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Method for processing microtantalum and/or niobium powder and powder made by said method

A processing method and fine technology, which is applied in the processing of fine tantalum and/or niobium powders and the powders produced therefrom, can solve the problems of inability to be exposed for a long time, no practical value, etc., and achieve good stability

Inactive Publication Date: 2003-10-22
NINGXIA ORIENT TANTALUM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This kind of fine tantalum and niobium powder has high activity, it will be oxidized rapidly when in contact with oxygen-containing medium, and cannot be exposed to the air for a long time, so it has little practical value

Method used

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  • Method for processing microtantalum and/or niobium powder and powder made by said method
  • Method for processing microtantalum and/or niobium powder and powder made by said method
  • Method for processing microtantalum and/or niobium powder and powder made by said method

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Put the fine tantalum powder obtained by the same method as the above comparative example into a tantalum crucible in a glove box filled with argon, and place the crucible with the sample above in a quartz tube container to seal, and place the quartz tube container Remove from glove box. Insert the quartz tube container into a heating furnace to evacuate. After evacuating until the pressure is lower than 1 Torr, fill it with argon to 1 atmospheric pressure, then carry out evacuation to 10-3 Torr, and raise the temperature to 500°C in 150 minutes. Maintain the pressure in the quartz tube container below 10 -3 Torr, the furnace temperature was 500° C. for 360 minutes, then cooled to room temperature, and after passivation for 20 minutes, the sample was taken out to obtain 2.2 grams of tantalum powder. The chemical composition of the tantalum powder was analyzed, and the data are listed in Table 1. The TEM image of tantalum powder is attached image 3 shown. Table 2 sh...

Embodiment 2

[0025] With 4.0 g NbCl 5 and 1.8 grams of Na are respectively dissolved in liquid ammonia at -40°C, and black niobium powder is formed after mixing and reacting, and then the above niobium powder is mixed with NaCl, NH 3 , Na to separate to obtain fine niobium powder. Above-mentioned fine niobium powder is carried out heat treatment the same as embodiment 1, is kept at 700 ℃ for 300 minutes and keeps the pressure in the quartz tube container always about 10 -2 Torr, and then cooled to room temperature, after 20 minutes of passivation, the sample was taken out, washed with deionized water and then vacuum-dried at 50°C to obtain 1.2 g of niobium powder. The chemical composition of niobium powder was analyzed, and the data are listed in Table 1. The TEM image of niobium powder is attached Figure 4 shown.

Embodiment 3

[0027] Same as embodiment 1, vacuumize to 10 -3Torr, the temperature was raised to 300° C. and filled with argon gas, and then the argon gas was kept flowing. Then, the temperature was raised to 900° C. and kept for 240 minutes to obtain 2.1 grams of tantalum powder. The chemical composition of the tantalum powder was analyzed, and the data are listed in Table 1. The TEM image of tantalum powder is attached Figure 5 shown. Table 2 shows the changes in oxygen content of tantalum powder exposed to air at a temperature of 20-35°C and a relative humidity of 30%-80% for 48 hours.

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Abstract

The present invention relates to a new treatment method for preparing microfine tantalum and / or niobium powder, specially, it relates to a method capable of making halide of tantalum and / or niobium mix with reduced metal in the liquid ammonia and produce reaction to produce microfine tantalum and / or niobium powder and making them undergo the processes of heat treatment and subsequent treatment at high-temp. in the non-oxidation atmosphere. The tantalum and / or niobium powder prepared according to the invented method is a kind of relatively-stable microfine nano-grade powder.

Description

technical field [0001] The present invention relates to a new processing method for preparing fine tantalum and / or niobium powders, in particular to a kind of fine tantalum and / or niobium powders produced by mixing and reacting tantalum and / or niobium halides and reducing metals in liquid ammonia. Treatment methods before contact with oxygen-containing media. Background technique [0002] Tantalum and niobium have similar properties, both of which are high-melting point metals. They have good chemical stability to inorganic acids except hydrofluoric acid, but have high activity to elements such as O, N, and C. Tantalum, niobium or nitrogen-containing tantalum and niobium are used to manufacture electrolytic capacitors, high temperature and corrosion resistant materials, superalloys, hard alloys, spraying protective layers and copper diffusion barrier layers for integrated circuits, etc. Especially when it is used as an electrolytic capacitor, it is required to have a fine p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F1/00B22F9/24
Inventor 朱鸿民何季麟乔芝郁李海军孙根生潘伦桃曹战民郑世萍马春红吕建波赵春霞
Owner NINGXIA ORIENT TANTALUM IND
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