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Black arsenic-phosphorus crystal and preparation method thereof

A technology of crystals and mixed materials, applied in crystal growth, chemical instruments and methods, single crystal growth, etc., can solve the problems of harsh growth equipment conditions, low growth temperature, high impurity content, etc., to expand the band gap change and application range , The effect of simple growth equipment and improved transportation efficiency

Inactive Publication Date: 2019-05-03
SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there are relatively few studies on black arsenic and phosphorus. The traditional method of preparing black arsenic and phosphorus is to use Au and Pb as mineralizers, and PbI 2 As a transport agent, the conditions of the growth equipment are harsh, the growth temperature is low, the transport speed is slow, and the growth time is long (more than three days). Limited range, low crystal quality and crystal size
At the same time, the phenomenon of incomplete phase transition in the growth process leads to the production of toxic arsenic-containing compounds and white phosphorus, which endangers safety.
On the other hand, the previous reports usually use small tube furnaces to grow, the yield is low, and it is only suitable for laboratory use, and cannot further expand its application range.
[0006] At present, there are only relevant literatures on the growth of black phosphorus, and there are no more relevant literatures on the research direction of black arsenic and phosphorus

Method used

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  • Black arsenic-phosphorus crystal and preparation method thereof
  • Black arsenic-phosphorus crystal and preparation method thereof
  • Black arsenic-phosphorus crystal and preparation method thereof

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preparation example Construction

[0026] As an aspect of the technical solution of the present invention, what it relates to is a method for preparing black arsenic phosphorus crystals, comprising the following steps:

[0027] (1) Mix the mixture of arsenic and phosphorus, tin powder and tin tetraiodide according to the mass ratio of 10~60:1~3:0.5~1.5, then vacuum seal, then heat the mixed material to 700℃~800℃ and keep it for 2~3h ;

[0028] (2) Cool the final mixed material obtained in step (1) to a temperature of 450-550°C and keep it for 3-4 hours;

[0029] (3) Cool the final mixed material obtained in step (2) to room temperature to obtain black arsenic phosphorus crystals.

[0030] In some embodiments, the step (1) includes: vacuum-packing the mixed material in a quartz tube, and then putting it into a heating furnace for heating.

[0031] Among them, a molecular pump unit and a hydrogen-oxygen flame can be used to vacuum-pack the mixed material in a quartz tube, and then place the quartz tube in the h...

Embodiment 1

[0049] Put a mixture of high-purity gray arsenic and red phosphorus crystals with an atomic ratio of 0.5:0.5, tin powder, and tin tetraiodide in a mass ratio of 25:1:0.6 into a quartz tube with an outer diameter of 10 mm and a wall thickness of 1 mm. Molecular pump unit and oxyhydrogen flame vacuum seal the quartz block to 10 -2 Pa, the content of the mixed ingredients in the quartz tube is 15~30mg / cm 3 ;

[0050] Put the sealed quartz tube horizontally into the heating zone of the tube furnace, set the temperature in the furnace, first heat the furnace to 750°C at a speed of 5°C / min, and keep it at 750°C for 3 hours, then after 5 hours The furnace was internally cooled to 500°C and held at this temperature for an additional 4 hours.

[0051] This was followed by further slow cooling to room temperature over 3 hours. Black arsenic phosphorus crystal b-As can be obtained at the cold end of the quartz glass tube 0.5 P 0.5 ,Such as figure 1 shown.

Embodiment 2

[0053] Put high-purity gray arsenic and red phosphorus crystals with an atomic ratio of 0.83:0.17, tin powder, and tin tetraiodide in a mass ratio of 30:2:1.5 into a quartz tube with an outer diameter of 15 mm and a wall thickness of 1.5 mm. The pump unit and oxyhydrogen flame vacuum seal the quartz block to 10 -2 Pa, the content of the mixed ingredients in the quartz tube is 15~30mg / cm 3 ;

[0054] Put the sealed quartz tube horizontally into the heating zone of the muffle furnace, set the temperature in the furnace, first heat the furnace to 750°C at a speed of 4°C / min, keep it at 750°C for 3 hours, and then heat it up for 7 hours The furnace was internally cooled to 500°C and held at this temperature for an additional 4 hours.

[0055] This was followed by further slow cooling to room temperature over 5 hours. Black arsenic phosphorus crystal b-As can be obtained at the cold end of the quartz glass tube 0.83 P 0.17 ,Such as figure 2 shown.

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Abstract

The invention discloses a preparation method for a black arsenic-phosphorus crystal. The preparation method comprises the following steps: (1) mixing an arsenic and phosphorus mixture, tin powder andtin tetraiodide according to a mass ratio of (10-60): (1-3): (0.5-1.5), carrying out vacuum packaging, then heating a mixed material to 700 DEG C to 800 DEG C, and maintaining the temperature for 2 to3 h; (2) cooling a mixed material obtained in the step (1) to a temperature of 450 to 550 DEG C, and maintaining the temperature for 3 to 4 h; and (3) cooling a mixed material obtained in the step (2) to a room temperature so as to obtain the black arsenic-phosphorus crystal. The preparation method provided by the invention can prepare a series of black arsenic-phosphorus crystals with an atomicratio, expands band gap changes and application range of black arsenic phosphorus, and realizes large-scale preparation of high-quality black arsenic-phosphorus crystals with adjustable band gap. Meanwhile, by adoption of the tin tetraiodide, the temperature of growth is reduced; the efficiency of transportation is improved; and vacuum equipment can prevent from generating corrosion. In addition,the preparation method provided by the invention has the advantages of high black arsenic phosphorus conversion rate, no generation of impurity phases, short growth time, simple growth equipment and high yield.

Description

technical field [0001] The invention relates to a black arsenic and phosphorus crystal and a preparation method thereof, belonging to the technical field of chemical material synthesis. Background technique [0002] In the past ten years, graphene-like two-dimensional layered materials have been a hot spot of academic research. This type of material is bonded by strong chemical bonds in the atomic plane, and is coupled by weak van der Waals force between atomic layers. Samples with different atomic layer thicknesses were obtained. Its unique microstructure and physical and chemical properties have been widely and deeply studied in the fields of semiconductor electronics, optics, energy storage, and catalysis. [0003] Although graphene and transition metal chalcogenide two-dimensional materials represented by molybdenum disulfide have many excellent properties, as semiconductor materials, both have their own differences in either band gap width or electron mobility. inher...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B9/04C30B29/10
Inventor 张凯史鑫尧徐轶君
Owner SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI
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