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Preparation method for orthorhombic crystal system black phosphorus monocrystalline

A technology of orthorhombic system and black phosphorus, which is applied in the field of preparation of orthorhombic black phosphorus single crystal, can solve the problems of high cost, harmful to human body, difficult industrial application, etc., and achieve low cost, high yield and high operation safety effect

Active Publication Date: 2015-12-09
BEIJING FUZHI CHUANGZHAN BUSINESS MANAGEMENT
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

[0003] CN104310326A discloses a method for preparing black phosphorus single crystals using red phosphorus, AuSn and tin tetraiodide as raw materials. However, this method relies on highly toxic and expensive metals and their compounds as catalysts, which is costly and harmful to the human body. Difficult to apply industrially

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  • Preparation method for orthorhombic crystal system black phosphorus monocrystalline
  • Preparation method for orthorhombic crystal system black phosphorus monocrystalline
  • Preparation method for orthorhombic crystal system black phosphorus monocrystalline

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preparation example Construction

[0014] The invention provides a method for preparing an orthorhombic black phosphorus single crystal, wherein the method comprises: making red phosphorus , metal tin and iodine simple substance are carried out contact reaction in the first area of ​​reaction system, wherein, in described contact reaction process, the temperature of the first area of ​​described reaction system is raised to 550-800 ℃, described reaction system The temperature of the second zone of the reaction system is raised to 400-700° C., and the temperature of the first zone of the reaction system is raised to a higher temperature than that of the second zone of the reaction system.

[0015] According to the present invention, the red phosphorus can be understood as the precursor for preparing the orthorhombic black phosphorus single crystal, and the present invention has no special limitation on the red phosphorus, in order to improve the The yield, preferably, the phosphorus element content of the red ph...

Embodiment 1

[0038] This example is used to illustrate the preparation method of the orthorhombic black phosphorus single crystal of the present invention.

[0039] 500mg of red phosphorus (P element content is 99.999% by weight, in sheet form, purchased from AlfaAesar company, the same below), 1500mg of metal tin (Sn element content is 99.999% by weight, in granular form, particle size is 1-2mm , purchased from AlfaAesar Company, hereinafter the same) and 500mg of iodine element (the iodine element content is 99.99% by weight, is a crystal, and the particle size is 1-2mm, purchased from AlfaAesar Company, hereinafter the same) and fully mixes and pours into a long about 13cm One end of the quartz tube (about 7mL in volume) is evacuated to a pressure of about 1 Pa in the quartz tube, and the quartz tube is sealed. Place one half of the raw material end of the sealed quartz tube in the high temperature zone of the dual temperature zone furnace (MTI company OTF-1200X model, the same below), ...

Embodiment 2

[0042] This example is used to illustrate the preparation method of the orthorhombic black phosphorus single crystal of the present invention.

[0043] Thoroughly mix 500mg of red phosphorus, 1000mg of metallic tin and 250mg of iodine, and pour it into one end of a 13cm-long quartz tube (volume is about 7mL), vacuumize the quartz tube to a pressure of about 1Pa, and seal the quartz tube. One half section of the raw material end in the sealed quartz tube is placed in the high temperature zone of the dual temperature zone furnace body, and the remaining half section is placed in the low temperature zone of the dual temperature zone furnace body. The high temperature zone was heated from room temperature (about 25°C) to 700°C at a rate of 67.5°C / h, while the low temperature zone was heated from room temperature (about 25°C) to 550°C at a rate of 52.5°C / h, and kept for 8 hours. Then the temperature in the high temperature zone was lowered to 350°C at a rate of 43.75°C / h, while the...

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Abstract

The invention discloses a preparation method for an orthorhombic crystal system black phosphorous monocrystalline. The method comprises the following steps: carrying out a contact reaction on red phosphorus, metallic tin and elementary iodine in a first area of a reaction system under a vacuum condition in the reaction system in which the first area and a second area are mutually communicated, wherein in the contact reaction process, the temperature of the first area of the reaction system is raised to 550 to 800 DEG C, the temperature of the second area of the reaction system is raised to 400 to 700 DEG C, and the temperature of the first area of the reaction system is raised to the temperature higher than that of the second area of the reaction system. The method disclosed by the invention can be used for preparing the orthorhombic crystal system black phosphorus monocrystalline at a relatively low cost and relatively high operation safety, in particular to large-size and high-quality orthorhombic crystal system black phosphorous monocrystalline at a relatively high yield.

Description

technical field [0001] The invention relates to a preparation method of orthorhombic black phosphorus single crystal. Background technique [0002] Elemental phosphorus has four allotropes, namely: white phosphorus, red phosphorus, purple phosphorus and black phosphorus. Black phosphorus has been confirmed to exist in three crystal systems, namely orthorhombic, trigonal and cubic. Among them, the orthorhombic black phosphorus single crystal is a direct band gap semiconductor (band gap is 0.3eV), and its structure is a layered structure very similar to two-dimensional materials such as graphene and molybdenum disulfide. force combined. Orthorhombic black phosphorus single crystal has excellent electron and hole mobility, which can realize the on and off of logic circuits, and electrons and photons show a high degree of anisotropy in the layered plane, making orthorhombic black phosphorus Single crystals have important application value in the fields of electronics and opto...

Claims

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Application Information

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IPC IPC(8): C30B29/02C30B1/10
Inventor 严清峰张子明
Owner BEIJING FUZHI CHUANGZHAN BUSINESS MANAGEMENT
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