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A kind of reactor for the scale-up preparation of black phosphorus crystal and its application

A technology of reactor and black phosphorus, which is applied in the field of two-dimensional materials, can solve problems such as difficult recycling and large-scale scale-up preparation, and achieve the goal of increasing utilization rate, realizing industrial continuous controllable scale-up preparation, and reducing cost and energy consumption Effect

Active Publication Date: 2022-03-22
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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  • A kind of reactor for the scale-up preparation of black phosphorus crystal and its application
  • A kind of reactor for the scale-up preparation of black phosphorus crystal and its application
  • A kind of reactor for the scale-up preparation of black phosphorus crystal and its application

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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 enlarged preparation of black phosphorus crystals and a use method. The reactor includes a heating device, a first reaction chamber and a second reaction chamber communicated with each other, a valve, a sensor, a pipe plug, a pressure relief valve, a sampling plate and a sampling rod. First, add phosphorus source to the first reaction chamber, add catalyst and transport agent to the second reaction chamber; open the valve, vacuum the reaction chamber and close the valve; then heat treatment, and adjust the reaction temperature according to the synchronous feedback of the sensor The program controls the opening and closing of the valve and the pressure relief valve; after the reaction, the sample is taken out to obtain high-purity and high-quality black phosphorus crystals. The double reaction chamber designed by the present invention can realize the continuous and real-time controllable reaction process, and the sensor and pressure relief valve further ensure the safety of the production process, which will be more conducive to improving production capacity and output, reducing cost and energy consumption, and realizing Industrial continuous controllable scale-up preparation of black phosphorus crystals.

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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Patent Type & Authority Patents(China)
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