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Preparation method of molybdenum boride powder

A molybdenum boride and powder technology is applied in the field of preparation of new materials to achieve the effect of accelerating the reaction rate, improving the purity and realizing the crystal structure

Active Publication Date: 2017-01-04
LUOYANG GOLDEN EGRET GEOTOOLS
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Problems solved by technology

In his doctoral dissertation "Preparation and Properties of Molybdenum-Based Alloy High-Temperature Oxidation-Resistant Coatings", Wang Yi from Central South University used in-situ chemical vapor deposition to first deposit highly active boron on the molybdenum substrate, and then through the boron The in-situ diffusion reaction between the element and the molybdenum element in the matrix forms a layer of molybdenum boride (MoB) on the surface of the molybdenum matrix. This method has great limitations, and molybdenum boride must be formed on the molybdenum matrix Synthetic molybdenum boride can only be used as a coating on molybdenum substrates

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preparation example Construction

[0026] A preparation method of a new type of molybdenum boride powder material. This preparation method uses high temperature and high pressure to synthesize molybdenum boride powder for the first time. No similar synthesis method has been found in the current patents, reports, papers and other documents. Its specific preparation method comprises the following steps:

[0027] Step 1. First place B powder and Mo powder in graphite crucible and metal molybdenum crucible coated with BN powder on the inner wall, and use hydrogen reduction furnace for reduction. The reduction temperature of boron powder is 1000-1500 °C, and the reduction temperature of molybdenum powder 600-1200℃;

[0028] Step 2: Put the reduced B powder and Mo powder into the ball mill mixing tank for 2-96 hours according to the molar ratio of 0.5 or 1 or 2 or 2.5 or 4, wherein the ball milling medium is edible alcohol, Both the ball milling jar and balls are made of polytetrafluoroethylene;

[0029] Step 3. Po...

Embodiment 1

[0033] (1) First place the B powder and Mo powder in the graphite crucible and the metal molybdenum crucible coated with BN powder on the inner wall respectively, and use a hydrogen reduction furnace for reduction. The reduction temperature of the boron powder is 1200 ° C, and the reduction temperature of the molybdenum powder is 1050 ° C. ℃;

[0034] (2) Put the reduced B powder and Mo powder into the ball mill mixing tank according to the molar ratio of 1:1, and ball mill them for 48 hours. The ball milling medium is edible alcohol. The material of vinyl fluoride;

[0035] (3) Pour the ball-milled mixture into a stainless steel tray, and then place it in a vacuum drying oven for drying at a drying temperature of 100°C;

[0036] (4) Transfer the dried material in step 3 to a graphite crucible coated with BN powder on the inner wall, then place the graphite crucible in a high-temperature and high-pressure container, and control the pressure in the container to 20 GPa at 3 °C ...

Embodiment 2

[0039] (1) First place the B powder and Mo powder in the graphite crucible and the metal molybdenum crucible coated with BN powder on the inner wall respectively, and use a hydrogen reduction furnace for reduction. The reduction temperature of the boron powder is 1200 ° C, and the reduction temperature of the molybdenum powder is 1050 ° C. ℃;

[0040] (2) Put the reduced B powder and Mo powder into the ball mill mixing tank according to the molar ratio of 1:1, and ball mill them for 48 hours. The ball milling medium is edible alcohol. The material of vinyl fluoride;

[0041] (3) Pour the ball-milled mixture into a stainless steel tray, and then place it in a vacuum drying oven for drying at a drying temperature of 100°C;

[0042] (4) Transfer the dried material in step 3 to a graphite crucible coated with BN powder on the inner wall, then place the graphite crucible in a high-temperature and high-pressure container, and control the pressure in the container to 28 GPa at 3 °C ...

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Abstract

The invention provides a preparation method of molybdenum boride powder. In the preparation steps, the molybdenum boride powder which completely accords with material design phase compositions can be controlled to be prepared by means of a high-temperature and high-pressure synthesis mode according to setting of the B / Mo mole ratio n (n=0.5, 1, 2, 2.5, 4) before synthesis, controllable synthesis of target molybdenum boride material phase compositions is achieved, and the synthesized molybdenum boride powder is uniform in particle size, complete in grain crystallization and excellent in property. The method is controllable in technological process, short in technological route, high in targeted property, convenient to operate, efficient, economical in energy, safe and good in reliability. The finished molybdenum boride powder is uniform in particle size distribution and complete in grain crystallization, the chemical purity is higher than or equal to 99.8%, and the product quality stability is good, the properties are obviously improved compared with a molybdenum boride material synthesized through a conventional method, and therefore the produced molybdenum boride material shows excellent physical and chemical properties in industrial application.

Description

technical field [0001] The invention relates to the technical field of preparation of novel materials, in particular to a preparation method of molybdenum boride powder. Background technique [0002] Molybdenum boride series compounds have the characteristics of high melting point, high hardness, wear resistance, high temperature resistance, corrosion resistance and low friction coefficient. They play an extremely important role in modern industry and are widely used in alloy materials, coatings materials, high-temperature structural materials, cathode materials, corrosion-resistant materials, wear-resistant materials and other fields, and with the advancement of science and technology, the application field of molybdenum boride compounds will be further expanded, and this material will show more excellent Application value and huge market prospect. [0003] According to the binary phase diagram of Mo-B, the molybdenum boride compound can be Mo 2 B, α-MoB, β-MoB, MoB 2 、M...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/04
CPCC01B35/04C01P2002/72C01P2004/03C01P2006/80Y02P20/10
Inventor 谢屹峰杨跃刘宝刚张国峰
Owner LUOYANG GOLDEN EGRET GEOTOOLS
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