US 12,291,449 B2
Black phosphorus nanosheet, preparation method therefor, and application thereof
Jie Chen, Nanjing (CN); Yanhua Luo, Nanjing (CN); Xiaodong Pei, Nanjing (CN); Fan Wang, Nanjing (CN); Fenglin Tang, Nanjing (CN); Yefeng Zhu, Nanjing (CN); Baojin Shen, Nanjing (CN); Xiuguang Yang, Nanjing (CN); and Ling Zhang, Nanjing (CN)
Assigned to SINOSTEEL NANJING ADVANCED MATERIALS RESEARCH INSTITUTE CO., LTD., Nanjing (CN)
Appl. No. 17/763,153
Filed by SINOSTEEL NANJING ADVANCED MATERIALS RESEARCH INSTITUTE CO., Ltd., Nanjing (CN)
PCT Filed Jun. 2, 2020, PCT No. PCT/CN2020/093829
§ 371(c)(1), (2) Date Mar. 23, 2022,
PCT Pub. No. WO2021/237763, PCT Pub. Date Dec. 2, 2021.
Claims priority of application No. 202010461825.9 (CN), filed on May 27, 2020.
Prior Publication US 2023/0075308 A1, Mar. 9, 2023
Int. Cl. C01B 25/02 (2006.01); B82Y 30/00 (2011.01); B82Y 40/00 (2011.01)
CPC C01B 25/02 (2013.01) [B82Y 30/00 (2013.01); B82Y 40/00 (2013.01)] 15 Claims
 
1. A method of preparing a black phosphorous nanosheet, the method comprising:
preparing an alkaline aqueous electrolyte by:
1) preparing 0.1˜2 mol/L of a sulfate solution A and 0.1˜2 mol/L of a sulfate solution B, adding an alkaline solution to the sulfate solution B to adjust the pH value of sulfate solution B to 8˜14, and mixing evenly to obtain an alkaline aqueous electrolyte C, and
2) preparing an N-N dimethylformamide solution in which an epoxy resin is dissolved;
performing an electrochemical reaction in a constant temperature environment of 0˜10° C., with a black phosphorus sheet as an anode, an inert electrode as a cathode, and the sulfate solution A as an electrolyte, and a surface current density of 200˜500 mA/dm2 under a DC voltage of 2.5˜3.5V for 1˜3 h;
transferring the anode and the cathode to the alkaline aqueous electrolyte C, and adding the N-N dimethylformamide solution with dissolved epoxy resin to the alkaline aqueous electrolyte C; and
applying a voltage of 5˜10V between the anode and the cathode, wherein the distance between electrodes remains unchanged, the area current density is controlled at 600˜900 mA/dm2, and precipitating black phosphorus for the black phosphorous nanosheet at the bottom of the alkaline aqueous electrolyte C for 0.5˜1.5 h.