Preparation method of coralline high-purity tantalum powder

A coral-like and high-purity technology is applied in the field of preparation of coral-like high-purity tantalum powder.

Active Publication Date: 2019-10-11
CONGHUA TANTALUM & NIOBIUM SMELTERY
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Problems solved by technology

At present, the preparation of high-purity tantalum powder generally adopts the method of reducing potassium fluorotantalate by metal sodium. The common problems are: high metal impurities, high melting point metal impurities in the prepared tantalum powder W>1ppm, Mo>1ppm, Nb>3ppm , these impurities have a high melting point and cannot be effectively removed, causing them to remain on the tantalum target, high-quality furnace materials, and high-purity tantalum rod plates, and the oxygen content of the tantalum powder is high, requiring subsequent purification processes such as magnesium deoxidation, resulting in higher production costs
[0003] Chinese patent CN104148654A provides a method for preparing target-grade high-purity tantalum powder. This method is also the reduction of potassium fluorotantalate by metal sodium. The focus is on pickling and impurity removal, and it also includes high-temperature sintering, magnesium oxygen reduction process and oxygen acid reduction. Washing steps, the disadvantage of this patent is that the subsequent magnesium deoxidation and purification process is added, and impurity magnesium is added, and the cost is higher
[0004] Chinese patent CN103447544A provides a method for preparing high-purity tantalum powder with centralized and controllable particle size distribution. This method is to make tantalum powder into high-purity tantalum ingot, then hydrogenate it to make powder, and then dehydrogenate it into high-purity tantalum powder. There are high energy consumption and production costs in subsequent processing. high problem
[0005] Chinese patent CN102994780A provides a method for purifying tantalum powder. This method focuses on pickling and impurity removal. However, the pickling process is complicated and the oxygen content is very high

Method used

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  • Preparation method of coralline high-purity tantalum powder

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Effect test

Embodiment 1

[0034] The preparation method of coral-shaped high-purity tantalum powder comprises the following steps:

[0035] (1) Heat needle-shaped high-purity potassium fluorotantalate to 350°C for 10 hours in a vacuum activation furnace to activate the needle-shaped potassium fluorotantalate into powdery high-purity potassium fluorotantalate. Among them, high-purity fluorotantalate W content in potassium tantalate ≤ 1ppm, Mo content ≤ 1ppm, Nb content ≤ 1ppm;

[0036] (2) Heat the diluent NaCl to 60°C in a drying oven for 22 hours, so that NaCl does not contain moisture;

[0037] (3) Filter and purify metallic sodium through a molten sodium system to obtain purified sodium, in which Na≥99.9w / w%, K≤0.003w / w%, Fe≤0.001w / w%, and heavy metals≤0.005w / w%, C content ≤ 30ppm, the filtration and purification process of the molten sodium system is as follows: heat the metal sodium to 150°C for melting, then remove oil at 130°C and -0.08MPa vacuum, and use a stainless steel mesh for coarse filt...

Embodiment 2

[0044] The preparation method of coral-shaped high-purity tantalum powder comprises the following steps:

[0045] (1) Heat the needle-shaped high-purity potassium fluorotantalate in a vacuum activation furnace to 300°C for 8 hours to activate the needle-shaped potassium fluorotantalate into powdery high-purity potassium fluorotantalate. W content in potassium tantalate ≤ 1ppm, Mo content ≤ 1ppm, Nb content ≤ 1ppm;

[0046] (2) Heat the diluent NaCl to 100°C in a drying oven for 20 hours, so that NaCl does not contain moisture;

[0047] (3) Filter and purify metallic sodium through a molten sodium system to obtain purified sodium, in which Na≥99.9w / w%, K≤0.003w / w%, Fe≤0.001w / w%, and heavy metals≤0.005w / w%, C content ≤ 30ppm, the filtration and purification process of the molten sodium system is as follows: heat the metal sodium to 150°C for melting, then remove oil at 130°C and -0.08MPa vacuum, and use a stainless steel mesh for coarse filtration at 130°C Then use a ceramic ...

Embodiment 3

[0054] The preparation method of coral-shaped high-purity tantalum powder comprises the following steps:

[0055] (1) Heat needle-shaped high-purity potassium fluorotantalate to 320°C for 12 hours in a vacuum activation furnace to activate the needle-shaped potassium fluorotantalate into powdery high-purity potassium fluorotantalate. Among them, high-purity fluorotantalate W content in potassium tantalate ≤ 1ppm, Mo content ≤ 1ppm, Nb content ≤ 1ppm;

[0056] (2) Heat the diluent NaCl in the drying oven to 80°C for 24 hours, so that NaCl does not contain moisture;

[0057] (3) Filter and purify metallic sodium through a molten sodium system to obtain purified sodium, in which Na≥99.9w / w%, K≤0.003w / w%, Fe≤0.001w / w%, and heavy metals≤0.005w / w%, C content ≤ 30ppm, the filtration and purification process of the molten sodium system is as follows: heat the metal sodium to 150°C for melting, then remove oil at 130°C and -0.08MPa vacuum, and use a stainless steel mesh for coarse fi...

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Abstract

The invention provides a preparation method of coralline high-purity tantalum powder, and the mehtod comprises the following steps of (1) activating needle-shaped potassium fluotantalate into powder;(2) making NaCl free of water; (3) filtering and purifying the metal sodium to obtain purified sodium; (4) filling powdery potassium fluotantalate and NaCl into a reduction tank, hoisting the reduction tank into a well chamber reduction furnace, vacuumizing, filling argon for replacement, heating to 100 DEG C, inputting purified sodium, and continuously heating; (5) when the temperature increasesto 750 DEG C, carrying out sodium reduction; (6) after the sodium injection is finished, keeping constant temperature, lifting out the reduction tank, naturally cooling, taking out and crushing into amixture; (7) washing with water and acid to obtain washing powder; and (8) carrying out heat treatment on the washing powder, taking out of the furnace, sieving, and analyzing the qualified undersizeto obtain the coralline high-purity tantalum powder. By controlling the reaction process of preparing the tantalum powder by reducing potassium fluotantalate with the sodium metal, the preparation method of coralline high-purity tantalum powder can absorb metal impurities as little as possible and prevent the reaction product metal tantalum from being oxidized, and can directly prepare the coralliform high-purity tantalum powder with low metal impurity content and low oxygen content.

Description

technical field [0001] The invention relates to a preparation method of high-purity tantalum powder, in particular to a preparation method of coral-like high-purity tantalum powder. Background technique [0002] Tantalum is a rare metal with a high melting point. It is a special functional material with excellent performance. It is widely used in high-end technical fields such as communications, computers, automotive electronics, missiles, aerospace, and automatic control devices. Used for tantalum targets, high-quality furnace materials and high-purity tantalum rods and plates. At present, the preparation of high-purity tantalum powder generally adopts the method of reducing potassium fluorotantalate by metal sodium. The common problems are: high metal impurities, high melting point metal impurities in the prepared tantalum powder W>1ppm, Mo>1ppm, Nb>3ppm , these impurities have a high melting point and cannot be effectively removed, causing them to remain on the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/20B22F1/00
CPCB22F1/0007B22F9/20
Inventor 月日辉郑辉权周丽
Owner CONGHUA TANTALUM & NIOBIUM SMELTERY
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