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Preparation of two-dimensional layered WS by a molten salt electrochemical exfoliation method 2 material method

A two-dimensional layered, electrochemical technology, applied in the direction of electrolysis components, electrolysis process, etc., can solve the problems of limiting the size and layer distribution of two-dimensional materials, high reaction temperature, non-uniformity, etc., to improve electrochemical performance, process flow and so on. Simple, environmentally friendly effects

Active Publication Date: 2020-03-31
NORTHEASTERN UNIV LIAONING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, the chemical vapor deposition method requires a higher reaction temperature, and has higher requirements on the tube furnace and substrate used for growth; 2 The size, shape and thickness are difficult to control, and the output is low
The liquid exfoliation method has disadvantages such as low yield and small and uneven products; chemical and electrochemical ion exfoliation methods limit the size and layer distribution of two-dimensional materials, and the oxygen-containing functional groups in the electrolyte affect the two-dimensional layered WS. 2 electrochemical performance

Method used

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  • Preparation of two-dimensional layered WS by a molten salt electrochemical exfoliation method <sub>2</sub> material method

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Embodiment 1

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

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

[0058] Step 1: NaCl and CaCl 2 salt pretreatment

[0059] (1) NaCl and CaCl 2 Grinding separately to obtain NaCl powder with a particle size of 2 mm and CaCl powder with a particle size of 2 mm 2 Powder, respectively poured into beakers, and placed in a muffle furnace to seal;

[0060] (2) In a vacuum state, raise the temperature of the muffle furnace to 200-350 ° C and keep the temperature for 12 hours for pretreatment to remove the water in the molten salt, and then cool down to room temperature to take out the molten salt to obtain dehydrated NaCl and dehydrated salt respectively. After CaCl 2 ;

[0061] Step 2: Electrode Preparation

[0062] (1) 1gWS 2 The powder was ...

Embodiment 2

[0075] Preparation of two-dimensional layered WS by a molten salt electrochemical exfoliation method 2 Material method, proceed as follows:

[0076] In this embodiment, the molten salt used is a chloride molten salt, specifically a mixture of LiCl-KCl, in a molar ratio, LiCl:KCl=0.592:0.408.

[0077] Step 1: Pretreatment of LiCl and KCl salts

[0078] (1) Grind LiCl and KCl separately to obtain NaCl powder with a particle size of 2 mm and CaCl powder with a particle size of 2 mm 2 Powder, respectively poured into beakers, and placed in a muffle furnace to seal;

[0079] (2) In a vacuum state, raise the temperature of the muffle furnace to 300°C and keep the temperature constant for 12 hours for pretreatment to remove the water in the molten salt, and then cool down to room temperature to take out the molten salt to obtain dehydrated LiCl and dehydrated LiCl respectively. KCl;

[0080] Step 2: Electrode Preparation

[0081] (1) 1gWS 2 The powder was pressed into an electr...

Embodiment 3

[0092] Preparation of two-dimensional layered WS by a molten salt electrochemical exfoliation method 2 Material method, proceed as follows:

[0093] 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.

[0094] Step 1: MgCl 2 , NaCl and KCl salt pretreatment

[0095] With embodiment 1, difference is:

[0096] (1) In step 1, the MgCl 2 , NaCl and KCl grinding;

[0097] (2) In step 1, the MgCl after dehydration is obtained 2 , NaCl after dehydration and KCl salt after dehydration.

[0098] Step 2: Electrode Preparation

[0099] Identical with embodiment 1;

[0100] Step 3: Assembly of the reaction system

[0101] With embodiment 1, difference is:

[0102] (1) In (2) of step 3, the MgCl after 275g dehydration 2 , 122.75g of dehydrated NaCl and 102.25g of dehydrated KCl were put into a corundum crucible.

[0103] (2) In (3) of step 2, keep the vacuum at 200...

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Abstract

A molten salt electrochemical exfoliation method to prepare two-dimensional layered WS 2 The material method belongs to the technical field of molten salt electrochemical stripping. In this method, the raw materials of the chloride molten salt system are first dried separately, then placed in a corundum crucible and placed in a muffle furnace for heating until the molten salt melts. After the constant temperature is stabilized, the graphite anode is placed in an argon atmosphere. and WS 2 The cathode piece is placed in the molten salt, and after a constant current reaction is applied, the WS 2 After the cathode sheet is lifted out of the molten salt and placed above it to cool, it is repeatedly washed with deionized water, centrifuged and dried to obtain a two-dimensional layered WS. 2 Material. Preparation of two-dimensional layered WS using this method 2 The material has the advantages of low cost, high yield, simple process flow, short time consumption, environmental friendliness and no influence of oxygen-containing functional groups.

Description

technical field [0001] The invention relates to the technical field of molten salt electrochemical exfoliation, in particular to a method for preparing two-dimensional layered WS by molten salt electrochemical exfoliation 2 material method. Background technique [0002] Since the advent of graphene, due to its unique layered structure and photoelectric properties, it has attracted extensive attention from scientific researchers. However, due to its zero-bandgap characteristics, its further application in the field of optoelectronics is limited. Recently, with WS 2 The representative two-dimensional transition metal chalcogenide material has a graphene-like two-dimensional layered structure and excellent electron conduction characteristics. When its bulk material is stripped into two-dimensional nanosheets, it has more excellent physical and chemical properties. performance, widely used in electrochemical energy storage, photoelectric catalysis and other fields. Currently...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B1/00
Inventor 尹华意张贝蕾谢宏伟赵海佳宋秋实
Owner NORTHEASTERN UNIV LIAONING
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