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Method for Manufacturing High-Purity Erbium, High-Purity Erbium, Sputtering Target Composed of High-Purity Erbium, and Metal Gate Film having High-Purity Erbium as Main Component

a technology of erbium and erbium, which is applied in the direction of vacuum evaporation coating, sputtering coating, coating, etc., can solve the problems of not many documents relating to practical methods of extracting erbium, limit in achieving high purification, and cannot be said that erbium attracted much attention, so as to achieve efficient and stably supply high-purity erbium, high vapor pressure, and difficult to be refined

Inactive Publication Date: 2011-12-08
JX NIPPON MINING & METALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

[0022]The present invention yields superior effects of being able to provide a method of highly purifying erbium, which has a high vapor pressure and is difficult to be refined in a molten metal state, as well as efficiently and stably providing high-purity erbium obtained thereby, a sputtering target composed of high-purity erbium, and a metal gate film having high-purity erbium as a main component.

Problems solved by technology

Nevertheless, since erbium metal has a problem in that it is easily oxidized during refining, a high-purity erbium product did not exist since its high purification was difficult.
Moreover, erbium has been used as a magnetic refrigerant material, but since its use as an electronic component was not considered, it cannot be said that it was a metal that attracted much attention.
Accordingly, there are not many documents relating to practical methods of extracting erbium.
In this example, although there is a scheme in the use of misch metal as the reductant, it does not aim for higher purification, and there is a problem in that there is a limit in achieving high purification.
Since this technology is unable to sufficiently eliminate the slag, there is a problem in that it is difficult to achieve high purification.
This technology is based on the use of a fused-salt electrolysis bath, and there is a problem in that a complicated process is required and the effect of oxygen elimination is also insufficient.
There is also the problem of lithium, barium, calcium and so on being included as impurities.
Although it is also possible to obtain high-purity rare-earth metals in which the oxygen content is 300 ppm or less, and with few impurities such as calcium, lithium and fluorine (for example, refer to Patent Document 4), this technology is also based on the use of a fused-salt electrolysis bath and requires a complicated process.
In addition, there is the problem of lithium, barium, calcium and so on being included as impurities, and effect of oxygen elimination is also insufficient.
Nevertheless, since there is a problem in that the added metal are included as impurities and the elimination of Ta is also insufficient, there is a problem in that the level of high purification is low.
As shown in the foregoing documents, the effect of refining erbium is not necessarily sufficient, and in particular only a handful of documents seek the reduction of oxygen.
Among those that do, there is a problem in that the reduction of oxygen is insufficient.
In addition, methods that adopt the fused-salt electrolysis entail a complicated process, and there is a problem in that the refining effect is insufficient.
Like this, the current situation is that there is no efficient and stable manufacturing method to obtain high-purity erbium that is a high-melting point metal, has a high vapor pressure, and in which refining is difficult in a molten metal state.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0044]As the erbium raw material, crude erbium oxide (Er2O3) of 3 N was used. The impurities contained in this raw material are shown in Table 1.

[0045]Subsequently, the erbium raw material was mixed with yttrium (Y) as the reducing metal, and a vacuum distillation apparatus was used to thermally reduce the mixture in a vacuum at 1600° C. Pursuant to the progress of reduction of erbium oxide, erbium was distilled to improve the purity, and the erbium with improved purity was stored in a capacitor.

[0046]Distillation and thermal reduction reaction was as follows:

Er2O3 (solid)+2Y (solid)→2Er (gas) +3Y2O3 (solid)

[0047]10 kg of erbium was extracted from the erbium distillate stored in the capacitor, a CaO crucible was used to melt the extracted erbium in Ar atmosphere, and this was solidified into an ingot.

[0048]It was thereby possible to manufacture high-purity erbium in which the purity excluding rare-earth elements and gas components is 4 N or higher, oxygen content is 40 wtppm or less...

example 2

[0051]The same raw material as Example 1 was used to perform reduction. The entire process was performed as with Example 1 other than that La was used as the reductant.

[0052]It was thereby possible to manufacture high-purity erbium in which the purity excluding rare-earth elements and gas components is 4 N or higher, oxygen content is 60 wtppm or less, elements of alkali metals are respectively 1 wtppm or less, elements of transition metals are respectively 10 wtppm or less, and radioactive elements are respectively 10 wtppb or less. Although both Example 1 and Example 2 were able to achieve an oxygen content of 100 wtppm or less, in the case of Example 2, the content of radioactive elements U and Th was slightly high.

[0053]The sputtering target obtained from the foregoing ingot was also able to retain a high purity level, and it was possible to form a high-purity erbium thin film with uniform characteristics on a substrate by sputtering the foregoing sputtering target. The results ...

example 3

[0054]The entire process was performed as with Example 1 other than that erbium oxide of 3 N level was used as the raw material and the reduction / distillation temperature was set to 2500° C.

[0055]It was thereby possible to manufacture high-purity erbium in which the purity excluding rare-earth elements and gas components is 4 N or higher, oxygen content is 200 wtppm or less, elements of alkali metals are respectively 10 wtppm or less, elements of transition metals are respectively 100 wtppm or less, and radioactive elements are respectively 5 wtppb or less. In this Example, the impurity content was high overall since the reduction / distillation temperature was high, but it was still possible to keep it within an acceptable range.

[0056]The sputtering target obtained from the foregoing ingot was also able to retain a high purity level, and it was possible to form a high-purity erbium thin film with uniform characteristics on a substrate by sputtering the foregoing sputtering target. Th...

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Abstract

Provided are a method for manufacturing high-purity erbium, wherein crude erbium oxide is mixed with reducing metal, erbium is reduced and distilled by heating the mixture in a vacuum, and the distillate is melted in an inert atmosphere to obtain high-purity erbium; and high-purity erbium, wherein the purity excluding rare-earth elements and gas components is 4 N or higher and the oxygen content is 200 wtppm or less. An object of this invention is to provide a method of highly purifying erbium, which has a high vapor pressure and is difficult to be refined in a molten metal state, as well as technology for efficiently and stably providing high-purity erbium obtained with the foregoing method, a sputtering target composed of high-purity erbium, and a metal gate film having high-purity erbium as a main component.

Description

TECHNICAL FIELD[0001]The present invention relates to a method of highly purifying erbium, which has a high vapor pressure and is difficult to be refined in a molten metal state, high-purity erbium obtained thereby, a sputtering target composed of high-purity erbium, and a metal gate film having high-purity erbium as a main component.BACKGROUND ART[0002]Erbium (Er) is a rare-earth element, and it is contained in the earth's crust as a mineral source and as a mixed composite oxide. Although rare-earth elements are so called because they are separated from relatively rare existing minerals, they are not that rare when viewed in light of the entire crust. Erbium's atomic number is 68, and it is a gray-colored metal having an atomic weight of 167.3 and comprising a hexagonal close-packed structure. Erbium has a melting point of 1530° C., a boiling point of 2860° C., and a density of 9.07 g / cm3. Erbium's surface is oxidized in the air, it gradually melts in water, and it is soluble in ac...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): C22C28/00C22B59/00
CPCC22B5/04C22B5/16C22B9/006C22B9/14C22B59/00C22C28/00C23C14/3414C22B9/02C22B9/04
Inventor SHINDO, YUICHIROYAGI, KAZUTO
Owner JX NIPPON MINING & METALS CO LTD
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