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High temperature molten salt method for preparing material with microscopic layered crystal structure

A layered crystal structure, high-temperature melting technology, applied in the direction of molybdenum sulfide, nitrogen and non-metallic compounds, etc., can solve the problems of layered materials such as instability, easy agglomeration, and affecting the application performance of layered nanomaterials, and achieve uniform morphology , not easy to reunite, excellent performance

Active Publication Date: 2016-08-03
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, the current synthesis methods of layered nanomaterials, such as high temperature pyrolysis, high temperature and high pressure synthesis, and electrochemical deposition, generally have shortcomings such as instability and easy agglomeration of layered materials, which greatly affect the application of layered nanomaterials. performance

Method used

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  • High temperature molten salt method for preparing material with microscopic layered crystal structure
  • High temperature molten salt method for preparing material with microscopic layered crystal structure
  • High temperature molten salt method for preparing material with microscopic layered crystal structure

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Weigh 500 g of LiCl, NaCl, KCl (molar ratio 47.5:15:37.5) and mix them evenly, put them into a quartz crucible, raise the temperature at 5°C / min to 200°C and keep it for 36 hours to remove the moisture in the salt, then raise the temperature at 5°C / min To 550 ℃, keep warm for half an hour to completely melt the salt and form a uniform mixed salt. Weigh 2g of melamine powder, press it into a tablet with a tablet machine, wrap it with nickel foam and tie it to a molybdenum wire, put it in a high-temperature molten salt and react for 40min, and the reaction is carried out under an inert atmosphere of Ar. The nickel foam was taken out and soaked in deionized water for 24 hours, the nickel foam was peeled off, and the product was collected. The obtained product was centrifuged and washed with deionized water and ethanol three times each at a rotational speed of 6000 r / min for 3 minutes. Then the product was dried at 70°C to obtain a layered material of molten salt carbonize...

Embodiment 2

[0036] Weigh Li 2 CO 3 , Na 2 CO 3 , K 2 CO 3 (The molar ratio is 43.5:31.5:25) A total of 500g is mixed evenly and placed in a quartz crucible, heated at 10°C / min to 250°C and kept for 24 hours to remove moisture in the salt, then heated at 10°C / min to 600°C and kept for half an hour until the salt is completely melted and a uniform salt mixture is formed. Weigh 1g ammonium tetrathiomolybdate ((NH 4 ) 2 MoS 4 ) powder, made into tablets with a tablet machine, wrapped with nickel foam and put into high-temperature molten salt to react for 30min, and reacted in N 2 in progress. Take out the foamed copper and soak it in deionized water for 24 hours, then peel off the foamed copper and collect the product. The obtained product was centrifuged and washed with deionized water and ethanol three times each at a rotational speed of 6000 r / min for 3 minutes. Then the product was dried at 80° C. to obtain a layered material of molten salt molybdenum disulfide.

Embodiment 3

[0040]Weigh 500 g of LiCl, NaCl, KCl (molar ratio 47.5:15:37.5) and mix them evenly, put them into a quartz crucible, dry at 200°C for 24 hours to remove the moisture in the salt, raise the temperature to 500°C, and keep it warm until the salt is completely melt. Take by weighing 2g melamine powder and 50mg ammonium tetrathiomolybdate ((NH 4 ) 2 MoS 4 ) powder and mixed evenly, pressed into tablets with a tablet machine, wrapped with nickel foam and put into high-temperature molten salt to react for 30min, and reacted in N 2 in progress. The nickel foam was taken out and soaked in deionized water for 48 hours, then the nickel foam was peeled off and the product was collected. The obtained product was centrifuged and washed with deionized water and ethanol three times each, at a rotational speed of 7000 r / min, for 3 minutes. Then the product is dried at 80° C. to obtain molten salt carbide nitrogen / molybdenum disulfide composite layered material.

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Abstract

The invention provides a high temperature molten salt method for preparing a material with a microscopic layered crystal structure. The method comprises the following steps: (1) placing solid salts into an enclosed high temperature resistant crucible, and heating the crucible to melt the solid salts into ionic liquid; (2) introducing inert gas into the enclosed crucible, pressing the precursor of a layered material into a sheet, wrapping the sheet, and adding the sheet into molten salt to carry out reactions in the atmosphere of inert gas; (3) after a while, taking out the reaction products, soaking reaction products in deionized water, centrifugally washing reaction products by deionized water and ethanol for several times, and drying to obtain the layered material. According to the high temperature molten salt method, the layered material is prepared in a high temperature ionic environment, due to the existence of ions, the layered material is not easy to agglomerate; moreover, ions enter the gap between lattice layers, the structure becomes more stable, and a layered material with a better using performance is obtained.

Description

technical field [0001] The invention relates to a novel method for preparing functional materials with high-temperature molten salt, and is especially suitable for preparing materials with microscopic layered crystal structures. Background technique [0002] Layered nanomaterials are a new type of nano-functional materials with special morphology, interface properties and various excellent properties. They are the frontier and hot spot in the field of chemistry and materials research. Batteries, functional ceramics and other fields have broad application prospects. Layered compounds have a two-dimensional laminate structure. The two-dimensional laminates are oriented and ordered to form a three-dimensional crystal structure. The chemical composition of the laminates, the type and quantity of interlayer ions, and the crystal particle size and distribution are very diverse and adjustable. . The structural characteristics of layered compounds allow certain substances to be in...

Claims

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Application Information

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IPC IPC(8): C01B21/082C01G39/06
CPCC01B21/082C01G39/06C01P2002/72C01P2004/03
Inventor 肖巍周静黄飞帆汪的华
Owner WUHAN UNIV
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