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Method for preparing molybdenum carbide by gaseous reduction of molybdenum oxide

A technology of molybdenum carbide and molybdenum oxide, which is applied in the field of gaseous reduction of molybdenum oxide to prepare molybdenum carbide and gaseous reduction of molybdenum oxide to prepare ultra-fine molybdenum carbide, which can solve the problems of high cost and many impurities in the product

Active Publication Date: 2018-12-04
CENT SOUTH UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] Aiming at the obvious shortcomings of existing methods such as low efficiency, high cost, and many impurities in the product, the present invention proposes to use low-cost pure molybdenum trioxide or high-grade molybdenum calcined sand as raw materials, and efficiently prepare ultra- Fine molybdenum carbide, the obtained product has uniform appearance, fine particle size, high purity, and is easy to disperse

Method used

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  • Method for preparing molybdenum carbide by gaseous reduction of molybdenum oxide
  • Method for preparing molybdenum carbide by gaseous reduction of molybdenum oxide
  • Method for preparing molybdenum carbide by gaseous reduction of molybdenum oxide

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Embodiment 1

[0028] Using pure molybdenum trioxide (≥99.9%) powder as raw material, the steam generation temperature is controlled at 950°C, the reduction temperature is controlled at 1050°C, the molybdenum trioxide vapor is mixed with methane through nitrogen transport, and the molar ratio of reducing gas to volatile molybdenum trioxide is 3.5 , the mixed gas flows in the high temperature section for about 12s, and the solid product is obtained and cooled to room temperature under the protection of nitrogen. SEM detection shows that the product is a uniform nanosheet with a side length of 300-600nm and a thickness of 30-60nm, which is approximately hexagonal; XRD pattern shows that the product is pure molybdenum carbide, free carbon and uncarburized molybdenum oxide.

Embodiment 2

[0030] Using pure molybdenum trioxide (≥99.9%) powder as raw material, the steam generation temperature is controlled at 950°C, the reduction temperature is controlled at 1050°C, the molybdenum trioxide vapor is mixed with methane through nitrogen transport, and the molar ratio of reducing gas to volatile molybdenum trioxide is 3.5 , the flow time of the mixed gas in the high temperature section was extended to about 18s, and the solid product was obtained and cooled to room temperature under the protection of nitrogen. SEM inspection shows that most of the products are approximately hexagonal flakes with a side length of 300-600nm and a thickness of 50-150nm, but a small amount of coarse-grained layered molybdenum carbide also appears.

Embodiment 3

[0032] Using high-grade molybdenum calcined sand (60.47wt%) as raw material, the steam generation temperature is controlled at 1000°C, the reduction temperature is controlled at 1050°C, the molybdenum trioxide vapor is mixed with methane through nitrogen transport, and the molar ratio of reducing gas to volatile molybdenum trioxide is 3.5, the mixed gas flows in the high temperature section for about 12s, and the solid product is cooled to room temperature under the protection of nitrogen. SEM detection shows that the product is a uniform sheet with a side length of 300-600nm and a thickness of 50-150nm, which is approximately hexagonal; XRD pattern shows that the product is pure molybdenum carbide without free carbon and uncarburized molybdenum oxide.

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Abstract

The invention relates to a method for preparing molybdenum carbide by gaseous reduction of molybdenum oxide, in particular to a method for preparing ultrafine molybdenum carbide by gaseous reduction of molybdenum oxide, and belongs to the field of preparation of ultrafine materials. The method of the invention adopts pure molybdenum trioxide or high-grade molybdenum calcine as a raw material, theraw material is placed in a high-temperature furnace, an inert gas is used as a carrier gas, heating is performed at 800 to 1200 DEG C for generating a molybdenum trioxide vapor, then the generated molybdenum trioxide vapor is uniformly mixed with a reducing gas at 800 to 1200 DEG C, reduction is performed for 3-30 s, and then cooling is performed under protection of an inert gas, so that a molybdenum carbide powder is obtained. The method has the advantages of low cost, high preparation efficiency and good product quality, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for preparing molybdenum carbide by reducing molybdenum oxide in a gaseous state, in particular to a method for preparing ultrafine molybdenum carbide by reducing molybdenum oxide in a gaseous state, and belongs to the field of ultrafine material preparation. Background technique [0002] Molybdenum carbide has the characteristics of high melting point and hardness, good thermal and mechanical stability and excellent corrosion resistance, and is widely used as material coating and particle reinforcement. At the same time, molybdenum carbide also has catalytic properties similar to noble metals. It is considered to be an effective substitute for platinum-based materials in the fields of traditional organic synthesis, methanol batteries, and hydrogen production by electrolysis of water, and has great application prospects. The ultra-fine-scale molybdenum carbide has become the focus of development and research due to its...

Claims

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Application Information

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IPC IPC(8): C01B32/949B82Y40/00
CPCC01P2002/72C01P2004/03C01P2004/62C01P2004/64
Inventor 李光辉孙虎彭志伟饶明军张元波姜涛张鑫苏子键殷金虎
Owner CENT SOUTH UNIV
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