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High purity hafnium, target and thin film comprising said high purity hafnium, and method for producing high purity hafnium

A manufacturing method and high-purity technology, applied in the direction of ion implantation plating, coating, metal material coating process, etc., can solve the problem of difficult to effectively remove impurities, no effective and stable high-purity hafnium material manufacturing technology, no separation And other issues

Inactive Publication Date: 2006-12-20
JX NIPPON MINING & METALS CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, since there is no idea of ​​separating hafnium and zirconium as described above, the reality is that there is no manufacturing technology to efficiently and stably obtain the aforementioned high-purity hafnium material with reduced zirconium, targets and thin films formed of the material.
In addition, due to the difficulty of effectively removing impurities such as oxygen, sulfur and phosphorus, this is another reason why high purification has been neglected so far.
[0008] In particular, a material with a high residual resistance ratio is required, and since high-purity hafnium materials have not been available conventionally, it is impossible to sufficiently satisfy the requirements as an electronic component material due to the low residual resistance ratio

Method used

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  • High purity hafnium, target and thin film comprising said high purity hafnium, and method for producing high purity hafnium

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Experimental program
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Effect test

Embodiment 1

[0038] Commercially available hafnium tetrachloride (HfCl) of purity 3N containing about 5000 ppm by weight of zirconium as shown in Table 1 was used. 4 ) 100kg as a raw material, it was dissolved in 1L of pure water to make a nitric acid solution.

[0039] as HfCl 4 The main impurities in the raw material contain iron, chromium and nickel at 500 ppm by weight, 40 ppm by weight and 1000 ppm by weight, respectively.

[0040] Then, the hafnium raw material (nitric acid solution) was extracted with a 4-stage organic solvent using TBP organic solvent, and neutralized to obtain hafnium oxide (HfO 2 ).

[0041] In addition, the hafnium oxide is chlorinated to obtain high-purity hafnium tetrachloride (HfCl 4 ), followed by magnesium reduction to obtain hafnium sponge as a raw material. The hafnium sponge contained 300 ppm by weight of zirconium, and the total content of other impurities was reduced to 300 ppm by weight.

[0042] Then, using the obtained hafnium sponge as a raw m...

Embodiment 2

[0049] 100 kg of zirconium metal raw material (zirconium content 2% by weight) shown in Table 2 was used and dissolved in nitric acid-hydrofluoric acid. As main impurities of the raw material, the raw material contained 15000 ppm by weight, 8000 ppm by weight and 5000 ppm by weight of iron, chromium and nickel, respectively.

[0050] Then, use TBP organic solvent to carry out 10 stages of organic solvent extraction on the hafnium raw material, and carry out neutralization treatment to obtain hafnium oxide (HfO 2 ).

[0051] In addition, the hafnium oxide is chlorinated to obtain high-purity hafnium tetrachloride (HfCl 4 ), followed by calcium reduction to obtain hafnium sponge. The hafnium sponge contained 1500 ppm by weight of zirconium, and the total content of other impurities was reduced to 1000 ppm by weight.

[0052] Then, using the obtained hafnium sponge as a raw material, further two-stage melting was performed by furnace melting and ingot melting using an electron...

Embodiment 3

[0058] Zirconia (HfO 2 ) raw material (3N level) 100kg and dissolved in nitric acid-hydrofluoric acid. As main impurities of the raw material, the raw material contained 15000 ppm by weight, 8000 ppm by weight and 5000 ppm by weight of iron, chromium and nickel, respectively.

[0059] Alternatively, the hafnium oxide raw material is chlorinated and purified by at least 10 stages of distillation followed by sodium reduction.

[0060] Then, using the obtained hafnium as a raw material, further two-stage melting is performed by furnace melting and ingot melting using an electron beam to remove volatile elements, gas components, and the like. Due to the above process, as shown in Table 3, Zr: 500 wtppm, O: 100 wtppm, C: 100 wtppm, N: 20 wtppm, S: 10 wtppm, P: 10 wtppm, others: 30 ppm by weight.

[0061] Then, using Ca and CaCl 2 The hafnium thus obtained was deoxidized at 1250° C. under argon pressure (4 atm) for 10 hours. Reductions were achieved where O, C, N, S, P < 10 wtp...

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Abstract

A high purity hafnium, characterized in that it has a purity of 4N or higher, with the exception of zirconium and gas components, and has an oxygen content of 40 wt ppm or less; a target and thin film comprising the high purity hafnium; a high purity hafnium, characterized in that it has a purity of 4N or higher, with the exception of zirconium and gas components, and has both of a sulfur content and a phosphorus content of 10 wt ppm or less; a target and thin film comprising the high purity hafnium; a high purity hafnium material which is prepared by the use of a hafnium sponge having been reduced in the content of zirconium as a raw material and is further reduced in the contents of oxygen, sulfur and phosphorus; a target and thin film comprising the high purity hafnium material; and a method for producing a high purity hafnium. An efficient and stable production technique, a high purity hafnium material prepared by the technique, and a target and a thin film comprising said material are provided.

Description

technical field [0001] The present invention relates to a high-purity hafnium material with reduced contents of impurities such as zirconium, oxygen, sulfur, and phosphorus contained in hafnium, a target and a thin film formed of the high-purity hafnium material, and a method for producing high-purity hafnium. Background technique [0002] So far, there is a lot of literature on the manufacture of hafnium, however, hafnium is very similar to zirconium in terms of atomic structure and chemical properties, as exemplified below, neither the presence of zirconium nor the presence of hafnium in zirconium has really been seen as a problem . [0003] Hafnium and zirconium are excellent in heat resistance and corrosion resistance, and have characteristics of high affinity with oxygen, nitrogen, and the like. Also, their oxides or nitrides have excellent stability at high temperatures, so they are used as refractory materials in the field of manufacturing nuclear ceramics, steel, or...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C14/34C22B34/14C22B9/22C22C27/00
CPCC22C27/00C22B34/14C23C14/3414
Inventor 新藤裕一朗
Owner JX NIPPON MINING & METALS CORP
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