Preparation method of micro-nano molybdenum carbide powder

A micro-nano, molybdenum carbide technology, applied in the direction of carbides, tungsten/molybdenum carbides, etc., can solve problems such as difficulty in popularization, complex structure and preparation process of metal complexes, expensive ligands, etc., to reduce airtightness Effects of sexual dependence, prevention of mutual association, and shortened reaction time

Inactive Publication Date: 2017-11-17
DONGGUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Through the design and selection of metal complexes, people can obtain molybdenum carbide materials with different shapes; however, the structure and preparation process of metal complexes are generally more complicated, and the price of ligands is relatively expensive, which is difficult to obtain in large-scale preparation and use. universal

Method used

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  • Preparation method of micro-nano molybdenum carbide powder
  • Preparation method of micro-nano molybdenum carbide powder
  • Preparation method of micro-nano molybdenum carbide powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Mix 1.356 grams of lithium chloride and 1.644 grams of potassium chloride and use it as a molten salt (melting point: 353 ° C), then add 1.26 grams of melamine and 0.63 grams of ammonium molybdate, and grind for 20 minutes; the above solid mixture is placed in an oxidation chamber with a lid. Aluminum ceramic crucible (capacity 30mL). The crucible containing the reaction precursor and the molten salt is placed in the middle of the microwave muffle furnace, and microwave heat treatment is performed in an air environment. The microwave treatment conditions are as follows: the temperature is raised from room temperature to 750°C at a rate of 10°C / min, and the temperature is kept at 750°C for 2 hours. After the reaction was completed and the sample was cooled, the obtained solid was washed with distilled water for more than 3 times to dissolve potassium chloride and lithium chloride, and dried at 80°C for 12 hours to obtain molybdenum carbide micro-nano powder.

[0044] In...

Embodiment 2

[0047] After mixing 1.356 g of lithium chloride and 1.644 g of potassium chloride uniformly, it was used as a molten salt medium (melting point: 353° C.), and then 1.26 g of melamine and 0.63 g of ammonium molybdate were added and ground for 20 minutes. The solid mixture obtained above was put into an alumina ceramic crucible (capacity 30 mL) with a lid. Place the crucible in the middle of the resistance muffle furnace, and heat it in the air environment: raise the temperature from room temperature to 750°C at a rate of 10°C / min, and keep it warm for 10h; after cooling, wash the obtained solid with distilled water for several The second time, potassium chloride and lithium chloride were dissolved and dried at 80°C for 12 hours to obtain molybdenum carbide.

[0048] In this embodiment, the mass ratio of melamine to molten salt is 42:100, the molar ratio of lithium chloride to potassium chloride is 59.2%:40.8%, and the mass ratio of melamine to ammonium molybdate is 2:1.

[004...

Embodiment 3

[0051] Mix 1.356 grams of lithium chloride and 1.644 grams of potassium chloride evenly as molten salt (melting point of molten salt: 353°C), add 1.26 grams of melamine and 0.63 grams of ammonium molybdate; after grinding for 20 minutes, put the above solid mixture into an alumina ceramic crucible (capacity 30ml). Place the crucible in the middle of the microwave muffle furnace, and process it in an air environment: raise the temperature from room temperature to 850°C at a rate of 10°C / min, and keep it warm for 4 hours; after cooling, wash the obtained solid with distilled water for several times , Dissolve potassium chloride and lithium chloride, and dry at 80°C for 12 hours to obtain molybdenum carbide.

[0052] In this embodiment, the mass ratio of melamine to molten salt is 42:100, the molar ratio of lithium chloride to potassium chloride is 59.2%:40.8%, and the mass ratio of melamine to ammonium molybdate is 2:1.

[0053] From Figure 6 It can be seen that the crystal p...

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Abstract

The invention discloses a preparation method of micro-nano molybdenum carbide powder. The preparation method comprises the specific steps that an organic precursor serves as a carbon source, molybdate serves as a molybdenum source, fused salt serves as a reaction medium, high-temperature processing, washing and drying are conducted in sequence in an air environment, and the micro-nano molybdenum carbide powder is prepared. The preparation method is quick in reaction speed, and the reaction time is effectively shortened. Besides, the fused salt exists between the generated solid-phase molybdenum carbide particles in the reaction process, so that the mutual bonding between the particles can be stopped, and the agglomeration phenomenon can be reduced. In the method, no special atmospheric conditions are needed, the micro-nano molybdenum carbide material can be prepared at a relatively low temperature; the process is simple, the preparation conditions are mild, and a large scale of production is easy to achieve.

Description

Technical field: [0001] The invention relates to the field of synthesis of nanomaterials, in particular to a method for preparing molybdenum carbide micro-nano powder. Background technique: [0002] With the gradual depletion of traditional fossil energy and the increasingly prominent environmental problems, the search for green and sustainable energy has become the focus of attention. Hydrogen, as an ideal clean energy, has the advantages of environmental protection, high energy density, and wide range of sources, and has attracted widespread attention. However, there are no natural deposits of hydrogen in nature, so hydrogen needs to be generated artificially. At present, hydrogen production methods are mainly divided into three types, namely natural gas method, water gas method and electrolysis water method. Among them, the electrolytic water method is safe, pollution-free, and low in energy consumption, and people pay more and more attention to it. [0003] In the ele...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/949
CPCC01P2002/72C01P2004/03
Inventor 陈德良王志强李涛徐勇军
Owner DONGGUAN UNIV OF TECH
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