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A method for preparing a single-layer two-dimensional transition metal sulfide material

A transition metal and sulfide technology, applied in the field of preparing single-layer two-dimensional transition metal sulfide materials, can solve the problems of waste of resources, environment, excessive crystal nuclei, pollution, etc.

Active Publication Date: 2020-04-14
SHENZHEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Existing CVD prior art such as CN104384527A and CN106571244A etc. adopt the commonly used M precursor as a powder, and the precursor usually needs to be discarded once used, resulting in waste of resources and environmental pollution
In addition, since a certain amount of Ar / H needs to be introduced into the CVD system 2 Such as protective or reactive gases, the existence of powder may cause too many crystal nuclei or sample contamination in the prepared sample, resulting in the formation of monolayer MX 2 decline in sample quality

Method used

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  • A method for preparing a single-layer two-dimensional transition metal sulfide material
  • A method for preparing a single-layer two-dimensional transition metal sulfide material
  • A method for preparing a single-layer two-dimensional transition metal sulfide material

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Embodiment 1

[0026] Use as figure 1 CVD growth equipment, parts 1, 2, 3 and 4 in the figure, regions 1 and 2 are the low temperature and high temperature regions of CVD respectively, 1 is S powder or Se powder, 2 is metal foil, 3 is sapphire substrate , 4 is Ar and H 2 The mixed gas.

[0027] A kind of preparation of monolayer MoS 2 Methods. It includes the following steps:

[0028] (1) First, put the Mo metal foil in a mixed solution of concentrated sulfuric acid and hydrogen peroxide (H 2 SO 4 : H 2 O 2 Volume ratio=2:1) ​​Soak for 2 hours, then place the Mo metal foil at 2 places in the high temperature zone 2 of the 2-inch quartz tube, and heat up to 400°C at a rate of 40°C / min. Annealing at atmospheric pressure in the air for 2 minutes to fully oxidize to Mo oxide MoO 3-X ;

[0029] (2) Put the cut 10*40mm single-polished quartz chip in a mixed solution of concentrated sulfuric acid and hydrogen peroxide (H 2 SO 4 : H 2 O 2 Volume ratio = 2:1) Soak for 2 hours, and then ultrasonically clea...

Embodiment 2

[0034] Use as figure 1 CVD growth equipment, components 1, 2, 3 and 4 in the figure, regions 1 and 2 are the low and high temperature regions of CVD respectively, 1 is Se powder, 2 is metal foil, 3 is sapphire substrate, 4 is Ar and H 2 The mixed gas.

[0035] A preparation of single-layer WSe 2 Methods. Using the oxidized W foil as the W precursor and Se powder as the Se source, a triangular shape WSe with a side length of about 4.5 microns is prepared 2 . Use optical microscope and Raman equipment to characterize the prepared samples, the results are as follows image 3 Shown. The sample presents a very good triangular shape and is a single-layer WSe with good uniformity 2 material. Specific steps are as follows:

[0036] (1) First, put the W metal foil in a mixed solution of concentrated sulfuric acid and hydrogen peroxide (H 2 SO 4 : H 2 O 2 Volume ratio = 2:1) Soak for 2 hours, then place the W metal foil at 2 places in the high temperature zone 2 of the 2-inch quartz tube...

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Abstract

The invention belongs to the technical field of material preparation, and particularly relates to a method for preparing a single-layer two-dimensional transition metal sulfide material. An oxidized Mfoil is used as an M precursor for preparing a two-dimensional material by CVD (chemical vapor deposition), X powder serves as an X source, the single-layer two-dimensional material MX2 with good crystallinity is prepared by setting a high-temperature area and a low-temperature area for CVD and by the aid of specific heating and cooling procedures, and a new idea is provided for growth and preparation of later large-area two-dimensional materials.

Description

Technical field [0001] The invention belongs to the technical field of material preparation, and particularly relates to a method for preparing a single-layer two-dimensional transition metal sulfide material. Background technique [0002] With the continuous advancement of the post-Moore era, new two-dimensional materials have gradually become a research hotspot in recent years. The discovery, large-scale preparation and application of graphene have opened up ideas for people in the field of two-dimensional materials. Transition sulfide MX 2 (M=Mo, W; X=S, Se) has a special layered structure. Atoms are bonded through strong covalent bonds in the layer, and different layers are combined by weak van der Waals force. When the thickness is In the case of a single layer, the material exhibits special physical properties, from the indirect band gap semiconductor of the bulk material to the direct band gap semiconductor, making MX 2 It is expected to become an emerging semiconductor m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G39/06C01G41/00C01B17/20C01B19/04
CPCC01B17/20C01B19/007C01G39/06C01G41/00C01P2002/82C01P2004/20
Inventor 时玉萌李贺楠姚慧珍陈龙龙
Owner SHENZHEN UNIV
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