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Oxygen-doped molybdenum disulfide material and preparation method thereof

A molybdenum disulfide and oxygen doping technology, which is applied in chemical instruments and methods, catalyst activation/preparation, chemical/physical processes, etc., to achieve the effect of large specific surface area and good thermal stability

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, for oxygen-doped materials, there is no similar method reported for the incorporation of Se

Method used

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  • Oxygen-doped molybdenum disulfide material and preparation method thereof
  • Oxygen-doped molybdenum disulfide material and preparation method thereof
  • Oxygen-doped molybdenum disulfide material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Use MoO 3 (7mmol) was added as the precursor of molybdenum, ammonium sulfide (21mmol) was added, the volume of the mixture was adjusted to 200mL and pH=10 with deionized water and ammonia water, and the reaction was stirred at 70°C for 2h. After the reaction was completed, it was transferred to a 300mL composite kettle, the gas inside the composite kettle was replaced with nitrogen, 100 mmol of hydrazine hydrate was added, the kettle was sealed, and then hydrothermally synthesized at 170°C for 12 hours. After the reaction is completed, filter, wash the obtained sample with deionized water, and dry it in vacuum at 100°C to obtain the sample, coded as O-MoS 2 (3.0-170-12). 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 ...

Embodiment 2

[0026] Use (NH 4 ) 6 Mo 7 o 24 . 4H 2 O (1 mmol) was added as the precursor of molybdenum, ammonium sulfide (24.5 mmol) was added, the volume of the mixture was adjusted to 200 mL and pH=11 with deionized water and ammonia water, and the reaction was stirred at 70° C. for 2 h. After the reaction was completed, it was transferred to a 300mL composite kettle, and the gas inside the composite kettle was replaced with nitrogen, 100 mmol of hydrazine hydrate was added, the kettle was sealed, and then hydrothermally synthesized at 180°C for 10 hours. After the reaction is completed, filter, wash the obtained sample with deionized water, and dry it in vacuum at 100°C to obtain the sample, coded as O-MoS 2 (3.5-180-10). 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 teste...

Embodiment 3

[0028] Use MoO 3 (7mmol) was added as the precursor of molybdenum, ammonium sulfide (26.25mmol) was added, the volume of the mixture was adjusted to 200mL and pH=10 with deionized water and ammonia water, and the reaction was stirred at 80°C for 1h. After the reaction was completed, it was transferred into a 300mL composite kettle, and the gas inside the composite kettle was replaced with nitrogen, 110 mmol of hydrazine hydrate was added, the kettle was sealed, and then hydrothermally synthesized at 180°C for 24 hours. After the reaction is completed, filter, wash the obtained sample with deionized water, and dry it in vacuum at 100°C to obtain the sample, coded as O-MoS 2(3.75-180-24). 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 ...

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Abstract

The invention relates to an oxygen-doped molybdenum disulfide material and a preparation method thereof. The preparation method comprises the following steps: dispersing and dissolving a precursor of molybdenum in an ammonium sulphide solution; adjusting the pH value of the solution to a range of no less than 10 and no more than 14 by using ammonia water; carrying out a reaction at 50 to 100 DEG C for 0.5 to 6 h; after completion of the reaction, transferring the solution to a hydro-thermal synthesis kettle and introducing nitrogen for protection; adding hydrazine hydrate into the solution and enclosing the hydro-thermal synthesis kettle; carrying out hydro-thermal treatment at 140 to 220 DEG C for 0.5 to 24 h; and then successively carrying out cooling to room temperature, filtering, washing with deionized water and vacuum drying so as to prepare the oxygen-doped molybdenum disulfide material. The material has the advantages of good heat stability, strong acid resistance and a large specific surface area, and has potential application value in fields like catalysis and electrode materials.

Description

technical field [0001] The invention belongs to the technical field of material synthesis, and in particular relates to an oxygen-doped molybdenum disulfide material and a preparation method thereof. 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 shown in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/051B01J37/16B01J35/10
CPCB01J27/051B01J37/16B01J35/613
Inventor 王峰张超锋徐杰张晓辰张志鑫陈海军王业红王敏刘慧芳
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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