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
  • Description
  • Claims
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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

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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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[0014] The present invention provides a method for preparing an orthorhombic black phosphorous single crystal, wherein the method includes: in a reaction system provided with a first region and a second region communicating with each other, and under vacuum conditions, making the red phosphorous , Metal tin and iodine are in contact reaction in the first zone of the reaction system, wherein during the contact reaction, the temperature of the first zone of the reaction system is increased to 550-800°C, and the 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 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. The invention does not specifically limit the red phosphorus, in order to impro...

Example Embodiment

[0037] Example 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 the form of flakes, purchased from AlfaAesar Company, the same below), 1500mg metal tin (Sn element content is 99.999% by weight, in granular form, with a particle size of 1-2mm , Purchased from AlfaAesar Company, the same hereinafter) and 500mg of iodine element (the iodine content is 99.99% by weight, crystals, the particle size is 1-2mm, purchased from AlfaAesar Company, the same hereinafter) mixed thoroughly and poured into a length of about 13cm One end of the quartz tube (volume about 7 mL) is evacuated until the pressure inside the quartz tube is about 1 Pa, and the quartz tube is sealed. Place one half section of the raw material end of the sealed quartz tube in the high temperature zone of the dual temperature zone furnace body (MTI Comp...

Example Embodiment

[0041] Example 2

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

[0043] Mix 500 mg of red phosphorous, 1000 mg of metallic tin, and 250 mg of iodine, and then pour it into one end of a 13 cm long quartz tube (about 7 mL), evacuate until the pressure inside the quartz tube is about 1 Pa, and seal the quartz tube. One half of the raw material end of the sealed quartz tube is placed in the high temperature zone in the dual temperature zone furnace body, and the remaining half is placed in the low temperature zone in the dual temperature zone furnace body. The high temperature zone is heated from room temperature (about 25°C) to 700°C at a rate of 67.5°C / h, while the low temperature zone is heated from room temperature (about 25°C) to 550°C at a rate of 52.5°C / h for 8 hours. Subsequently, the temperature in the high temperature zone was reduced to 350°C at a rate of 43.75°C / h, and the te...

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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...

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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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