Preparation method and application of black phosphorus nanosheets
A nanosheet, black phosphorus technology, applied in nanotechnology, chemical instruments and methods, phosphorus and other directions, can solve the problems of poor peeling quality, low peeling efficiency, high peeling cost, etc., achieve large size, simple and efficient peeling process, high The effect of stability
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[0052] A kind of preparation method of black phosphorus nanosheet provided by the invention comprises:
[0053] In step R1, a black phosphorous crystal block is synthesized in a reaction device.
[0054] The reaction device has a connected raw material end and a product end; preferably, the raw material end and the product end are relatively connected. The reaction device may be, for example, a quartz tube or the like.
[0055] Specifically, first, a substrate coated with an Au film is placed on the product side.
[0056] The Au film may have any thickness, but an increase in the thickness of the Au film means an increase in production cost, and therefore, an Au film with a thickness of 10 nm to 500 nm is preferable.
[0057] Then, red phosphorus, tin and tin iodide are placed on the raw material end according to the mass ratio of 450~550:15~25:5~15, and heat treatment is carried out to control the temperature of the raw material end higher than the product end, and keep the...
Embodiment 1
[0096] This embodiment provides a method for preparing black phosphorus nanosheets, comprising the steps of:
[0097] In step R1, a layer of Au film with a thickness of 100 nm was deposited on the silicon substrate, and then 100 mg of red phosphorus, 40 mg of tin and 20 mg of SnI were mixed at 750 °C 4 The raw material end of the quartz tube is loaded, the silicon substrate deposited with the Au film is loaded into the product end of the quartz tube, and the quartz tube is vacuum sealed, wherein the raw material end and the product end are opposite ends of the quartz tube. Then place the quartz tube horizontally in the tube furnace, set the temperature rise and fall program for heating and growth, and finally obtain the black phosphorus crystal block.
[0098] Wherein, the heating and cooling program of growing black phosphorus crystal block is:
[0099] From room temperature to 750°C, the heating time is 180min, and the temperature is maintained at 750°C for 60min; then from...
Embodiment 2
[0114] Put the silicon substrate deposited with the Au film into a quartz tube with an outer diameter of 10mm and a wall thickness of 1mm, and put red phosphorus, tin powder and tin tetraiodide into the quartz tube according to the mass ratio of 25:1:0.6 In the process, the quartz tube was vacuum-sealed to 10 by using a molecular pump unit and a hydrogen-oxygen flame. -2 Pa, the content of the mixed ingredients in the quartz tube is 15mg / cm 3 ~30mg / cm 3 .
[0115] Put the sealed quartz tube horizontally into the heating zone of the tube furnace, set the temperature in the furnace, first heat the furnace to 750°C at a speed of 5°C / min, and keep it at 750°C for 3 hours, then within 5 hours The furnace was cooled to 500 °C and held at this temperature for a further 4 h.
[0116] Then it was further slowly cooled to room temperature within 3 hours, and black phosphorus crystals were obtained at the cold end of the quartz glass tube.
[0117] With reference to the electrochemic...
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Abstract
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