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Method for preparing target-level 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 effects of improving purity, low production cost and reducing cost.

Active Publication Date: 2014-11-19
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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  • Method for preparing target-level high-purity tantalum powder
  • Method for preparing target-level high-purity tantalum powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Use NaCl as the diluted salt to prepare the sodium-reduced tantalum powder. After the reduction, the mixed lump material of the sodium-reduced tantalum powder and the diluted salt NaCl is added to pure water and washed for 10 hours. When the conductivity of the filtrate is When it is 3000us / cm, it shows 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 weight ratio of the material to the ball is controlled at 1:2.5. The liquid ratio is controlled at 1:0.8, and the ball milling time is 5 hours. Then take out the material and carry out pickling, and the acid solution is composed of HNO with a mass concentration of 10%. 3 , 2% H 2 o 2 , add 0.5% HF, pickle for 2 hours, let it stand still, then soak for 1.5 hours, then rinse with pure water, filter with suction, and dry under vacuum (120°C / 14h) to get the original powder of tantalum powder . The raw tantalu...

Embodiment 2

[0028] Use KCl as the diluted salt to prepare the sodium-reduced tantalum powder. After the reduction, add the mixed block material of the sodium-reduced tantalum powder and the diluted salt KCl to pure water for 15 hours, and when the conductivity of the filtrate is When it is 1500us / cm, it shows 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 weight ratio of the material to the ball is controlled at 1:4. The liquid ratio is controlled at 1:1, and the ball milling time is 8 hours. Then take out the material and carry out pickling, and the acid solution is composed of HNO with a mass concentration of 8%. 3 , 3% H 2 o 2 , add 0.7% HF pickling for 2.5h, let it stand still, then soak for 1h, then rinse with pure water, filter with suction, and dry under vacuum (150°C / 12h) to get the original tantalum powder. The raw tantalum powder also undergoes normal follow-u...

Embodiment 3

[0030]The mixed salt of KCl and NaCl is used as the diluted salt to prepare the sodium-reduced tantalum powder. After the reduction is completed, the mixed block material of the sodium-reduced tantalum powder and the diluted salt KCl and NaCl is added to pure water for 20 hours, and when When the conductivity of the filtrate 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 the material to the ball is controlled at 1:5 , the solid-to-liquid ratio of material to pure water is controlled at 1:1.5, and the ball milling time is 9 hours. Then take out the material and carry out pickling, and the acid solution is composed of HNO with a mass concentration of 10%. 3 , 2% H 2 o 2 , add 0.5% HF pickling for 2 hours, let it stand still, then soak for 1.5 hours, then rinse with pure water, filter with suction, and dry under vac...

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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 method for preparing 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 for its advantages of easy to obtain uniform fine-grained structure, saving raw materials, and high production efficiency. Main preparation methods and research hotspots. [0003] The tantalum powder used as a tantalum target must meet two important conditions: one is high purity, generally above 4N; the other is that the particles should preferably be solid particles with high bulk density, because texture factors aside, 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 tantalu...

Claims

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Application Information

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Patent Type & Authority Applications(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
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