Method for preparing orthorhombic crystal system black phosphorus single crystal

A technology of orthorhombic system and black phosphorus, which is applied in the field of optoelectronic semiconductor two-dimensional materials, can solve the problems of black phosphorus purity reduction, limited application, temperature control and high requirements for red phosphorus raw materials, etc., to optimize the reaction temperature and simplify the heating process , the effect of shortening the reaction time

Inactive Publication Date: 2017-03-15
NANJING UNIV OF TECH
View PDF8 Cites 11 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the highly toxic and pyrophoric properties of white phosphorus limit the application of these methods
In 2007, Nilges, Tom utilized Au, Sn and SnI 4 As a combined catalyst, red phosphorus is heated to 600°C in a vacuum environment to obtain black phosphorus, but the introduction of noble metals increases the production cost and the purity of black phosphorus decreases; CA105133009A, CA105460910 and CA105565289 also published improvements to this method , but the requirements for temperature control and red phosphorus raw materials are higher, and the catalyst selection has certain limitations (only limited to Au, Sn, l 2 or their mutual reaction products) and have not been reused; in 2010, Cheol-Min Park used a high-energy ball mill to synthesize a composite material of red phosphorus and black phosphorus, but the high-energy ball mill method is difficult to accurately control the pressure and temperature inside the reactor , affecting the controllability of the preparation process
Therefore, the more commonly used synthesis methods are high-pressure (10kbar) methods, but these methods have extremely high requirements for experimental instruments.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for preparing orthorhombic crystal system black phosphorus single crystal
  • Method for preparing orthorhombic crystal system black phosphorus single crystal
  • Method for preparing orthorhombic crystal system black phosphorus single crystal

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0014] The invention provides a method for preparing a black phosphorus single crystal, wherein the method comprises: mixing phosphorus raw materials, metal indium, and tin iodide, placing them in a reactor, removing oxygen from the reactor and then sealing it, and heating and cooling through a program Process for preparing black phosphorus. Among them, tin iodide is SnI 4 , SnI 2 Or a mixture of the two; the removal of oxygen can be achieved by vacuuming or exhausting the air with an inert gas; 1 Warming up to the sublimation temperature T 1 , after time t 2 down to the initial crystallization temperature T 2 , the elapsed time t 3 reaches the crystallization termination temperature T 3 . where time t 1 , t 2 Not limited, T 1 Greater than or equal to 450°C, preferably T 1 Greater than or equal to 535°C; time t 3 Relatively long, greater than 4 hours, T 3 Greater than or equal to 416°C, preferably, T 3 Greater than or equal to 450°C; T 3 The process of lowering ...

Embodiment 1

[0020] 0.3g red phosphorus, 0.02g metal indium, 0.01g SnI 4 Put into the glass quartz tube, then vacuumize the quartz tube, when the vacuum degree reaches 1Pa, package the quartz tube (inner diameter 1cm, length 10cm). React according to the following heating program: room temperature-60min-535°C-30min-450°C-480min-416°C-room temperature, and the cooling process adopts a natural cooling method.

[0021] The obtained black phosphorus has a conversion rate of 52% and is in the shape of a block with a size of about 0.5 cm×0.4 cm.

Embodiment 2

[0023] 0.3g red phosphorus, 0.1g metal indium, 0.01g SnI 2 Put into the glass quartz tube, then vacuumize the quartz tube, when the vacuum degree reaches 1Pa, package the quartz tube (inner diameter 1cm, length 10cm). React according to the following heating program: room temperature-60min-535°C-30min-450°C-480min-416°C-room temperature.

[0024] The obtained black phosphorus has a conversion rate of 60% and is in the form of a block with a size of about 0.6cm×05cm.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
carrier mobilityaaaaaaaaaa
Login to view more

Abstract

The invention relates to a preparation method of an orthorhombic crystal system black phosphorus single crystal. The preparation method comprises the following steps: mixing phosphorus raw materials, metallic indium and stannic iodide; putting in a reactor; tightly sealing; preparing black phosphorus by improving and reducing the temperature through optimized procedures. The obtained black phosphorus is good in crystallization property and high in purity; in addition, the catalyst can be repeatedly used; a preparation process is low in requirement on equipment and easy for realization, and provides great convenience for subsequent application and development of the black phosphorus.

Description

technical field [0001] The invention belongs to the field of photoelectric semiconductor two-dimensional materials, and in particular relates to a preparation method of orthorhombic black phosphorus material. Background technique [0002] The rapid development of the semiconductor electronics industry has put forward higher requirements for the development of materials. Graphene has ushered in the era of two-dimensional materials, with its ultra-high carrier mobility (15000cm 2 / V*s) and other superior physical and chemical properties make it considered the most likely material to replace silicon, but the zero band gap limit the development of graphene. Similar to graphene, black phosphorus is a single-element two-dimensional material with van der Waals force between layers, and flake crystals with different layers can be obtained by exfoliation. Black phosphorus not only has graphene-like ultra-high carrier mobility (200~50000cm 2 / V*s), and its bandgap can be adjusted b...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/02C30B23/00
CPCC30B29/02C30B23/00
Inventor 闾敏王东亚谢小吉黄岭黄维
Owner NANJING UNIV OF TECH
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products