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Method for preparing orthorhombic black phosphors monocrystals at low pressure

An orthorhombic, black phosphorus technology, applied in the field of optoelectronic semiconductor two-dimensional materials, can solve the problems of reduced black phosphorus purity, limited application, higher requirements for temperature control and red phosphorus raw materials, etc., to reduce the reaction time and optimize the reaction. temperature, the effect of simplifying the heating process

Inactive Publication Date: 2016-11-09
NANJING UNIV OF TECH
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  • Claims
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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 Snl 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 relatively high; in 2010, Cheol-Min Park used a high-energy ball mill to synthesize a composite material of red phosphorus and black phosphorus, but it is difficult to accurately control the pressure inside the reactor by high-energy ball milling and temperature, which affect the controllability of the preparation process
Therefore, the more commonly used synthesis methods are high temperature (1000) and high pressure (10kbar) methods, but these methods have extremely high requirements for experimental instruments.

Method used

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  • Method for preparing orthorhombic black phosphors monocrystals at low pressure
  • Method for preparing orthorhombic black phosphors monocrystals at low pressure
  • Method for preparing orthorhombic black phosphors monocrystals at low pressure

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preparation example Construction

[0014] The invention provides a method for preparing black phosphorus single crystal, wherein the method comprises: mixing phosphorus raw material, elemental Sn, and mineralizer Sn14, placing them in a quartz tube, vacuumizing and sealing at high temperature, and placing the sealed quartz tube in a In a Furnace, black phosphorus is prepared through a process of programmed heating and cooling. In the process of temperature programming, firstly, time t elapses from room temperature 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 above 450°C, preferably T 1 Higher than 535°C; time t 3 Relatively long, greater than 4 hours, T 3 greater than 416°C, preferably, T 3 Greater than 450°C; T 3 The process of lowering the temperature to room temperature is not limited, and it can be realized...

Embodiment 1

[0020] Add 1g of red phosphorus, 0.05g of tin, and 0.01g of tin iodide into the glass quartz tube, then vacuumize the quartz tube, and seal the quartz tube (inner diameter 1cm, length 10cm) when the vacuum reaches 1Pa. Then set the following heating program in the muffle furnace: room temperature-60min-650°C-120min-650°C-480min-500°C-room temperature.

[0021] The obtained black phosphorus has a conversion rate of 80% and is in the form of a block with a size of 0.8 cm×0.8 cm.

Embodiment 2

[0023] Add 2g of red phosphorus, 0.1g of tin, and 0.01g of tin iodide into the glass quartz tube, and then vacuumize the quartz tube. When the vacuum reaches 1Pa, package the quartz tube (inner 2cm, length 10cm). Then set the following heating program in the muffle furnace: room temperature-10min-450°C-120min-450°C-480min-416°C-room temperature.

[0024] The conversion rate of the obtained black phosphorus was 64.3%, which was in block shape with a small amount of flakes, and the size was 1.6cm×1.2cm.

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Abstract

The invention relates to a method for preparing orthorhombic black phosphors monocrystals. The method comprises the following steps: mixing a phosphorus raw material, elemental Sn and a mineralizer SnI4, placing the obtained mixture in a quartz tube, carrying out vacuum pumping and high temperature sealing, placing the sealed quartz tube in a muffle furnace, and carrying out optimized temperature programming and cooling to prepare black phosphorus. Black phosphorscrystals obtained in the invention have the advantages of large size, good crystallization performance and high purity, and the preparation method has the advantages of low device requirements, easy realization, and provision of great convenience for subsequent black phosphorus application and development.

Description

technical field [0001] The invention belongs to the field of photoelectric semiconductor two-dimensional materials, and in particular relates to a low-pressure 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 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/02C30B23/00
CPCC30B23/00C30B29/02
Inventor 闾敏王东亚谢小吉黄岭黄维
Owner NANJING UNIV OF TECH
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