Method used for growth of transition metal chalcogenide crystals via metal fluxing agent method

A technology of chalcogen compound and flux method, which is applied in chemical instruments and methods, melt from molten solvent, single crystal growth, etc., can solve the problem of difficult to obtain high-quality and large-sized crystals, and achieve high chemical stability Sex and heat stability, good quality, short growth cycle

Active Publication Date: 2015-08-19
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the methods for preparing transition metal chalcogenides mainly include hydrothermal method, chemical vapor deposition method, thermal decomposition method, etc. Through these methods, nanosheets, thin films or small crystals of transition metal chalcogenides can be grown and synthesized. It is difficult to obtain high quality and large size crystals

Method used

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  • Method used for growth of transition metal chalcogenide crystals via metal fluxing agent method
  • Method used for growth of transition metal chalcogenide crystals via metal fluxing agent method
  • Method used for growth of transition metal chalcogenide crystals via metal fluxing agent method

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Embodiment 1

[0037] Growth of transition metal chalcogenide MoS by a metal flux method 2 A method for crystallization comprising the steps of:

[0038] (1) The raw materials elemental Mo, elemental S, and elemental Sn are mixed according to the molar ratio of 1:2:10, mixed evenly, put into a clean high-purity quartz tube, and vacuumed by a vacuum pump to make the inside of the quartz tube reach 1×10 -3 Pa, and then sinter and seal the quartz tube with an oxyhydrogen flame; put the quartz tube into a well-type furnace, raise the temperature to 1150°C, and keep it warm for 20h;

[0039] (2) Cool down at a rate of 6°C / h for the first stage of cooling, so that the crystals spontaneously crystallize. When the temperature drops to 900°C, after holding at 900°C for 20 hours, quickly take out the quartz tube from the pit furnace, and then centrifugally quench , let it cool down to room temperature within 10 minutes, and then get silver-gray 0.5mm×1mm MoS 2 crystals.

[0040] Test the MoS obtain...

Embodiment 2

[0042] Growth of transition metal chalcogenide MoS by a metal flux method 2 A method for crystallization comprising the steps of:

[0043] (1) The raw materials elemental Mo, elemental S, and elemental Sn are mixed according to the molar ratio of 1:2:10, mixed evenly, put into a clean high-purity quartz tube, and vacuumed by a vacuum pump to make the inside of the quartz tube reach 1×10 -3Pa, and then sinter and seal the quartz tube with an oxyhydrogen flame; put the quartz tube into a well-type furnace, raise the temperature to 1150°C, and keep it warm for 20h;

[0044] (2) Cool down at a rate of 2°C / h for the first stage of cooling, so that the crystals crystallize spontaneously. When the temperature drops to 900°C, after holding at 900°C for 20 hours, quickly take out the quartz tube from the pit furnace, and then centrifugally quench it. Allow it to cool down to room temperature in 10 minutes to obtain silver-gray 3mm×4mm flake MoS 2 Crystal, the crystal quality is the b...

Embodiment 3

[0051] Growth of transition metal chalcogenide MoS by a metal flux method 2 A method for crystallization comprising the steps of:

[0052] (1) The raw materials elemental Mo, elemental S, and elemental Sn are mixed according to the molar ratio of 1:2:5, mixed evenly, put into a clean high-purity quartz tube, and vacuumed by a vacuum pump to make the inside of the quartz tube reach 1×10 -3 Pa, then sinter and seal the quartz tube with an oxyhydrogen flame; put the quartz tube into a well-type furnace, raise the temperature to 1100°C, and keep it warm for 20h;

[0053] (2) Cool down at a rate of 6°C / h for the first stage of cooling, so that the crystals crystallize spontaneously. When the temperature drops to 900°C, after holding at 900°C for 20 hours, quickly take out the quartz tube from the pit furnace, and then centrifugally quench it. Allow it to cool down to room temperature in 5 minutes to obtain silver-gray millimeter-scale flake MoS 2 crystals.

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Abstract

The invention relates to a method used for growth of transition metal chalcogenide crystals via metal fluxing agent method. The method comprises following steps: (1) elementary substance M, elementary substance X, and elementary substance Sn are mixed, an obtained mixture is heated to 1100 to 1150 DEG C at a vacuum degree of 1*10<-3> to 1*10<-4>Pa, and thermal prevention is carried out for 20 to 40h, wherein M is used for representing Cr, Mo, or W, and X is used for representing S, Se, or Te; and (2) the mixture is subjected to first stage temperature reducing at a temperature reducing speed of 1-6 DEG C / h so as to realize crystal spontaneous crystallization, when the temperature is reduced to 900 to 1000 DEG C, thermal preservation is carried out for 20 to 40h, quenching is carried out, and an obtained product is cooled to room temperature in 5 to 10min so as to obtain the transition metal chalcogenide crystals. Operation conditions of the method are easy to realize, and controllable; raw materials are easily available, and are cheap; the obtained transition metal chalcogenide crystals are high in quality; and application prospect in the fields of photon, photoelectric, and electronic devices is promising.

Description

technical field [0001] The invention relates to a method for growing transition metal chalcogen compound crystals by a metal flux method, and belongs to the technical field of crystal growth. Background technique [0002] With the development of science, technology and economy, silicon, the basic support material of the information society, will reach its physical limit, and it is imminent to find alternative materials for silicon. In recent years, it has been discovered that transition metal chalcogenides may surpass graphene as a substitute for silicon due to their excellent semiconductor properties. Moreover, this kind of material also has important application prospects in the fields of photonics and optoelectronics. Transition metal chalcogenides (TMDCs) have the chemical formula MX 2 (M=Cr, Mo, W; X=S, Se, Te), belonging to the hexagonal crystal system, is a layered semiconductor material, and the layers are combined by weak van der Waals force, so it can be peeled o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B9/10C30B29/46
Inventor 陶绪堂张西霞王善朋
Owner SHANDONG UNIV
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