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An industrial method for preparing tungsten powder with low impurity content

An industrial method and low-impurity technology, applied in lighting and heating equipment, furnaces, crucible furnaces, etc., can solve the problems that quartz tubes are easily broken, mass production cannot be realized, and industrial production is difficult to achieve.

Active Publication Date: 2019-07-09
厦门朋鹭金属工业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method uses high-purity quartz as the furnace tube in the stage of reducing tungsten powder. So far, there is no large-scale high-purity quartz reduction furnace in the industry, and continuous mass production cannot be realized. Moreover, the quartz tube is easily broken during the production process, and the production cost High, this method is difficult to realize in industrial production

Method used

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  • An industrial method for preparing tungsten powder with low impurity content
  • An industrial method for preparing tungsten powder with low impurity content
  • An industrial method for preparing tungsten powder with low impurity content

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 1. Prepare the boat:

[0033] In the raw material preparation process: prepare 99.9% of purity Cr, 99.9% of purity Ni, 99.9% of purity Fe and 99.9% of purity Ta, prepare by mass percentage wt%. The content of each element is shown in Table 2. Each serial number group was prepared according to the element composition in Table 2, and 8Kg of raw materials were weighed and prepared respectively.

[0034] The raw materials prepared in each embodiment were put into alumina crucibles, vacuum smelted in a vacuum induction melting furnace, and poured into investment molds to obtain boats. The properties of the boats are shown in Table 2.

[0035] Proportion and performance of each element in table 2

[0036]

[0037] The detection of the yield strength in the present invention is carried out at normal temperature, but we found in the production process that the normal temperature yield strength has a corresponding relationship with the high temperature yield strength, the hi...

Embodiment 2

[0056] 1. Prepare the boat:

[0057] In the raw material preparation process: prepare Cr, Fe, Ta, Nb, Ni, C, B, Al and Ti with a purity of 99.9%, and prepare them in wt%. Each serial number group was prepared according to the element composition in Table 6, and 8Kg of raw materials were weighed and prepared respectively.

[0058] The raw materials prepared in each embodiment and comparative example were put into a crucible made of alumina, vacuum smelted in a vacuum induction melting furnace, and poured into an investment mold to obtain a boat. The boat performance of each embodiment, comparative example is as shown in table 6:

[0059] Proportioning (wt%) and performance of each element of table 6

[0060]

[0061] 2. Reduction reaction:

[0062] Add tungsten trioxide as shown in Table 3 to the boats obtained in each embodiment.

[0063] The loading capacity of the boat is controlled at 1.1kg; the pushing speed is controlled at 11min; the hydrogen flow rate is controll...

Embodiment 3

[0072] The difference between Example 3.1, Example 3.2, and Comparative Example 3.1 and Example 1.1 is that tungsten trioxide with the composition shown in Table 8 is added to the boat obtained in Example 1.1.

[0073] The difference between Comparative Example 3.2 and Comparative Example 1 is that tungsten trioxide with the composition shown in Table 8 is added to the boat obtained in Comparative Example 1.

[0074] The proportioning (wt%) of each element of table 8

[0075]

[0076] The loading capacity of the boat is controlled at 1.1Kg; the pushing speed is controlled at 11 minutes; the hydrogen flow rate is controlled at 25m 3 / h, its purity is greater than 99.999%; H 2 Dew point: 0°C to 10°C; reduction temperature is divided into three zones and controlled respectively at: 860°C to 870°C, 970°C to 980°C, and 970°C to 980°C, and the reduction time for each stage is 150 minutes to obtain W powder.

[0077] The content detection result of W powder Cr, Ni, Fe and 200 me...

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Abstract

The invention discloses an industrial method for preparing low-impurity-content tungsten powder. The industrial method comprises the following steps that raw material ammonium paratungstate (APT) is put into a rotary furnace pipe through a screw feeding mechanism and is calcined to form tungsten trioxide, the tungsten trioxide is put into a boat, H2 reduction is conducted under the temperature of 800 DEG C-1000 DEG C, and the tungsten powder is obtained; the boat comprises the following components of, by weight, 25%-29% of Cr, 20%-35% of Fe, 2%-4% Ta and / or Nb, 0.1% or less of C, 0.8 % or less of B, 0.5% or less of Al, 0.5% or less of Ti, and the balance Ni and unavoidable impurities; the Cl content of the raw material ammonium paratungstate is 10 ppm or less, and the Cl content of the tungsten trioxide is 10 ppm or less. Through the preparation method, the impurity content during tungsten powder manufacturing can be controlled effectively.

Description

technical field [0001] The invention relates to a method for preparing tungsten powder, in particular to an industrial method for preparing tungsten powder with low impurity content. Background technique [0002] High-purity tungsten above 5N has high resistance to electron migration, high temperature stability, and the ability to form stable silicides, and is widely used as gate circuit electrode materials for large-scale integrated circuits. At present, there are two key points in the preparation of high-purity tungsten powder: 1) The improvement of smelting and purification technology, the purity of raw materials meets the corresponding purity requirements; 2) The preparation process of tungsten powder is clean, and the pollution of impurities is reduced in the production process. [0003] Liu Wensheng et al. pointed out in the "Research Status and Preparation Process of High-purity Tungsten" (Powder Metallurgy Technology, 2012, 30-3: 223-228) that the traditional prepara...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F9/22F27B14/10C22C19/05C22C30/00
CPCB22F9/22C22C19/058C22C30/00C22C38/06C22C38/48C22C38/50C22C38/54F27B14/10
Inventor 林高安陈杉杉周军姜春辉曹友东谢颖
Owner 厦门朋鹭金属工业有限公司
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