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Method for preparing two-dimensional layered MoS2 material through molten salt electrochemical intercalation method

A two-dimensional layered, electrochemical technology, applied in the electrolytic process, electrolytic components, etc., can solve the problems that affect the electrochemical performance of MoS2, limit the size and layer distribution of two-dimensional materials, and the shape and thickness are difficult to control, so as to improve the electrochemical performance. Effects of chemical properties, low cost, and low precursor requirement

Active Publication Date: 2019-04-23
NORTHEASTERN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, the mechanical exfoliation method has low yield, layered MoS 2 It is difficult to control the size, shape and thickness of the substrate, the precursor needs a large-sized layered crystal, and the dependence on the substrate is large
The liquid exfoliation method has the disadvantages of low yield, small and uneven products, etc.
Chemical, electrochemical ion intercalation and exfoliation methods limit the size and layer distribution of 2D materials, while the oxygen-containing functional groups in the electrolyte affect the 2D layered MoS 2 electrochemical performance

Method used

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  • Method for preparing two-dimensional layered MoS2 material through molten salt electrochemical intercalation method

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Effect test

Embodiment 1

[0056] Preparation of two-dimensional layered MoS by a molten salt electrochemical intercalation method 2 Material method, proceed as follows:

[0057] In this embodiment, the molten salt used is a chloride molten salt, specifically NaCl-CaCl 2 The mixture, by molar ratio, NaCl:CaCl 2 =0.479:0.521.

[0058] Step 1: Preparation

[0059] (1) NaCl and CaCl 2 salt pretreatment

[0060] Weigh NaCl and CaCl according to the distribution ratio of molten salt raw materials 2 , NaCl and CaCl 2 Grinding separately to obtain NaCl and CaCl with a particle size of 2mm 2 , poured into beakers after grinding, and placed in a muffle furnace to seal;

[0061] In a vacuum state, the muffle furnace was heated up to 200°C at a heating rate of 3°C / min, and the temperature was maintained for 12 hours for pretreatment to remove the water in the molten salt raw material, and then cooled to room temperature to take out the molten salt to obtain dehydrated NaCl and dehydrated CaCl 2 ;

[006...

Embodiment 2

[0078] Preparation of two-dimensional layered MoS by a molten salt electrochemical intercalation method 2 Material method, proceed as follows:

[0079] In this embodiment, the molten salt used is a chloride molten salt, specifically a mixture of LiCl-KCl, with a molar ratio of LiCl:KCl=0.592:0.408.

[0080] Step 1: Pretreatment of LiCl and KCl salts

[0081] Weigh LiCl and KCl according to the distribution ratio of molten salt raw materials, grind LiCl and KCl respectively to obtain LiCl and KCl with a particle size of 1.5 mm, pour them into beakers after grinding, and place them in a muffle furnace to seal;

[0082] In a vacuum state, the muffle furnace was heated up to 300°C at a heating rate of 4°C / min, and kept at a constant temperature for 12 hours for pretreatment to remove the water in the molten salt raw material, and then cooled to room temperature to take out the molten salt to obtain dehydrated LiCl and KCl after dehydration;

[0083] (2) Preparation of electrode...

Embodiment 3

[0096] Preparation of two-dimensional layered MoS by a molten salt electrochemical intercalation method 2 Material method, proceed as follows:

[0097] In this embodiment, the molten salt used is a chloride molten salt, specifically MgCl 2 -Mixture of NaCl-KCl, in molar ratio, MgCl 2 : NaCl: KCl = 0.454: 0.33: 0.216.

[0098] Step 1: Preparation

[0099] (1) MgCl 2 , NaCl and KCl salt pretreatment

[0100] With embodiment 1, difference is:

[0101] 1) In step 1, the MgCl 2 , NaCl and KCl grinding;

[0102] 2) In step 1, obtain dehydrated MgCl respectively 2 , NaCl after dehydration and KCl salt after dehydration.

[0103] (2) Preparation of electrodes

[0104] With embodiment 1;

[0105] Step 2: Assembly of the reaction system

[0106] With embodiment 1, difference is:

[0107] 1) In (2) of step 2, the MgCl after 275g dehydration 2 , 122.75g of dehydrated NaCl and 102.25g of dehydrated KCl were put into the corundum crucible.

[0108] 2) In (3) of step 2, keep t...

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Abstract

The invention discloses a method for preparing a two-dimensional layered MoS2 material through a molten salt electrochemical intercalation method and belongs to the technical field of molten salt electrochemical intercalation. The method includes: removing water in a molten salt raw material of a molten salt system, and heating the molten salt system until molten salt is molten; putting a graphiteanode and a MoS2 cathode piece in an argon atmosphere into the molten salt after constant-temperature stabilization, applying 25-100mA constant current reaction, cooling the MoS2 cathode piece, usingdeionized water for repeatedly cleaning and centrifuging, and drying to obtain the two-dimensional layered MoS2 material. The two-dimensional layered MoS2 material prepared by the method has the advantages of low cost, high yield, simple technological process, short consumed time, environment friendliness and no impact of oxygen-containing functional group.

Description

technical field [0001] The invention relates to the technical field of molten salt electrochemical intercalation, in particular to a molten salt electrochemical intercalation method for preparing two-dimensional layered MoS 2 material method. Background technique [0002] In recent years, two-dimensional semiconductor materials, because of their heterostructures, have very promising application prospects in many fields such as electricity, optics and clean energy, thus attracting more and more interest and research by researchers. Although great progress has been made since graphene was first prepared, its application in practical circuits has been limited by the fact that graphene is a zero-bandgap material. And with MoS 2 The representative two-dimensional transition metal chalcogenide material has very good applications in many fields such as flexible photodetectors, optical switches, optical emitters, information electronics, and solar cells due to its excellent flexib...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B1/00
CPCC25B1/00
Inventor 尹华意赵海佳谢宏伟宁志强宋秋实
Owner NORTHEASTERN UNIV
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