Metal cation doped molybdenum disulfide material, preparation method and applications thereof

A metal cation, molybdenum disulfide technology, applied in molybdenum sulfide, chemical instruments and methods, chemical/physical processes, etc., can solve problems such as changing the structure of molybdenum disulfide materials

Active Publication Date: 2017-05-03
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the metal impregnated by the preparation method of this type of material is easy to agglomerate and cannot be well dispersed in the material (Adv.Mater.2006,18(19), 2561-2564.), and the introduced metal ions cannot enter well. The lattice of molybdenum disulfide does not serve the purpose of changing the structure of molybdenum disulfide material very well

Method used

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  • Metal cation doped molybdenum disulfide material, preparation method and applications thereof
  • Metal cation doped molybdenum disulfide material, preparation method and applications thereof
  • Metal cation doped molybdenum disulfide material, preparation method and applications thereof

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Experimental program
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Effect test

Embodiment 1

[0024] Use MoO 3 (10mmol) was added as the precursor of molybdenum, ammonium sulfide (40mmol) was added, the volume of the mixture was adjusted to 200mL and pH=11 with deionized water and ammonia water, and the reaction was stirred at 70°C for 2h. Add 0.1mmol Fe 2+ EDTA complex, stirred and reacted for 1.0h, stirred and evaporated the solvent at 70°C, dried in vacuum at 100°C, put the obtained sample in the Ar gas flow after grinding, and roasted at 400°C for 3h to obtain the sample, coded as Fe -MoS 2 (0.01-400-3), and the XRD pattern shows that the interlayer spacing is 6.90 angstroms. Micromeritics ASAP 2010 physical adsorption instrument was used to measure the specific surface area of ​​the sample. Before the test, the sample was vacuum treated at 110 ° C for more than 3 hours to make the vacuum degree reach 10 -6 About torr, and then tested at the temperature of liquid nitrogen (-196°C), the specific surface area is calculated using the BET equation. Nitrogen adsorpt...

Embodiment 2

[0026] Use MoO 3 (10mmol) was added as the precursor of molybdenum, ammonium sulfide (40mmol) was added, the volume of the mixture was adjusted to 200mL and pH=11 with deionized water and ammonia water, and the reaction was stirred at 70°C for 2h. Add 0.1mmol Mn EDTA complex, stir for 1.0h, stir and evaporate the solvent at 70°C, vacuum dry at 100°C, put the obtained sample in the Ar gas flow after grinding, and roast at 450°C for 3h to obtain the sample , numbered as Mn-MoS 2 (0.01-450-3), and the XRD pattern shows that the interlayer spacing is 6.50 angstroms. Micromeritics ASAP 2010 physical adsorption instrument was used to measure the specific surface area of ​​the sample. Before the test, the sample was vacuum treated at 110 ° C for more than 3 hours to make the vacuum degree reach 10 -6 About torr, and then tested at the temperature of liquid nitrogen (-196°C), the specific surface area is calculated using the BET equation. Nitrogen adsorption and desorption experime...

Embodiment 3

[0028] Use MoO 3 (10mmol) was added as the precursor of molybdenum, ammonium sulfide (40mmol) was added, the volume of the mixture was adjusted to 200mL and pH=11 with deionized water and ammonia water, and the reaction was stirred at 70°C for 2h. Add 0.2mmol Co 2+ EDTA complex, stirred and reacted for 1.0h, stirred and evaporated the solvent at 70°C, dried in vacuum at 100°C, put the obtained sample in the Ar gas flow after grinding, and roasted at 420°C for 4h to obtain the sample, coded as Co -MoS 2 (0.02-430-4), and the XRD pattern shows that the interlayer spacing is 6.75 angstroms. Micromeritics ASAP 2010 physical adsorption instrument was used to measure the specific surface area of ​​the sample. Before the test, the sample was vacuum treated at 110 ° C for more than 3 hours to make the vacuum degree reach 10 -6 About torr, and then tested at the temperature of liquid nitrogen (-196°C), the specific surface area is calculated using the BET equation. Nitrogen adsorpt...

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Abstract

The present invention relates to a metal cation doped molybdenum disulfide material, a preparation method and applications thereof. The preparation method comprises: dispersing and dissolving a molybdenum precursor in an ammonium sulfide solution, adjusting the pH value of the solution to more than or equal to 10 and less than or equal to 14 with ammonia water, carrying out a reaction at a temperature of 50-100 DEG C, adding a coordination reagent protected metal coordination compound solution to the solution after the reaction, stirring until achieving a dried state, carrying out vacuum drying, grinding the obtained solid powder, placing in an inert atmosphere (nitrogen or argon) gas flow, treating for 0.5-8 h at a temperature of 380-500 DEG C, and cooling to a room temperature to prepare the metal cation doped molybdenum disulfide material. According to the present invention, the metal cations are uniformly dispersed between each layer of molybdenum disulfide through the doping; the crystal structure of the metal cation doped molybdenum disulfide material maintains the two-dimensional layered structure of molybdenum disulfide; the material interlayer spacing fluctuates between 6.15-10.0 angstrom according to different types and different contents of the doped metals; and the metal cation doped molybdenum disulfide material has advantages of good thermal stability, strong-acid resistance and large specific surface area, and has potential applications in the fields of catalysis, electrode materials, and the like.

Description

technical field [0001] The invention belongs to the technical field of material synthesis, and in particular relates to a cation-doped molybdenum disulfide material and its preparation method and application. Background technique [0002] As an important class of two-dimensional planar materials, molybdenum disulfide has a wide range of applications in catalysis, electrochemistry, and electronic devices. However, experiments and theoretical calculations have confirmed that the largest exposed surface of the molybdenum disulfide material is the chemically inert basal surface, and the highly active edge structure is less exposed. Improving its material activity will be a very important work. [0003] In order to improve the catalytic properties of molybdenum disulfide, chemical or mechanical exfoliation techniques are usually used to exfoliate the bulk molybdenum disulfide material into single-layer or multi-layer nanosheets to expose more active edge structures. However, as...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/06B01J27/051
CPCB01J27/051C01G39/06C01P2002/72C01P2004/04C01P2006/12
Inventor 王峰张超锋徐杰陈海军侯婷婷张晓辰张哲王业红张志鑫
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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