Low-temperature Electrochemical-assisted Preparation Of Nano-black Phosphorus And Its Formation Mechanism

Nano-black phosphorus has a good application prospect in energy storage,catalysis,biomedicine,sensors,solar cells and other fields,and how to effectively prepare nano-black phosphorus is the key to its application.In addition,the research shows that the nano-black phosphorus with different structure and morphology will have different properties and application fields.Therefore,the development of nano-black phosphorus with different structure and morphology is expected to improve the performance of nano-black phosphorus and broaden its application field.At the same time,with the nanometer of black phosphorus,its oxidizability also increases.In this paper,the efficient preparation of nano-black phosphorus and the formation mechanism of nano-black phosphorus with different morphologies were studied.A new efficient preparation method of nano-black phosphorus was developed.The oxidation of nano-black phosphorus was inhibited at low temperature,and nano-black phosphorus with different morphologies holey phosphorene and black phosphorus quantum dots were prepared.The formation mechanism of nano-black phosphorus with different morphologies was studied by comparing the control conditions.The specific research contents are as follows:（1）Holey phosphorene was prepared by low-temperature electrochemically-assisted stripping.The AFM,TEM,XPS,UV-vis,Raman and other technologies were used to characterize and analyze the holey phosphorene,and the photocatalytic performance of ammonia synthesis of holey phosphene was studied.The results of related studies show that the pore size of holey phosphorene is several nanometers to tens of nanometers,with a thickness of 1 to 4 nm（about 1 to 4 layers thick）,has certain photocatalytic properties for ammonia synthesis.The UV-vis absorption spectrum results show that the trend of the ultraviolet spectrum of holey phosphorene compared with ordinary black phosphorene is different,indicating that different forms of nano black phosphorus have different properties.This method uses low temperature to suppress oxidation.Holey phosphene is prepared by ion intercalation and attack.Compared with other methods,the whole process takes less time（about 1 h）.（2）Black phosphorus quantum dots were prepared by low-temperature electrochemically-assisted stripping.TEM,AFM,XPS,Raman,UV-vis and other technologies were used to characterize and analyze the prepared black phosphorus quantum dots.The results show that the lateral size of the black phosphorus quantum dots is several nanometers to several tens of nanometers,and the thickness is 1-10 nm（about 1to10 layers thick）,the stability in air is better than that holey phosphorene.（3）Aiming at the problem of obtaining nano-black phosphorus with different morphologies under different preparation conditions,it is conjectured that the conductivity and metal ions may affect the morphology of nano-black phosphorus,so four sets of comparative experiments were designed for comparison.It was found that from the perspective of conductivity,conductivity can change the size of nano-black phosphorus,and the higher the conductivity,the smaller the black phosphorus,but the conductivity cannot change the morphology of nano-black phosphorus,and When Cu²⁺is involved in the reaction,holey phosphorene can be obtained.