Preparation method of nano 1T phase molybdenum disulfide/nickel disulfide composite nano material

A composite nanomaterial, molybdenum disulfide technology, applied in nickel sulfide, molybdenum sulfide, nanotechnology and other directions, can solve the problems of low purity, insufficient stability, low yield, etc., to achieve safe preparation process, maintain stability, and high production efficiency Effect

Active Publication Date: 2019-11-29
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In order to solve the problems of low yield, low purity and insufficient stability in alkaline environment in the current preparation of 1T phase molybdenum disulfide

Method used

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  • Preparation method of nano 1T phase molybdenum disulfide/nickel disulfide composite nano material
  • Preparation method of nano 1T phase molybdenum disulfide/nickel disulfide composite nano material
  • Preparation method of nano 1T phase molybdenum disulfide/nickel disulfide composite nano material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Put 0.581g of nickel nitrate, 1.68g of hexamethylenetetramine, 0.3g of ammonium molybdate and 0.02g of trisodium citrate dihydrate in 50mL of water, stir for half an hour to a light green transparent solution, pour into poly Store in a 100mL hydrothermal kettle lined with tetrafluoroethylene, seal and store, heat to 120°C, keep warm for 24h, and cool to room temperature, wash and centrifuge repeatedly with deionized water and absolute ethanol, and vacuum dry at 60°C for 12 hours to obtain Precursor (Ni(OH) 2-x -Mo 7 o 24 6- ); put 0.1g precursor and 2.0g thioacetamide into 35mL deionized water and stir vigorously for 1h, pour it into a 50mL polytetrafluoroethylene-lined hydrothermal kettle, keep it sealed, heat to 220°C, and keep it warm for 24h , cooled to room temperature, washed and centrifuged repeatedly with deionized water and absolute ethanol, and vacuum-dried at 60°C for 12 hours to obtain a 1T phase molybdenum disulfide / nickel disulfide composite. As shown ...

Embodiment 2

[0032] Put 0.581g of nickel nitrate, 1.68g of hexamethylenetetramine, 0.3g of ammonium molybdate and 0.02g of trisodium citrate dihydrate in 50mL of water, stir for half an hour to a light green transparent solution, pour into poly Store in a 100mL hydrothermal kettle lined with tetrafluoroethylene, seal and store, heat to 120°C, keep warm for 24h, and cool to room temperature, wash and centrifuge repeatedly with deionized water and absolute ethanol, and vacuum dry at 60°C for 12 hours to obtain Precursor (Ni(OH) 2-x -Mo 7 o 24 6- ); put 0.1g precursor and 2.0g thioacetamide into 35mL deionized water and stir vigorously for 1h, pour it into a 50mL polytetrafluoroethylene-lined hydrothermal kettle, keep it sealed, heat to 220°C, and keep it warm for 24h , cooled to room temperature, washed and centrifuged repeatedly with deionized water and absolute ethanol, and vacuum-dried at 60°C for 12 hours to obtain a 1T phase molybdenum disulfide / nickel disulfide composite.

Embodiment 3

[0034] Put 0.581g of nickel nitrate, 1.68g of hexamethylenetetramine, 0.1g of ammonium molybdate and 0.02g of trisodium citrate dihydrate in 50mL of water, stir for half an hour to a light green transparent solution, pour into poly Store in a 100mL hydrothermal kettle lined with tetrafluoroethylene, heat up to 120°C, keep warm for 20h, and cool to room temperature, wash and centrifuge repeatedly with deionized water and absolute ethanol, mix 0.1g of precursor with 2.0g of thio Put acetamide into 35mL deionized water and stir vigorously for 1h, pour it into a 50mL polytetrafluoroethylene-lined hydrothermal kettle, keep it sealed, heat to 220°C, keep it warm for 24h, cool to room temperature, and use deionized water and anhydrous Wash and centrifuge repeatedly with ethanol, and dry in vacuum at 60°C for 12 hours to obtain a 1T phase molybdenum disulfide / nickel disulfide composite.

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Abstract

The invention discloses a preparation method of a nano 1T phase molybdenum disulfide/nickel disulfide composite nano material, belonging to the field of preparation of inorganic material transition metal chalcogenide. The preparation method adopts a two-step method, and comprises the following steps of: firstly, synthesizing a molybdate- radical- intercalated nano nickel hydroxide nanosheets froma plurality of substances of nickel nitrate, nickel chloride, ammonium molybdate hydrate, sodium molybdate, hexamethylene tetramine, trisodium citrate dihydrate, sodium dodecyl benzene sulfonate and sodium dodecyl sulfate as raw materials; and then carrying out hydrothermal synthesis by taking the nanosheets as templates and taking one or more of thiourea, thioacetamide or L-cysteine as sulfur sources to obtain a high-purity nano 1T-phase molybdenum disulfide/nickel disulfide composite nano material. The preparation method has simple process, mild conditions, high production efficiency and safe preparation process. By adjusting the dosage of the sulfur sources, the proportion of 1T phase molybdenum disulfide can be adjusted to obtain high purity 1T phase molybdenum disulfide.

Description

technical field [0001] The invention relates to a preparation method of a nanometer 1T phase molybdenum disulfide / nickel disulfide compound, which belongs to the field of preparation of inorganic material transition metal chalcogenides. Background technique [0002] Molybdenum disulfide is a special layered two-dimensional material, which is widely used in industrial fields such as catalysis, lubrication, and hydrogen storage. The common polycrystalline phases are 2H, 3R, and 1T phases. The 2H and 3R phases are semiconductor structures with poor electrical conductivity, which is not conducive to electron transport in catalytic reactions. The 1T phase molybdenum disulfide has a special layered structure, large specific surface area, high conductivity and hydrophilicity, and more importantly, for the electrochemical catalytic hydrogen production reaction, because the base surface of the 1T phase molybdenum disulfide is also It has catalytic activity, so the density of active ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G53/11C01G39/06B82Y40/00
CPCB82Y40/00C01G39/06C01G53/11C01P2002/72C01P2002/85C01P2004/04
Inventor 于然波陈晓煜王祖民魏延泽张行
Owner UNIV OF SCI & TECH BEIJING
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