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Reactor for amplified preparation of black phosphorus crystals and application thereof

A reactor and black phosphorus technology, applied in the field of two-dimensional materials, can solve problems such as difficult recycling and large-scale scale-up preparation, and achieve the effects of increasing utilization rate, realizing real-time controllability, and improving production capacity and output

Active Publication Date: 2020-12-18
深圳市中科墨磷科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with the chemical vapor transport method widely used at present, the present invention overcomes a series of problems in the past, such as difficulty in recycling due to the complexity of sealing tubes in quartz reactors, and difficulty in large-scale scale-up preparation due to easy explosion of tubes.

Method used

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  • Reactor for amplified preparation of black phosphorus crystals and application thereof
  • Reactor for amplified preparation of black phosphorus crystals and application thereof
  • Reactor for amplified preparation of black phosphorus crystals and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] A reactor for the enlarged preparation of black phosphorus crystals and its application, the specific steps are as follows:

[0068] 1) Weigh 120g of red phosphorus, 4.8g of catalyst Sn and transport agent I according to the ratio of 50:2:1 2 2.4g, wherein the phosphorus source is added to the first reaction chamber through the phosphorus source feed port, the catalyst and transport agent are added to the second reaction chamber through the auxiliary agent feed port, and the sealing baffle is closed after the feeding is completed;

[0069] 2) Place the sampling plate at the bottom of the pipe plug and install a fixed pipe plug to ensure that the overall airtightness of the reaction chamber is good;

[0070] 3) Open the valve to connect the first reaction chamber and the second reaction chamber, and use the pipe plug to vacuum the reaction chamber to below 1Pa, and close the valve after the treatment is completed;

[0071] 4) Turn on the heating device and set the temp...

Embodiment 2

[0076] 1) Weigh 110g of red phosphorus, 3.67g of catalyst In and transport agent SnI according to the ratio of 300:10:8 4 2.93g, wherein the phosphorus source is added to the first reaction chamber through the phosphorus source feed port, the catalyst and transport agent are added to the second reaction chamber through the auxiliary agent feed port, and the sealing baffle is closed after the feeding is completed;

[0077] 2) Place the sampling plate at the bottom of the pipe plug and install a fixed pipe plug to ensure that the overall airtightness of the reaction chamber is good;

[0078] 3) Open the valve to connect the first reaction chamber and the second reaction chamber, and use the pipe plug to vacuum the reaction chamber to below 1Pa, and close the valve after the treatment is completed;

[0079] 4) Turn on the heating device and set the temperature rise-fall program to provide a stable heat source for the reactor; the specific temperature rise program is: the first re...

Embodiment 3

[0084] 1) Weigh 115g of red phosphorus, 4.6g of catalyst Bi and transport agent SnI according to the ratio of 500:20:20 2 4.6g, wherein the phosphorus source is added to the first reaction chamber through the phosphorus source feed port, the catalyst and the transport agent are added to the second reaction chamber through the auxiliary agent feed port, and the sealing baffle is closed after the feeding is completed;

[0085] 2) Place the sampling plate at the bottom of the pipe plug and install a fixed pipe plug to ensure that the overall airtightness of the reaction chamber is good;

[0086] 3) Open the valve to connect the first reaction chamber and the second reaction chamber, and use the pipe plug to vacuum the reaction chamber to below 1Pa, and close the valve after the treatment is completed;

[0087] 4) Turn on the heating device and set the temperature rise-fall program to provide a stable heat source for the reactor; the specific temperature rise program is: the firs...

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Abstract

The invention discloses a reactor for amplified preparation of black phosphorus crystals and a use method. The reactor comprises a heating device, a first reaction bin, a second reaction bin, a valve,a sensor, a pipe plug, a pressure release valve, a sampling plate and a sampling rod, wherein the first reaction bin and the second reaction bin are communicated with each other. The use method comprises the following steps: firstly, adding a phosphorus source into the first reaction bin, and adding a catalyst and a transport agent into the second reaction bin; opening the valve, and closing thevalve after vacuumizing the reaction bins; then carrying out heating treatment, adjusting a reaction temperature program according to synchronous feedback of a sensor, and controlling the opening andclosing of the valve and the pressure release valve; and after the reaction is finished, taking out the sample to obtain the high-purity and high-quality black phosphorus crystal. The double reactionbins designed by the invention can realize the continuity and real-time control of the reaction process, and the sensor and the pressure release valve further ensure the safety of the production process, so that the productivity and yield are improved, the cost and energy consumption are reduced, and the industrial continuous controllable amplified preparation of the black phosphorus crystal is realized.

Description

technical field [0001] The invention belongs to the technical field of two-dimensional materials, and in particular relates to a reactor for the enlarged preparation of black phosphorus crystals and its application. Background technique [0002] Today, when the graphene industry is booming, a "dream material" that is expected to surpass graphene has gradually been discovered, and it is black phosphorus. [0003] Black phosphorus is an allotrope of phosphorus, which has a wrinkled structure similar to but different from the graphene sheet structure, and has a semiconducting direct band gap that graphene does not have. The direct bandgap of black phosphorus can be adjusted with the number of layers (0.3-2.0eV), and it can be switched between insulating and conductive states. In addition, the electron migration speed of black phosphorus is fast (greater than 1000cm 2 V -1 the s -1 ), the switch is relatively high (10 5 ), which is expected to be widely used in the field of ...

Claims

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Application Information

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IPC IPC(8): C30B25/08C30B25/16C30B25/10C30B28/14C30B29/02
CPCC30B25/08C30B25/16C30B25/10C30B28/14C30B29/02
Inventor 喻学锋汪建南王佳宏喻彬璐
Owner 深圳市中科墨磷科技有限公司