A constant-temperature large-scale preparing method of belt-shaped black phosphorus

A large-scale preparation and strip-shaped technology, which is applied in the field of constant temperature and large-scale preparation of strip-shaped black phosphorus, can solve the problems of inability to achieve large-scale mass production, the limitation of black phosphorus production, and the increase of preparation cost, and achieves improved productivity and surface area. Smooth, easy-to-use effects

Active Publication Date: 2016-04-06
ZHEJIANG UNIV
View PDF4 Cites 26 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Recently, also have article report to prepare black phosphorus with red phosphorus, tinned gold, tin tetraiodide as raw material, but the cost of gold and tin tetraiodide in the raw material used is extremely high, and tin tetraiodide also needs to be prepared in advance, greatly improves The cost of preparation is reduced, and the process is

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A constant-temperature large-scale preparing method of belt-shaped black phosphorus
  • A constant-temperature large-scale preparing method of belt-shaped black phosphorus
  • A constant-temperature large-scale preparing method of belt-shaped black phosphorus

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Tin, high-purity red phosphorus, and iodine are mixed according to the ratio (mass ratio) of tin: red phosphorus: iodine=0.6:20:0.1, and then put into a quartz tube and directly seal the tube; then put the sealed quartz tube into a horse boiling furnace , the number of quartz tubes to be put in depends on the volume of the horse boiling furnace; set the reaction time, then raise the temperature to 650°C, keep it for 2h, then cool it down to 300°C, keep it for 2h, and finally cool down slowly to room temperature (10h). The resulting strip-shaped black phosphorus is evenly distributed in the quartz tube, such as figure 1 shown.

[0016] The resulting product is a black ribbon block, figure 2 Its XRD figure, its SEM such as image 3 As shown, it can be seen that the obtained product is black phosphorus. And it is measured that the mass of the obtained black phosphorus is about 97% of the mass of the red phosphorus in the raw material.

[0017] Select the resulting str...

Embodiment 2

[0018] Tin, high-purity red phosphorus, and iodine are mixed according to the ratio of tin: red phosphorus: iodine=1:18:0.4, then put into the quartz tube and directly seal the tube; then put the sealed quartz tube into the horse boiling furnace, the number of quartz tubes Depends on the volume of the horse boiler; set the reaction time, then raise the temperature to 750°C, keep it warm for 5h, then cool down to 400°C, keep warm for 5h, and finally cool down slowly to room temperature (15h). The obtained long black phosphorus is evenly distributed in the quartz tube.

Embodiment 3

[0020] Tin, high-purity red phosphorus, and iodine are mixed according to the ratio of tin: red phosphorus: iodine=3:40:0.5, then put into the quartz tube and directly seal the tube; then put the sealed quartz tube into the horse boiling furnace, the number of quartz tubes Depends on the volume of the horse boiler; set the reaction time, then raise the temperature to 500°C, keep it warm for 10h, then cool down to 200°C, keep it warm for 8h, and finally cool down slowly to room temperature (20h). The obtained long black phosphorus is evenly distributed in the quartz tube.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention discloses a constant-temperature large-scale preparing method of belt-shaped black phosphorus to prepare the black phosphorus in a constant-temperature manner. Cheap red phosphorus, tin and iodine are adopted as raw materials and subjected to a solid-phase reaction at a constant temperature under a low pressure to prepare the pure-phase belt-shaped black phosphorus. The method is simple in steps and high in operability. The method is advantageous in that 1) the adopted raw materials are nontoxic so that the method is clean and environmental friendly, 2) tin tetraiodide is replaced by the iodine, thus greatly reducing a cost, 3) the conversion ratio of the black phosphorus is high, and 4) black phosphorus growth is performed with a muffle furnace in place of a tube furnace, so that the yield of the black phosphorus is greatly increased, a single-pass black phosphorus yield only depends on the volume of the muffle furnace, and the single-pass yield is increased by at least 10 times or above than a single-pass yield when black phosphorus growth is performed in a tube furnace. The prepared belt-shaped black phosphorus is characterized in that crystallinity is good, and thin-layer black phosphorus with a large area can be stripped mechanically more easily. The method provides great convenience for subsequent preparation and applications of photoelectric devices based on the black phosphorus.

Description

technical field [0001] The invention relates to the field of synthesis of chemical materials, in particular to a method for constant temperature and large-scale preparation of strip-shaped black phosphorus. technical background [0002] Graphene-like two-dimensional semiconductor materials are expected to replace the traditional semiconductor silicon due to their high conductivity, high toughness and large specific surface area, triggering a new round of revolution in the field of electronic technology. However, since graphene has no energy band structure, it cannot realize the on and off of logic circuits, which greatly limits its application in the fields of electronic devices and optoelectronic devices, such as photodetectors, solar cells, field effect transistors, etc. In recent years, searching for new two-dimensional semiconductor materials has become one of the important research fields of materials science. [0003] Black phosphorus is the most dense (2.69g / cm3) of ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C01B25/02
CPCC01B25/02C01P2004/01C01P2004/02C01P2004/03
Inventor 王业伍赵明钱皓磊牛欣玥沙健
Owner ZHEJIANG UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap