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Preparation method of amorphous MoSx monolayer nanosheet

A nanosheet and amorphous technology, which is applied in the field of preparation of amorphous MoSx single-layer nanosheets, can solve the problems of restricting the application of amorphous MoSx materials, and achieve the effects of easy large-scale production, low energy consumption, and simple equipment

Inactive Publication Date: 2019-09-03
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the particularity of its structure, there is no effective technical method to achieve large-scale preparation of monolayer amorphous MoS x materials, which severely limits the amorphous MoS x Applications of Materials in Catalysts

Method used

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  • Preparation method of amorphous MoSx monolayer nanosheet
  • Preparation method of amorphous MoSx monolayer nanosheet
  • Preparation method of amorphous MoSx monolayer nanosheet

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] An amorphous MoS x A method for preparing a single-layer nanosheet, comprising the steps of:

[0048] Preparation of MoS by structure reconstruction method 4 2- Intercalated LDHs complex.

[0049] Take 200ml deionized water, 6.8gMg(NO 3 ) 2 ·6H 2 O, 5.0gAl(NO 3 ) 3 9H 2 O and 8g of urea were added to a three-necked flask, stirred at room temperature for 0.5h to dissolve the solid, and refluxed in an oil bath at 90°C for 24h. After filtering, washing, and drying at 60°C for 12 hours, CO 3 2- Intercalated LDHs. The prepared LDHs were calcined in a muffle furnace at 400 °C for 2 h to obtain MMO templates. Weigh 4.0gMMO and 6.0g (NH 4 ) 2 MoS 4 , put into 100ml of degassed deionized water, and stirred for 24h under the protection of nitrogen, and the temperature was kept at 40°C. Then the dispersion was filtered, washed, and dried at 60°C for 12 hours to obtain MoS 4 2- Intercalated LDHs composites (referred to as MoS 4 2- / LDHs).

[0050] 5gMoS 4 2- ...

Embodiment 2

[0058] An amorphous MoS x A method for preparing a single-layer nanosheet, comprising the steps of:

[0059] Preparation of MoS by ion exchange method 4 2- Intercalated LDHs complex:

[0060] Take 10.2gMg(NO 3 ) 2 ·6H 2 O and 7.6gAl(NO 3 ) 3 9H 2 O was dissolved in 200ml deionized water to obtain solution A. Take 6.4g NaOH and dissolve in 200ml deionized water to obtain solution B. Solutions A and B were simultaneously added dropwise to 50 ml of degassed deionized water under stirring condition, under nitrogen protection and the pH was controlled to be 10.0. After stirring at room temperature for 30 min, it was aged in an oven at 80° C. under nitrogen protection for 12 h. After filtration, washing, and vacuum drying at 60°C for 12 hours, NO 3 - Intercalated LDHs. Weigh 5.0g of prepared LDHs and 5.0g (NH 4 ) 2 MoS 4 Add 100ml degassed deionized water, N 2 Under protection, stir at 40°C for 24h. MoS was obtained by filtration, washing, and vacuum drying. 4 2...

Embodiment 3

[0063] An amorphous MoS x A method for preparing a single-layer nanosheet, comprising the steps of:

[0064] MoS 4 2- The preparation of the intercalated LDHs complex is as described in Example 1;

[0065] 5gMoS 4 2- The intercalated LDHs composite powder was placed in a tube furnace, N 2 Under protection, the temperature was raised to 280°C for calcination for 1 hour, and the heating rate was 2°C / min. After natural cooling to room temperature, MoS x / MMO complex. Take 2gMoS x / MMO complex was added to 100ml of 0.5mol / L hydrochloric acid, stirred at room temperature for 12h, then filtered, washed with water, and freeze-dried for 10h to obtain amorphous MoS x monolayer nanosheets.

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Abstract

The invention provides a preparation method of an amorphous MoSx (x=2-4) monolayer nanosheet. The method includes: taking the interlayer of layered double hydroxides (LDHs) as the microreactor, and firstly preparing an MoS4<2-> intercalated LDHs compound; then performing low temperature calcination to enable low temperature decomposition of MoS4<2-> into Mo3S13 nanoclusters, then conducting arrangement at the interlayer to form MoSx monolayer nanosheet, and then carrying out acid dissolution to remove mixed metal oxides (MMO), thus obtaining the amorphous MoSx monolayer nanosheet. The preparation method is simple, has mild reaction conditions, and is easy to realize, does not use organic reagents, is safe, green and environment-friendly. The obtained amorphous MoSx is a monolayer and porous nanosheet structure, has large specific surface area, also has a large number of active sites and defects on the surface, and has excellent electrocatalytic hydrogen evolution performance.

Description

technical field [0001] The present invention relates to an amorphous MoS x The invention discloses a method for preparing single-layer nanosheets, belonging to the field of nanomaterial preparation. Background technique [0002] The current combustion of fossil fuels produces a lot of pollution, and hydrogen, as a clean energy source, is an ideal fuel. Transition metal sulfides such as molybdenum sulfide have attracted much attention due to their great application potential in the fields of electrocatalysis and energy storage materials. However, both density functional theory (DFT) calculations and experimental studies have demonstrated that crystalline MoS 2 The catalytic hydrogen evolution performance mainly depends on the edge active sites, while the laminates are inactive, which severely limits the application of molybdenum sulfide as a hydrogen evolution catalyst. Although a large number of researchers have activated the active sites of the laminates by doping and cr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/06C25B11/06C25B1/04B82Y40/00B01J27/051B01J35/10B01J35/02
CPCC01G39/06C01G39/003C25B1/04B82Y40/00B01J27/051C01P2004/64C01P2004/24C25B11/075B01J35/33B01J35/40B01J35/613B01J35/633Y02E60/36
Inventor 侯万国王德良李海平杜娜
Owner SHANDONG UNIV
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