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A kind of preparation method of nano molybdenum disulfide powder

A nano-molybdenum disulfide and powder technology, applied in the direction of molybdenum sulfide, etc., can solve the problems of difficulty in obtaining products with uniform composition, inability to obtain two-dimensional lamellar structure, expensive raw materials for atmosphere sintering, etc., and achieve uniform grain size Controllable, low-cost, and easy-to-operate effects

Inactive Publication Date: 2017-12-29
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] (1) The raw materials of the atmosphere sintering method are expensive, and it is difficult to obtain a product with uniform composition;
[0006] (2) Although nano-molybdenum disulfide with controllable grain size can be obtained by hydrothermal synthesis, etc., the nano-molybdenum disulfide prepared by this method often self-assembles to form a larger micron structure, and cannot obtain a two-dimensional sheet structure;
[0007] (3) Although the equipment and process are simple by adopting physical crushing method, ordinary mechanical ball milling method, etc., the product obtained has lower purity and uneven grain size distribution;

Method used

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  • A kind of preparation method of nano molybdenum disulfide powder
  • A kind of preparation method of nano molybdenum disulfide powder
  • A kind of preparation method of nano molybdenum disulfide powder

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Add 10mmol ammonium molybdate and 20mmol thiourea to the beaker, add 100ml of deionized water to the beaker, stir for 1 hour to fully dissolve the ammonium molybdate and thiourea, and transfer the solution into a 150ml polythene In the reaction kettle lined with tetrafluoroethylene, seal it; place the reaction kettle in an electric oven, set the oven temperature to 220°C, and set the reaction time to 24 hours; when the reaction time is up, take out the reaction kettle and put the inside The mixture in the lining is suction filtered and dried; the dried solid is placed in a beaker, and an aqueous solution with a volume fraction of isopropanol of 30% is added. After ultrasonic stripping for 5 hours, the dispersion is transferred to a centrifuge tube, and the centrifugal speed is 5000r / min Centrifuge down, retain the supernatant and collect the solid therein, and the obtained product is nanometer molybdenum disulfide powder with a particle size of about 500nm. Such as fig...

Embodiment 2

[0037] Add 10mmol ammonium molybdate and 20mmol thiourea to the beaker, add 100ml of deionized water to the beaker, stir for 1 hour to fully dissolve the ammonium molybdate and thiourea, and transfer the solution into a 150ml polythene In the reaction kettle lined with tetrafluoroethylene, it is sealed; the reaction kettle is placed in an electric oven, the oven temperature is set to 220 ° C, and the reaction time is set to 18 hours; when the reaction time is up, the reaction kettle is taken out, and the inner The mixture in the lining is suction filtered and dried; the dried solid is placed in a beaker, and an aqueous solution with a volume fraction of isopropanol of 50% is added, and after ultrasonic stripping for 5 hours, the dispersion is transferred to a centrifuge tube, at a centrifugal speed of 7000r / min Centrifuge down, retain the supernatant and collect the solid therein, and the obtained product is nanometer molybdenum disulfide powder with a particle size of about 40...

Embodiment 3

[0039] Add 10mmol ammonium molybdate and 20mmol thiourea to the beaker, add 100ml of deionized water to the beaker, stir for 1 hour to fully dissolve the ammonium molybdate and thiourea, and transfer the solution into a 150ml polythene In the reaction kettle lined with tetrafluoroethylene, seal it; place the reaction kettle in an electric oven, set the oven temperature to 240°C, and set the reaction time to 9 hours; when the reaction time is up, take out the reaction kettle and put the inside The mixture in the lining is suction filtered and dried; the dried solid is placed in a beaker, and an aqueous solution with a volume fraction of isopropanol of 60% is added, and after ultrasonic peeling for 8 hours, the dispersion is transferred to a centrifuge tube, and the centrifugal speed is 12000r / min centrifuge, retain the supernatant and collect the solid therein, and the obtained product is nanometer molybdenum disulfide powder with a particle size of 200nm. From figure 1 It can...

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Abstract

The invention relates to a method for preparing nanometer molybdenum disulfide powder. The method includes the following steps that 1, ammonium molybdate or sodium molybdate and a sulfur source are mixed, deionized water is added, the mixture is stirred and dissolved, and after dissolution is completed, a solution is transferred into a reaction kettle and sealed; 2, the reaction kettle is put into an electric heating drying oven, and reacting is carried out for 9 hours to 24 hours; 3, the reaction kettle is taken out, the mixture in a lining is subjected to suction filtration and dried, and an aqueous solution of alcohol is added into dried solid; 4, a beaker is put into an ultrasonic cleaning pool and subjected to ultrasonic exfoliation; 5, dispersion liquid is transferred into a centrifuging tube and centrifuged, supernatant liquid is reserved, and sedimentation is removed; 6, the supernatant liquid is subjected to suction filtration and dried, and the nanometer molybdenum disulfide powder with the even-and-controllable grain size and the lamellar structure is obtained. Compared with the prior art, the method has the advantages that a device and the technology are simple, and operation is convenient; the prepared nanometer molybdenum disulfide powder is even and controllable in grain size and obvious in lamellar structure; environment pollution is avoided, and energy consumption and cost are low.

Description

technical field [0001] The invention relates to a preparation method of nano molybdenum disulfide powder, belonging to the technical field of nano material preparation. Background technique [0002] In recent years, molybdenum disulfide low-dimensional nanomaterials have achieved rapid development in the field of optoelectronic device applications, and have been successfully applied to single-photon light sources and solar cells. Nano-molybdenum disulfide powder, as the main raw material of a new generation of optoelectronic semiconductors and high-performance light source materials, has a wide band gap (~1.9eV) and excellent physical and chemical properties, such as quantum size effect, quantum tunneling effect, special Optical and electrical properties and high magnetoresistance, nonlinear optical effects, and when used as an additive, it can improve the strength, elasticity, aging resistance and chemical corrosion resistance of the material. In order to prepare nano-moly...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G39/06
CPCC01G39/06C01P2002/72C01P2002/84C01P2004/03C01P2004/62
Inventor 李昱秦志扬张润霖苏宝连王洪恩陈丽华吴旻阳晓宇邓兆
Owner WUHAN UNIV OF TECH