Synthesis method of two-dimensional transition metal chalcogenide

A technology of transition metal chalcogenides and synthesis methods, which is applied in the fields of energy technology, physics and electronics, and can solve problems such as harsh reaction conditions, high cost, and low yield

Active Publication Date: 2021-04-20
济南三川新材料科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Vapor deposition method is an effective method for preparing two-dimensional transition metal chalcogenides with uniform thickness, large size and more types, but this method requires harsh reaction conditions (such as pressure, temperature, substrate, precursor, Cooling rate) and high cost limit the further promotion and application of this method
However, using the exfoliation method, the thickness of the obtained two-dimensional transition metal chalcogenides usually has a wide distribution (single layer to tens of layers), and the yield of this method is low. For example: in 2011, Jonathan of Trinity College, Dublin N. Coleman et al first reported the preparation of two-dimensional materials by liquid phase exfoliation and published it in the journal "Science". The corresponding molybdenum disulfide and tungsten disulfide nanosheets were obtained by centrifugation, and the yield of the obtained single-layer two-dimensional nanosheets was less than 1%.

Method used

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  • Synthesis method of two-dimensional transition metal chalcogenide
  • Synthesis method of two-dimensional transition metal chalcogenide
  • Synthesis method of two-dimensional transition metal chalcogenide

Examples

Experimental program
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Embodiment 1

[0054]This embodiment provides a method of preparing a transition metal compound MX, including:

[0055]1) Etching step: The powder of the transition metal compound Max is placed in an acidic solution, and the acidic ingredient in the acidic solution is etched after etching the A element, to obtain a suspension containing the transition metal compound MX;

[0056]2) Cleaning and drying step: The suspension liquid obtained by step 1) was purified and washed with deionized water. After removing the acidic component, the dry treatment obtained the powder of the transition metal compound MX;

[0057]Among them, in the transition metallic compound MAX, M represents one or more of transition metal elements, titanium, vanadium, ruthenium, zirconium, niobium, molybdenum, hafnium, tantalum, tungsten, and A represents aluminum, silicon, One of the elements of phosphorus, sulfur, gallium, germanium, arsenic, cadmium, indium, tin, 铊, lead and other elements, represents one of carbon, silicon, boron elem...

Embodiment 2

[0060]This example is in Mo2C Nanoflakes as an example to illustrate the preparation method of MX in the present invention, including steps:

[0061]1) Etch step: Put the raw material mo2GA2C powder is placed in aqueous hydrofluoric acid solution for etching, HF is etched after etching the Ga element.2C Nanofold Suspension;

[0062]2) Cleaning and drying step: The suspension liquid obtained by step 1) is purified and cleaned with deionized water. After removing the HF component, the freeze-drying treatment results in MO.2The powder of the c nanoflakes.

[0063]Example 1 and Example 2 Methods of MX nano sheets, wherein the preferred raw material MAX, including MO2GA2C, Mo2GEC, TI3SiC2, Ti2SNC, Ti2ALC, NB2ALC, TA2Alc, Tinbalc, Mo2TIALC2Or (w2 / 3Y1 / 3)2One or more of ALCs. MX nanofrapins for the synthesis method for the present invention, including: mo, by preparing the preferred raw material Max, including: Mo2C, Ti3C2, Ti2C, NB2C, TA2C, Tinbc, Mo2TIC2Or (w2 / 3Y1 / 3)2One or more of C in C.

Embodiment 3

[0065]This embodiment provides a method of synthesizing a two-dimensional transition metal thiomide compound, such asFigure 18 As shown, including the steps:

[0066]1) Heating step: In an inert gas environment, the raw material transition metal compound Mx is heated to a reaction temperature;

[0067]2) Topological conversion reaction step: a gas containing a sulfur element, or a mixed gas containing a sulfur element and a mixed gas containing a phosphor element, and maintains the reaction temperature, set the time long, so that the sulfur Elements, or, sulfur elements, and phosphoric elements, the topology transformation reaction occurs with the transition metal compound MX, and generate two dimensional transition metal sulfide compounds.

[0068]Among them, a gas containing a sulfur element refers to one or more of highly active gaseous sulfur, selenium,, hydrogen sulfide, selenide or hydrogen or hydrogen, containing a gas, including high-active gaseous phosphorus. One or more of arsenic,...

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Abstract

The invention discloses a synthesis method of a two-dimensional transition metal chalcogenide, which comprises the following steps: heating: heating a transition metal compound raw material to a reaction temperature in an inert gas environment; topological conversion reaction step: introducing a gas containing a chalcogen or a mixed gas of the gas containing the chalcogen and the gas containing the phosphorus, and maintaining the reaction temperature for a set period of time, so that the chalcogen, or the chalcogen and the phosphorus are subjected to a topological conversion reaction with the transition metal compound raw material, and generating the two-dimensional transition metal chalcogenide. The synthesis method has the advantages of high reaction degree, high yield, low energy consumption and high efficiency, the obtained two-dimensional transition metal chalcogenide is high in single-layer rate and narrow in layer number distribution, macro preparation can be realized, and the synthesis method has an excellent industrial application prospect.

Description

Technical field[0001]The present invention belongs to the energy technique, physical and electronics, and the method of preparation of metal sulfide, and more particularly, the method of synthesizing a two-dimensional transition metal sulfide compound can be more specifically.Background technique[0002]The graphene has attracted the attention of the majority of researchers due to its excellent electrical, optical and mechanical properties. At the same time, the zero band gap of graphene limits its application in the electronics. Transition metal sulfur compound, including: MOS2, Mose2Mote, Mote2TIS2TISE2, WS2WSE2WTE2Wait, it is a class of graphite structural materials that bind to Van Dehua's power, which presents naturally occurring three prism phases (usually 2H) and non-naturally occurring four-sided phases (usually in 1T) two crystalline states, And its band gap is adjustable as the thickness of the material is adjustable, and there is an application prospect in terms of electron...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/914C01B19/04C01B32/90C01B32/921C01B33/06C01B35/04C01G39/06C01G41/00B82Y30/00B82Y40/00
Inventor 杨树斌杜志国
Owner 济南三川新材料科技有限公司
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