Method for preparing high-melting-point metal powder through multistage depth reduction

一种高熔点金属、深度的技术，应用在金属加工、工艺效率的提高、可持续制造/加工等方向，能够解决设备和安全的要求高等问题，达到设备要求低、工艺高效、工艺条件和仪器设备要求低的效果

Active Publication Date: 2017-10-10
NORTHEASTERN UNIV LIAONING
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  • Description
  • Claims
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Problems solved by technology

The introduction of hydrogen makes the process have high requirements for equipment and safety

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  • Method for preparing high-melting-point metal powder through multistage depth reduction

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Experimental program
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Effect test

Embodiment 1

[0056] A method for preparing high-melting-point metal powder by multi-stage deep reduction is carried out according to the following steps:

[0057] Step 1, self-propagating reaction

[0058] Put the tungsten oxide powder in an oven and dry at 100-150°C for 24 hours to obtain the dried tungsten oxide powder. The molar ratio of the dried tungsten oxide powder and magnesium powder is WO 3 : Mg=1:1 mixed to obtain a mixed material, press the mixed material at 20MPa to obtain a block billet, put it into a self-propagating reaction furnace, and initiate a self-propagating reaction by means of partial ignition, the temperature is controlled at 500 ° C, after cooling , to obtain the subvalent oxide Me of the refractory metal x The intermediate product of O dispersed in the MgO matrix; among them, the subvalent oxide Me of the refractory metal x The intermediate product of O dispersed in the MgO matrix is ​​a mixture of non-stoichiometric metal oxides with low valence and high melt...

Embodiment 2

[0068] A method for preparing high-melting-point metal powder by multi-stage deep reduction is carried out according to the following steps:

[0069] Step 1, self-propagating reaction

[0070] Put the tungsten oxide powder in an oven and dry at 100-150°C for 24 hours to obtain the dried tungsten oxide powder. The molar ratio of the dried tungsten oxide powder and magnesium powder is WO 3 : Mg=1:1.2 mixed to obtain a mixed material, press the mixed material under 10MPa to obtain a block billet, put it into a self-propagating reaction furnace, and initiate a self-propagating reaction by means of partial ignition, the temperature is controlled at 750 ° C, after cooling , to obtain the subvalent oxide Me of the refractory metal x The intermediate product of O dispersed in the MgO matrix; among them, the subvalent oxide Me of the refractory metal x The intermediate product of O dispersed in the MgO matrix is ​​a mixture of non-stoichiometric metal oxides with low valence and high...

Embodiment 3

[0080] A method for preparing high-melting-point metal powder by multi-stage deep reduction is carried out according to the following steps:

[0081] Step 1, self-propagating reaction

[0082] Put the tungsten oxide powder in an oven and dry at 100-150°C for 24 hours to obtain the dried tungsten oxide powder. The molar ratio of the dried tungsten oxide powder and magnesium powder is WO 3 :Mg=1:0.8 mixed to obtain a mixed material, press the mixed material at 60MPa to obtain a block billet, put it into a self-propagating reaction furnace, and initiate a self-propagating reaction by means of partial ignition, the temperature is controlled at 650 ° C, after cooling , to obtain the subvalent oxide Me of the refractory metal x The intermediate product of O dispersed in the MgO matrix; among them, the subvalent oxide Me of the refractory metal x The intermediate product of O dispersed in the MgO matrix is ​​a mixture of non-stoichiometric metal oxides with low valence and high mel...

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Abstract

The invention discloses a method for preparing high-melting-point metal powder through multistage depth reduction, and belongs to the technical field of powder preparing. The method comprises the steps that dried high-melting-point metallic oxide powder and magnesium powder are mixed and then subject to the self-propagating reaction, and high-melting-point metal Me is one or several of W, Mo, Ta, Nb, V, Zr, Hf or Re; intermediate products are placed in a seal reaction kettle, hydrochloric acid serves as a leaching agent to carry out leaching, and low-valence oxide MexO precursor of low-valence high-melting-point metal is obtained; the precursor is evenly mixed with calcium powder to be pressed, a mixture is placed in a vacuum reduction furnace, heating is carried out to enable the temperature to rise to 700 DEG C to 1200 DEG C, deep reduction is carried out for 1 h to 6 h, hydrochloric acid serves as the leaching agent to carry out leaching on a deep reduction product, and through treatment, high-melting-point metal powder is obtained. The method is low in raw material cost, easy to operate, and low in requirement for process and instrument equipment, the foundation is laid for industrial production, and the high-melting-point metal powder has the beneficial effects of being high in purity, controllable in granularity distribution, high in powder activity and the like.

Description

technical field [0001] The invention belongs to the technical field of powder making in the powder metallurgy process, and in particular relates to a method for preparing high-melting-point metal powder through multi-stage deep reduction. Background technique [0002] High melting point metals, also known as "refractory metals". Usually refers to tungsten, molybdenum, niobium, tantalum, vanadium, zirconium, and can also include hafnium and rhenium. This type of metal is characterized by high melting point, high strength, and strong corrosion resistance. Most of them can form compounds with high melting point, high hardness and good chemical stability with carbon, nitrogen, silicon, boron, etc. [0003] Zirconium is a metal with a high melting point. It has a small thermal neutron capture cross-section and outstanding nuclear performance. It is an indispensable material for the development of the atomic energy industry. Tantalum is one of the rare metal resources. It has mo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B34/00B22F9/20
CPCC22B34/00B22F9/20C22B34/14C22B34/20C22B34/24C22B34/34C22B34/36C22B5/04C22B5/18C22B61/00C22C1/045C22C1/0458B22F2201/01B22F2201/20B22F2003/241B22F2998/10B22F9/24B22F2301/20
Inventor 张廷安豆志河刘燕范世钢张子木吕国志赵秋月牛丽萍傅大学张伟光
Owner NORTHEASTERN UNIV LIAONING
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