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 dep

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
Comparison scheme
Effect test

Example Embodiment

[0031] Example 1

[0032] Weigh 500g of LiCl, NaCl, KCl (molar ratio is 47.5:15:37.5), mix them evenly, put them in a quartz crucible, heat up at 5°C / min to 200°C for 36h to remove water from the salt, and then heat up at 5°C / min Heat to 550°C for half an hour to completely melt the salt and form a uniform mixed salt. Weigh 2g of melamine powder, press it into tablets with a tablet press, wrap them with foamed nickel and tie them on a molybdenum wire, put them in high-temperature molten salt and react for 40 minutes, and the reaction is carried out under an inert atmosphere of Ar. After taking out the foamed nickel and soaking in deionized water for 24 hours, strip the foamed nickel and collect the product. The obtained product was centrifuged and cleaned three times with deionized water and ethanol at a rotation speed of 6000 r / min and a time of 3 min. The product is then dried at 70°C to obtain a molten salt carbonized nitrogen layered material.

Example Embodiment

[0035] Example 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 uniformly and put into a quartz crucible, heated at 10℃ / min to 250℃ for 24h to remove the water in the salt, and then heated at 10℃ / min to 600℃ for half an hour Until the salt is completely melted and a uniform mixed salt is formed. Weigh 1g of ammonium tetrathiomolybdate ((NH 4 ) 2 MoS 4 )Powder, made into tablets with a tablet machine, wrapped in foamed nickel and put in high temperature molten salt to react for 30 minutes, the reaction is in N 2 In progress. After taking out the foamed copper and immersing it in deionized water for 24 hours, strip the foamed copper and collect the product. The obtained product was centrifuged and washed three times with deionized water and ethanol at a rotation speed of 6000 r / min and a time of 3 min. Then the product is dried at 80°C to obtain molten salt molybdenum disulfide layered material.

Example Embodiment

[0039] Example 3

[0040] Weigh 500g of LiCl, NaCl, KCl (molar ratio 47.5:15:37.5), mix them evenly, put them in a quartz crucible, dry at 200℃ for 24h to remove the moisture in the salt, heat up to 500℃, keep warm until the salt is complete melt. Weigh 2g of melamine powder and 50mg of ammonium tetrathiomolybdate ((NH 4 ) 2 MoS 4 )Powder and mix uniformly, press it into tablets with a tablet press, wrap it with foamed nickel and put it in high temperature molten salt to react for 30 minutes, the reaction is in N 2 In progress. After taking out the foamed nickel and soaking in deionized water for 48 hours, peel off the foamed nickel and collect the product. The obtained product was centrifuged and cleaned with deionized water and ethanol three times at a speed of 7000 r / min and a time of 3 min. Then the product is dried at 80° C. to obtain a molten salt carbonized 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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