A kind of high-purity tantalum powder and its preparation method

A tantalum powder and high-purity technology, applied in the field of high-purity tantalum powder and its preparation, can solve problems such as limitations of design process parameters, high content of magnesium and hydrogen in the final product, sintering and growth of tantalum particles, etc.

Active Publication Date: 2018-02-06
NINGXIA ORIENT TANTALUM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantages of this method are: first: because the equipment it uses is made of high-purity tantalum, it requires high equipment and is expensive
Second, because there is no deoxidation step in the method, the oxygen content of the resulting product is extremely unstable, with great differences, and it is difficult to be less than 1000ppm
Third, due to the grading treatment, the availability of materials is greatly reduced, and it is difficult to refine the particle size of tantalum powder
[0010] At present, the production process of metallurgical grade tantalum powder generally adopts the method of simultaneous dehydrogenation and deoxidation, which will cause limitations in the design process parameters
Specifically, if the temperature is set too low, it will cause incomplete dehydrogenation and lead to high hydrogen content in the final product
At the same time, the properties (such as lattice constant, resistance, hardness, etc.) of tantalum after hydrogen absorption cannot be completely eliminated.
If the temperature is s...

Method used

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  • A kind of high-purity tantalum powder and its preparation method
  • A kind of high-purity tantalum powder and its preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Embodiment 1: Select sodium-reduced tantalum powder as raw material, carry out layering, sintering, electron beam melting to form tantalum ingot, and carry out hydrogenation treatment on the tantalum ingot. The tantalum scrap obtained after hydrogenating the tantalum ingot is crushed by ball milling and passed through a 500-mesh sieve. The tantalum powder sieved by the ball mill is used with HNO 3 Mixed acid with HF (HNO 3 , HF and water volume ratio is 4:1:20) pickling to remove metal impurities, drying and sieving (put the above tantalum powder in a closed furnace and heat it to 900°C for 180 minutes, then cool it out of the furnace and sieve After sieving, the oxygen content analysis is carried out, and the analysis results are shown in Table 1. Then the tantalum powder is mixed with 1% magnesium powder based on the weight of the tantalum powder, and then heated to 700 ° C in a closed furnace with argon, and kept for 2 hours. Then cool out of the furnace, wash with...

Embodiment 2

[0036] Example 2: Select sodium-reduced tantalum powder as raw material to form tantalum ingots by layering, sintering, and electron beam smelting, and then hydrogenate the tantalum ingots. The tantalum scrap obtained after hydrogenating the tantalum ingot is crushed by ball milling and passed through a 500-mesh sieve. Ball milled and sieved powder with HNO 3 Mixed acid with HF (HNO 3 , HF and water volume ratio is 4:1:20) pickling to remove metal impurities, drying and sieving. Place the above tantalum powder in a closed furnace, fill it with argon and heat it to 900°C for 180 minutes, then cool it out of the furnace and sieve it. After sieving, the oxygen content was analyzed, and the analysis results are shown in Table 1. Then mix tantalum powder with magnesium powder of 1% of the weight of tantalum powder, then heat it to 750°C in a closed furnace filled with argon, keep it warm for 2 hours, then cool it out of the furnace, wash with nitric acid to remove excess magnesi...

Embodiment 3

[0037] Embodiment 3: select sodium-reduced tantalum powder as raw material, carry out layering, sintering, and electron beam melting to form tantalum ingot, and then hydrogenate the tantalum ingot. The tantalum scrap obtained after hydrogenating the tantalum ingot is crushed by ball milling and passed through a 500-mesh sieve. Ball milled and sieved powder with HNO 3 Mixed acid with HF (HNO 3 , HF and water volume ratio is 4:1:20) pickling to remove metal impurities, drying and sieving. Place the above tantalum powder in a closed furnace, fill it with argon and heat it to 900°C for 180 minutes, then cool it out of the furnace and sieve it. After sieving, the oxygen content was analyzed, and the analysis results are shown in Table 1. Then mix tantalum powder with magnesium powder of 1% of the weight of tantalum powder, then heat it to 700°C in a closed furnace filled with argon, keep it warm for 2 hours, then cool it out of the furnace, wash with nitric acid to remove excess...

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Abstract

The invention relates to a high-purity tantalum powder and a preparation method thereof. The GDMS analysis purity of the tantalum powder is greater than 99.995%. Preferably, the oxygen content of the tantalum powder is not higher than 1000ppm, the nitrogen content is not higher than 50ppm, the hydrogen content is not higher than 20ppm, the magnesium content is not higher than 5ppm, and the particle size D50<25μm.

Description

technical field [0001] The invention relates to a high-purity tantalum powder and a preparation method thereof. More specifically, the tantalum powder has a purity greater than 99.995%, an average particle size D50<25 μm, an oxygen content of no higher than 1000 ppm, a nitrogen content of no higher than 50 ppm, a hydrogen content of no higher than 20 ppm, and a magnesium content of no higher than 5 ppm. Background technique [0002] In recent years, semiconductor technology has developed rapidly, and the demand for tantalum used as a sputtered film has gradually increased. In integrated circuits, tantalum is placed between silicon and copper conductors as a diffusion barrier. The production methods of tantalum sputtering targets include ingot metallurgy (I / M) method and powder metallurgy (P / M) method. Tantalum targets with lower requirements are generally made of tantalum ingots. However, in some cases with higher requirements, the I / M method cannot be used, and the ta...

Claims

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Application Information

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IPC IPC(8): B22F9/20B22F1/00
CPCB22F9/04C22F1/18B22F1/00B22F9/023B22F9/16B22F2009/043B22F2301/20B22F2304/10B22F2998/10C23G1/00
Inventor 李仲香程越伟陈学清王葶师德军童泽堃闫燕田小玉赵忠环
Owner NINGXIA ORIENT TANTALUM IND
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