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A kind of preparation method of target grade high-purity tantalum powder

A tantalum powder and high-purity technology is applied in the field of preparation of target-grade high-purity tantalum powder, which can solve the problem of high manufacturing cost and achieve the effect of improving purity, reducing cost and high purity.

Active Publication Date: 2019-08-16
NINGXIA ORIENT TANTALUM IND +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method is too expensive to manufacture

Method used

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  • A kind of preparation method of target grade high-purity tantalum powder

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Experimental program
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Effect test

Embodiment 1

[0026] The sodium-reduced tantalum powder is prepared by using NaCl as the dilution salt. After the reduction, the mixed bulk material of the sodium-reduced tantalum powder and the diluted salt NaCl is added to pure water for filtration and washing for 10 hours. When the conductivity of the filtrate and washing solution is At 3000us / cm, it indicates that most of the salt in the tantalum powder has been removed, and then the filtered and washed material is poured into a horizontal ball mill for ball milling. The liquid ratio was controlled at 1:0.8, and the ball milling time was 5 hours. Then take out the material for pickling, and the acid solution is composed of HNO with a mass concentration of 10% 3 , 2% H 2 O 2 , plus 0.5% HF, pickling for 2h and then standing, then soaking for 1.5h, then adding pure water for rinsing, suction filtration and suction filtration, drying under vacuum (120℃ / 14h) to get the original tantalum powder . The original tantalum powder also undergo...

Embodiment 2

[0028] The sodium-reduced tantalum powder is prepared by using KCl as the dilution salt. After the reduction, the mixed bulk material of the sodium-reduced tantalum powder and the dilution salt KCl is added to pure water for filtration and washing for 15 hours. When the conductivity of the filtration and washing solution is At 1500us / cm, it indicates that most of the salt in the tantalum powder has been removed, and then the filtered and washed material is poured into a horizontal ball mill for ball milling. The liquid ratio was controlled at 1:1, and the ball milling time was 8 hours. Then take out the material for pickling, and the acid solution is composed of HNO with a mass concentration of 8% 3 , 3% H 2 O 2 , plus 0.7% HF pickling for 2.5h, let stand, then soak for 1h, then add pure water for rinsing, suction filtration and suction filtration, and dry under vacuum (150℃ / 12h) to get the original tantalum powder. The original tantalum powder also undergoes normal follow-...

Embodiment 3

[0030]The sodium-reduced tantalum powder was prepared by using the mixed salt of KCl and NaCl as the dilution salt. After the reduction, the mixed bulk material of the sodium-reduced tantalum powder and the diluted salt KCl and NaCl was added to pure water for filtration and washing for 20 hours. When the conductivity of the filtration and washing liquid is 1000us / cm, it indicates that most of the salt in the tantalum powder has been removed, and then the filtered and washed material is poured into a horizontal ball mill for ball milling, and the weight ratio of material to ball is controlled at 1:5 , the solid-liquid ratio of material and pure water is controlled at 1:1.5, and the ball milling time is 9 hours. Then take out the material for pickling, and the acid solution is composed of HNO with a mass concentration of 10% 3 , 2% H 2 O 2 , plus 0.5% HF pickling for 2 hours, let stand, then soak for 1.5 hours, then add pure water for rinsing, suction filtration and suction f...

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Abstract

The invention relates to a method for preparing target-level high-purity tantalum powder. According to the method for preparing the target-level high-purity tantalum powder, a block-shaped mixture of tantalum powder prepared through potassium fluotantalate sodium reduction and one or more of diluted slats including NaCl, KCl and KF is filtered and washed with pure water, when the conductivity of filtering and washing liquid is smaller than 5000 us / cm, the filtered and washed mixture is poured into a horizontal type ball mine for wet-type ball milling, the mixture is taken out, acid pickling, suction filtration and drying are conducted on the mixture, so that raw tantalum powder is obtained, thermal treatment, oxygen reduction, oxygen-reduction acid pickling, secondary drying and detection are conducted on the raw tantalum powder, and then the target-level high-purity tantalum powder is obtained. According to the method for preparing target-level high-purity tantalum powder, the technology is simple, the production cost is low, the tantalum powder prepared according to the method is large in apparent density, high in purity, low in oxygen content and capable of meeting the requirement of a target for the purity and the density of materials, and therefore tantalum target cost and tantalum alloy target cost are greatly reduced.

Description

technical field [0001] The invention relates to the technical field of non-ferrous metal materials, in particular to a preparation method of target-grade high-purity tantalum powder. Background technique [0002] In the prior art, the preparation of tantalum targets is mainly based on the processing of tantalum ingots. Powder metallurgy has become another magnetron sputtering target due to its advantages of easy to obtain a uniform fine-grained structure, saving raw materials, and high production efficiency. The main preparation methods and research hotspots. [0003] The tantalum powder used as a tantalum target must have two important conditions: one is high purity, generally above 4N; the other particles are preferably solid particles with high bulk density, because regardless of the texture factor, The density of the tantalum target is closely related to the quality of the tantalum target. The higher the density of the tantalum target, the better the quality of the tant...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F9/04B22F1/00
Inventor 杨国启郑爱国马跃忠周小军
Owner NINGXIA ORIENT TANTALUM IND