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Preparation method of molybdenum diselenide/cobalt diselenide nanocomposite

A nanocomposite material, a technology of cobalt diselenide, which is applied in the field of preparation of molybdenum diselenide/cobalt diselenide nanocomposite materials, can solve problems such as complicated operation, achieve simple raw materials, good electrocatalytic activity, and simple process equipment Effect

Inactive Publication Date: 2016-03-09
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above methods all adopt the preparation of binary chalcogenides in different forms to prepare composite materials, and the operation is more complicated.

Method used

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  • Preparation method of molybdenum diselenide/cobalt diselenide nanocomposite
  • Preparation method of molybdenum diselenide/cobalt diselenide nanocomposite
  • Preparation method of molybdenum diselenide/cobalt diselenide nanocomposite

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preparation example Construction

[0030] A preparation method of molybdenum diselenide / cobalt diselenide nanocomposite material, comprising the following steps:

[0031] Step 1: Add molybdate, cobalt salt and selenium dioxide into deionized water under the stirring condition of 200-500rpm, stir and mix evenly to obtain a mixed liquid; wherein, the concentration of molybdate is 0.002-0.05mol / L , the concentration of cobalt salt is 0.01~0.1mol / L, the concentration of selenium dioxide is 0.02~0.5mol / L;

[0032] Step 2: Under the stirring condition of 200~500rpm, add a complexing agent to the mixed solution obtained in step 1, and continue to stir until an emulsion is obtained; wherein, the volume ratio of the added complexing agent to the deionized water described in step 1 is 0.5~2;

[0033] Step 3: Transfer the emulsion obtained in step 2 to a stainless steel autoclave lined with polytetrafluoroethylene, place the autoclave in a heating furnace, and perform a hydrothermal reaction at a temperature of 160 to 24...

Embodiment 1

[0039] A preparation method of molybdenum diselenide / cobalt diselenide nanocomposite material, comprising the following steps:

[0040] Step 1: Dissolve 0.17mmol ammonium molybdate, 1.2mmol cobalt acetate and 4.8mmol selenium dioxide powder in 20mL deionized water under the stirring condition of 200rpm, and continue stirring until a uniform mixed solution A is obtained;

[0041] Step 2: Under the stirring condition of 200rpm, add 20mL of ethylenediamine as a complexing agent to the mixed solution A obtained in step 1, and keep stirring until the emulsion B is obtained;

[0042] Step 3: Transfer the emulsion B obtained in step 2 to a 100mL stainless steel autoclave lined with polytetrafluoroethylene, place the autoclave in a heating furnace, react at 180°C for 18h, and then cool naturally to room temperature, and transfer the solution C after the reaction in the autoclave to the beaker;

[0043] Step 4: The reacted solution C obtained in step 3 was subjected to high-speed cent...

Embodiment 2

[0048] A preparation method of molybdenum diselenide / cobalt diselenide nanocomposite material, comprising the following steps:

[0049] Step 1: Dissolve 0.26mmol ammonium molybdate, 1.2mmol cobalt acetate and 4.8mmol selenium dioxide powder in 20mL deionized water under the stirring condition of 300rpm, and continue stirring until a uniform mixed solution A is obtained;

[0050] Step 2: Under the stirring condition of 300rpm, add 20mL of ethylenediamine as a complexing agent to the mixed solution A obtained in step 1, and keep stirring until the emulsion B is obtained;

[0051] Step 3: Transfer the emulsion B obtained in step 2 to a 100mL stainless steel autoclave lined with polytetrafluoroethylene, place the autoclave in a heating furnace, react at 220°C for 20h, and then cool naturally to room temperature, and transfer the solution C after the reaction in the autoclave to the beaker;

[0052] Step 4: The reacted solution C obtained in step 3 was subjected to high-speed cent...

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Abstract

The present invention provides a preparation method of a molybdenum diselenide / cobalt diselenide nanocomposite, and belongs to the technical field of preparation of inorganic nanocomposites. The preparation method comprises the following steps: adding 0.002-0.05 mol / L of molybdate, 0.01-0.1 mol / L of cobalt salt and 0.02-0.5 mol / Lof molybdenum diselenide into deionized water to obtain mixed liquid at first; adding a complexing agent into the mixed liquid, and stirring to obtain emulsion, wherein the volume ratio of the complexing agent and the deionized water is 0.5-2; transferring the emulsion to an autoclave, reacting for 6-24 hours at the temperature of160-240 DEG C, after cooling down the reacted solution, centrifuging, washing and drying to obtain solid powder; and annealing the solid powder for 1-4 hours at the temperature of 400-600 DEG C. The method provided by the present invention has the advantages that raw materials and technological equipment are simple, production cost is low, and the molybdenum diselenide / cobalt diselenide nanocomposite is easy to produce in large scale; and the obtained composite is composed of a micro-tube which is obtained by nanosheets in a self-assembling manner, so that electrocatalytic activity is good.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic nanometer materials, and in particular relates to a method for preparing a molybdenum diselenide / cobalt diselenide nanocomposite material with a two-level hierarchical structure. Background technique [0002] Transition metal binary chalcogenides have a graphite-like layered structure, and the layers are combined by weak van der Waals forces, which have good optical / electrical properties, lubricity and catalytic activity. In the field of semiconductor material technology, because binary chalcogenides can form large-area single-layer or multi-layer sheet single crystals, they can be applied to the development of new semiconductor transistors; at the same time, due to their special crystal structure, they are easy to form under certain conditions. Nanostructures such as flake nanoparticles and nanoflowers have a high specific surface area, and atomic defects are prone to occur at th...

Claims

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Application Information

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IPC IPC(8): B01J27/057B82Y30/00B82Y40/00
CPCB01J27/0573B82Y30/00B82Y40/00
Inventor 宋远强慕春红齐红雪吴鹏邓凯
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA
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