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Method for preparing nano-scale molybdenum powder

A nano-scale, molybdenum powder technology, applied in the field of ultrafine metal powder preparation, can solve the problems of low process yield, unsuitable for large-scale production, and high production cost, and achieves short process flow, difficult grain growth, and production cost. low effect

Inactive Publication Date: 2008-12-17
JIANGSU GUANGMING NEW MATERIAL
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  • Claims
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Problems solved by technology

The methods for preparing molybdenum powder in the prior art include molybdenum chloride steam method, plasma reduction method, carbonyl thermal decomposition method, hydrogen reduction vapor deposition method and microwave plasma method. The raw materials used in these methods are ammonium molybdates or molybdates, and the prepared The particle size of molybdenum powder is at the micron level, and molybdenum powder with a particle size of nanometer level can also be prepared by adjusting the process flow, but the production cost is high and the process yield is low, so it is not suitable for large-scale production

Method used

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[0019] The nanoscale molybdenum powder preparation method of the present invention adopts the nanoscale ammonium octamolybdate having a particle diameter less than 100nm as a raw material, and adopts two reduction methods to prepare, and the preparation process includes the following steps:

[0020] (1) Spread the raw materials evenly in the burning boat, with a thickness of 6-13mm;

[0021] (2) For the first reverse reduction treatment, the reduction condition is furnace temperature 380-560°C, the reducing agent is hydrogen produced by water electrolysis, and the hydrogen flow rate is 20-50m 3 / h, dew point ≤ -30°C, the residence time of raw materials in the furnace is 90-180min;

[0022] (3) For the second reverse reduction treatment, the reduction condition is furnace temperature 600-750°C, the reducing agent is hydrogen produced by water electrolysis, and the hydrogen flow rate is 60-100m 3 / h, dew point ≤ -30°C, raw material residence time in the furnace is 120-180min. ...

Embodiment

[0024] This embodiment is carried out in a 160KW four-tube furnace, and the raw material used is nano-scale ammonium octamolybdate, and its quality analysis test results are shown in Table 1. The burning boat used is made of molybdenum, the size is 390×280×40mm, and the charging thickness is between 10.5 and 12.5mm. The hydrogen produced by water electrolysis is used as the reverse reducing agent, the dew point is ≤ -30°C, the reduction reaction is carried out in a closed environment, and the recovered hydrogen is recycled after being deoxygenated and dried.

[0025] According to the above-mentioned technological process, the relevant reduction conditions were appropriately changed, and the embodiment operations were carried out in batches. The quality analysis and test results of the finished products were shown in Table 2 below.

[0026] Table 1: Analysis and test results of raw materials (nano-scale ammonium octamolybdate)

[0027]

[0028] Table 2: The quality analysis...

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Abstract

The invention discloses a preparation method for nanometer molybdenum powder, and the method takes nanometer ammonium octamolybdate as raw material. In a closed environment, hydrogen backward reduction reaction is carried out twice, and the prepared nanometer molybdenum powder is purple and is of grain diameter of 55 to 92nm and the average purity of above 99.80 percent by controlling the furnace temperature and the hydrogen flow in the first reduction and the second reduction. In the invention, the hydrogen can be recycled, thus saving the production cost, and the method also has the advantages of short process flow, easy control of process conditions, no special requirement on production equipment and being suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of ultrafine metal powder, in particular, the invention relates to a preparation method of molybdenum powder with a particle size of nanometer. Background technique [0002] Molybdenum is a rare metal with good physical properties and is widely used in steel industry, electronics industry, aerospace and agriculture. For example, adding an appropriate amount of molybdenum during iron and steel smelting can significantly improve the strength, toughness, corrosion resistance and heat resistance of steel. The particle size of molybdenum powder has a very significant impact on its addition effect. Practice has proved that the finer the particle size of molybdenum powder, the better the addition effect. More prominent, especially in the molybdenum powder spraying process, the sprayed surface structure is dense and uniform. The methods for preparing molybdenum powder in the prior art include molybdenum chloride ...

Claims

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Application Information

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IPC IPC(8): B22F9/22
Inventor 丁舜
Owner JIANGSU GUANGMING NEW MATERIAL
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