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Low-energy-consumption preparation method for black phosphorus single crystals

A technology of low energy consumption and black phosphorus, which is applied in the preparation of phosphorus, etc., can solve the problems of high reaction temperature and high requirements for reaction devices, and achieve the effects of high purity, reduced energy consumption, and lowered sublimation temperature

Active Publication Date: 2018-09-21
HUBEI MOPHOS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN105133009A, CN105603517A and CN106087050A have also announced improvements to the method, but there are still problems such as high requirements for the reaction device (the first two require dual temperature zone temperature control) and high reaction temperature (the minimum temperature is all above 500° C.)

Method used

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  • Low-energy-consumption preparation method for black phosphorus single crystals
  • Low-energy-consumption preparation method for black phosphorus single crystals
  • Low-energy-consumption preparation method for black phosphorus single crystals

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Weigh 5 g of 99.999 mass % red phosphorus, add 160 g of stainless steel balls, and ball mill for 7 hours at a rotational speed of 1500 r / min to collect crude black phosphorus powder.

[0027] Weigh 300mg of the above crude black phosphorus powder, 12mg of tin elemental substance, and 6mg of tin tetraiodide, put them in a quartz tube with a length of about 10cm, evacuate until the pressure in the quartz tube is 0.1Pa, and seal the quartz tube. Put the sealed quartz tube in a muffle furnace, raise it from room temperature to 480°C over 60 minutes, keep it warm for 2 hours, and then start to cool down. The cooling process is from 480°C to 300°C over 12 hours, and then down to 100°C over 10 hours. , and then cooled to room temperature over 1 h.

Embodiment 2

[0029] Weigh 2 g of 99.999 mass % red phosphorus, add 120 g of stainless steel balls, and ball mill for 7 hours at a speed of 1000 r / min to collect crude black phosphorus powder.

[0030] Weigh 300mg of the above crude black phosphorus powder, 12mg of tin elemental substance, and 6mg of tin tetraiodide, put them in a quartz tube with a length of about 10cm, evacuate until the pressure in the quartz tube is 0.1Pa, and seal the quartz tube. Put the sealed quartz tube in a muffle furnace, raise it from room temperature to 480°C over 60 minutes, keep it warm for 2 hours, and then start to cool down. The cooling process is from 480°C to 300°C over 12 hours, and then down to 100°C over 10 hours. , and then cooled to room temperature over 1 h.

Embodiment 3

[0032] Weigh 5 g of 99.999 mass % red phosphorus, add 160 g of stainless steel balls, and ball mill for 7 hours at a rotational speed of 1500 r / min to collect crude black phosphorus powder.

[0033] Weigh 300mg of the above crude black phosphorus powder, 12mg of tin elemental substance, and 6mg of tin tetraiodide, put them in a quartz tube with a length of about 10cm, evacuate until the pressure in the quartz tube is 0.1Pa, and seal the quartz tube. Put the sealed quartz tube in the muffle furnace, rise from room temperature to 400°C over 60 minutes, keep it warm for 2 hours, and then start to cool down. The cooling process is from 400°C to 300°C over 12 hours, and then down to 100°C over 12 hours. , and then cooled to room temperature over 1 h.

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Abstract

The invention discloses a low-energy-consumption preparation method for black phosphorus single crystals. The method comprises the following steps that rough black phosphorus powder is used as a phosphorus raw material and subjected to a heating reaction with metal simple substance tin and mineralizer stannic iodide under the vacuum condition, and through programmed cooling, the black phosphorus single crystals with larger size and higher purity are obtained. According to the method, required equipment is simple, the reaction temperature is low, the obtained black phosphorus single crystals are good in crystal form, the energy consumption can be obviously lowered, and the method helps to achieve industrial large-scale preparation of the black phosphorus single crystals.

Description

technical field [0001] The invention belongs to the field of semiconductor material preparation, and in particular relates to a low energy consumption black phosphorus single crystal preparation method. Background technique [0002] The semiconductor industry is playing an increasingly important role in my country's national economy, and the preparation and application of new semiconductor materials is an inevitable requirement for the development of the new era. Theoretical calculations show that black phosphorene is a p-type semiconductor with a direct band gap and has extremely high charge carrier mobility, up to 10000 cm 2 / V·s. Compared with graphene materials with zero bandgap, black phosphorene can realize the switching of logic circuits, and it has better application prospects in sophisticated fields such as field effect transistors and photodetectors. As a precursor for preparing black phosphorene, black phosphorus crystals have a great market demand. Therefore, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/02
CPCC01B25/02
Inventor 喻学锋童睿锋黄浩王佳宏
Owner HUBEI MOPHOS TECH CO LTD
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