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Molybdenum disulfide nano-sheet film material and its preparation methods

A technology of molybdenum disulfide and thin film materials, applied in the directions of molybdenum sulfide, nanotechnology, nanotechnology, etc., can solve the problems of cumbersome preparation process and inconvenient promotion, and achieve the effects of good repeatability, simple synthesis method and uniform structure

Active Publication Date: 2013-01-02
深圳海氢科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the preparation process is loaded down with trivial details, is not convenient for the popularization of industrialization

Method used

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  • Molybdenum disulfide nano-sheet film material and its preparation methods
  • Molybdenum disulfide nano-sheet film material and its preparation methods
  • Molybdenum disulfide nano-sheet film material and its preparation methods

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A. Take the titanium sheet, put it into concentrated hydrochloric acid and ultrasonically wash it, then transfer it to deionized water and ethanol, and ultrasonically wash it respectively;

[0037] B. Prepare 0.25mol / L (NH 4 ) 6 Mo 7 o 24 4H 2 O aqueous solution 4ml, 0.15mol / L thiourea aqueous solution 4ml, mix above-mentioned two solutions, then add 30ml of deionized water, stir fully to obtain homogeneous and stable solution, then transfer to 40ml autoclave; Inclined into the reactor. Heat water at 180°C for 12 hours, and cool to room temperature with cooling water after the reaction is complete.

[0038] C. Take out the titanium sheet in the reaction kettle, wash it with deionized water and ethanol, dry it, and dry it at 80° C. for 1 hour to obtain the product.

[0039] The product has been tested by X-ray photoelectron spectroscopy ( figure 1 ) identified as MoS 2 , after SEM electron microscope picture ( figure 2 ) Observing the morphology of the product...

Embodiment 2

[0041] A. Take the titanium sheet, put it into concentrated hydrochloric acid and ultrasonically wash it, then transfer it to deionized water and ethanol, and ultrasonically wash it respectively;

[0042] B. Prepare 1mol / L Na 2 MoO 4 2H 2 O aqueous solution 15ml, the thioacetamide aqueous solution 15ml of 0.5mol / L, above-mentioned two solutions are mixed, add the deionized water of 8ml again, transfer in the 40ml autoclave after fully stirring to obtain uniform stable solution; The titanium sheet is put into the reaction kettle obliquely. Heat water at 220°C for 24 hours, and cool to room temperature with cooling water after the reaction is complete.

[0043] C. Take out the titanium sheet in the reaction kettle, wash it with deionized water and ethanol, dry it, and dry it at 80° C. for 1 hour to obtain the product.

[0044] The product has passed the SEM electron microscope picture ( Figure 5 ) Observing the morphology of the product, nanosheets with a diameter of 1.6-2...

Embodiment 3

[0046] A. Take the molybdenum sheet, put it into concentrated hydrochloric acid and ultrasonically wash it, then transfer it to deionized water and ethanol, and ultrasonically wash it respectively;

[0047] B. Prepare 0.5mol / L H 2 MoO 4 Aqueous solution 8ml, 0.5mol / L thiourea aqueous solution 8ml, mix above-mentioned two solutions, then add 20ml of deionized water, fully stir to obtain homogeneous and stable solution and then transfer to 40ml autoclave; placed in the reactor. Heat water at 170°C for 24 hours, and cool to room temperature with cooling water after the reaction is complete.

[0048] C. Take out the molybdenum sheet in the reaction kettle, wash it with deionized water and ethanol, dry it, and dry it at 80°C for 1 hour to obtain the product.

[0049] The product has passed the SEM electron microscope picture ( Image 6 ) Observing the morphology of the product, nanosheets with a diameter of 80-200nm and a thickness of 10-20nm grow vertically on the substrate. ...

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Abstract

The invention discloses a molybdenum disulfide (MoS2) nano-sheet film material and its preparation methods. The film material is characterized in that MoS2 nano-sheets vertically and sequentially grow on a conductive substrate, and the diameters and the thicknesses of the MoS2 nano-sheets are 0.05-2mum and 2-30nm respectively. There are two preparation methods of the film material. One preparation method comprises the following steps: a substrate which can be a copper sheet, a silver sheet, a titanium sheet, a tungsten sheet, a molybdenum sheet or carbon is placed in a solution comprising a molybdate and sulfur-containing compounds (comprising thiourea, thioacetamide and L-cysteine); and the sulfur-containing compounds undergo a hydrothermal reaction to grow the compactly-grown and uniformly-sequential MoS2 nano-sheet films on the substrate. Another method comprises the following steps: the molybdenum sheet is directly placed in a solution of the sulfur-containing compounds (comprising thiourea, thioacetamide and L-cysteine); and the sulfur-containing compounds undergo a sulfuration reaction under a hydrothermal condition to form the compact and uniform MoS2 nano-sheet ordered films. The film has a low hydrogen evolution overpotential (-30mv), a small Tafel slope (52mV / dec) and a high electrochemical stability, and is a hydrogen evolution electrode material extremely having an application prospect.

Description

Technical field [0001] The invention relates to the technical field of inorganic advanced nanofilm materials, and specifically relates to a method for preparing MoS on a conductive substrate. 2 Nanosheet thin film materials and their preparation methods and applications. Background technique [0002] Hydrogen is one of the most promising clean energy sources used by humans in the future. It has the advantages of high combustion calorific value and no environmental pollution in the combustion product (water). The effective production of hydrogen is one of the bottlenecks limiting the widespread application of hydrogen. There are currently many methods for producing hydrogen, among which hydrogen production by water electrolysis has attracted much attention due to its simple equipment, no pollution, and high product purity [Nature 2001, 414, 332]. The hydrogen evolution overpotential is caused by polarization on the electrode. Due to the existence of hydrogen evolution over...

Claims

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Application Information

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IPC IPC(8): C01G39/06B82Y30/00H01B13/00
Inventor 孙晓明陆之毅于晓游朱炜
Owner 深圳海氢科技有限公司
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