and large-area stripping, and the influence of acetonitrile on the stripping effect, that is, the cleanliness of the sheet obtained by stripping.

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Abstract

The invention discloses a large-area thin-layer high-quality black phosphorus nano-sheet and an electrochemical stripping preparation method thereof. The preparation method comprises: taking black phosphorus as a working electrode, and at least constructing an electrochemical reaction system with a counter electrode and an electrolytic solution, wherein the electrolytic solution is an acetonitrilesolution containing tetrabutylammonium ions; and respectively and electrically connecting the working electrode and the counter electrode with a negative electrode and a positive electrode of a powersupply so as to apply a selected voltage between the working electrode and the counter electrode, so that large-area thin-layer high-quality black phosphorus nano-sheets are strip from the black phosphorus. Compared with the black phosphorus nano-sheet in the prior art, the black phosphorus nano-sheet prepared by the electrochemical stripping method of the invention has the following characteristics that the yield is high, the stripped few-layer black phosphorus film is high in proportion, large in area and low in oxygen content, and the preparation process is simple, low in cost, high in safety and suitable for mass production.

Description

technical field [0001] The invention relates to the preparation of black phosphorus nanosheets, in particular to a method for obtaining large-area thin-layer high-quality black phosphorus nanosheets based on an electrochemical method, and belongs to the technical field of nanomaterial preparation. Background technique [0002] Two-dimensional materials such as graphene have been favored by researchers because of their unique physical and chemical properties and wide range of applications. In recent years, the high carrier mobility of black phosphorus (BP) (~1000cm 2 / Vs), high switching ratio (>10 5 ) and tunable direct bandgap (0.3-2eV) with the number of layers, which makes up for the performance defects of graphene's zero bandgap and TMDs carrier mobility, and shows great promise in the application of new optoelectronic devices. potential. Similar to other two-dimensional materials, there is a weak van der Waals force between BP layers, so the exfoliation of layered...

Claims

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Application Information

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IPC IPC(8): C01B25/02C01B25/00B82Y40/00
CPCB82Y40/00C01B25/003C01B25/02
Inventor 张凯杨泽园
Owner SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI
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