JPH04176886A - Apparatus for producing high-purity y - Google Patents
Apparatus for producing high-purity yInfo
- Publication number
- JPH04176886A JPH04176886A JP30379990A JP30379990A JPH04176886A JP H04176886 A JPH04176886 A JP H04176886A JP 30379990 A JP30379990 A JP 30379990A JP 30379990 A JP30379990 A JP 30379990A JP H04176886 A JPH04176886 A JP H04176886A
- Authority
- JP
- Japan
- Prior art keywords
- electrodeposited
- bath
- electrolytic
- housing device
- purity
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000003860 storage Methods 0.000 claims description 10
- 238000004070 electrodeposition Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000005292 vacuum distillation Methods 0.000 claims description 2
- 238000005868 electrolysis reaction Methods 0.000 abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 6
- 229910002804 graphite Inorganic materials 0.000 abstract description 6
- 239000010439 graphite Substances 0.000 abstract description 6
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 abstract description 6
- 239000002184 metal Substances 0.000 abstract description 6
- 229910009523 YCl3 Inorganic materials 0.000 abstract 1
- 238000010924 continuous production Methods 0.000 abstract 1
- PCMOZDDGXKIOLL-UHFFFAOYSA-K yttrium chloride Chemical compound [Cl-].[Cl-].[Cl-].[Y+3] PCMOZDDGXKIOLL-UHFFFAOYSA-K 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 description 15
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910013618 LiCl—KCl Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- BUKHSQBUKZIMLB-UHFFFAOYSA-L potassium;sodium;dichloride Chemical compound [Na+].[Cl-].[Cl-].[K+] BUKHSQBUKZIMLB-UHFFFAOYSA-L 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
Landscapes
- Manufacture And Refinement Of Metals (AREA)
- Electrolytic Production Of Metals (AREA)
Abstract
Description
【発明の詳細な説明】
１班例技芸次且
本発明は、高純度金属Ｙの製造装置に関するものであり
、特には半導体デバイス用のＹ酸化物（Ｙ。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an apparatus for producing high-purity metal Y, particularly Y oxide (Y) for semiconductor devices.
０３）の形成に用いる高純度Ｙの製造装置に関する。This invention relates to an apparatus for producing high-purity Y used in the formation of 03).
本発明の装置は、電析Ｙの収納装置がついており、かつ
移動可能であるため、大気にさらすことなくかつ連続的
に操業できるため効率的である。The apparatus of the present invention is equipped with a storage device for depositing Y and is movable, so it is efficient because it can be operated continuously without being exposed to the atmosphere.
丈光孜歪
Ｙ金属の製錬方法の一つとして、溶融塩電解法が採用さ
れている。Molten salt electrolysis is used as one of the methods for smelting strained Y metal.
溶融塩電解法においては、−回の電解が終了した後、電
析したＹを溶融塩から引き上げる。その後、−旦電解炉
を冷却してから電解蓋を取外し、大気に触れさせてカソ
ード棒から電析したＹを脱着する。In the molten salt electrolysis method, the electrodeposited Y is pulled up from the molten salt after -times of electrolysis are completed. Thereafter, the electrolytic furnace is cooled down, and then the electrolytic lid is removed, and the electrodeposited Y is desorbed from the cathode rod by exposing it to the atmosphere.
さらに、その塩の付着した電析Ｙを真空蒸留していた。Furthermore, the electrodeposited Y with the salt attached was vacuum distilled.
このように、電析したＹの後処理において、−担外気に
触れると付着した塩が吸湿して、脱塩処理が良好にでき
ないことが多く、残留した浴に含有されている不純物の
影響を受ける。さらにその後のＥＢ溶解においてもスプ
ラッシュが多くなり、歩留も悪かった。また、電析した
Ｙを取り出すためには溶融塩を一担冷却せねばならずバ
ッチ式となり、連続操業ができなかった。In this way, in the post-treatment of electrodeposited Y, the attached salt often absorbs moisture when exposed to the outside air, making it difficult to desalinate properly. receive. Furthermore, there was a lot of splash in the subsequent EB melting, and the yield was also poor. In addition, in order to take out the deposited Y, the molten salt had to be cooled once, which required a batch process, which made continuous operation impossible.
そこで、本発明者等が鋭意検討した結果、以下の発明が
なされた。Therefore, as a result of intensive study by the present inventors, the following invention was made.
且ユｎ孟疾
（１）下部に電解装置を有し、該電解装置の上部に脱着
可能な電析Ｙ収納装置を有する装置で、該電析Ｙ収納装
置に前記電解装置で回収したＹを有するカソード電極棒
が、収納しうるような構造としたことを特徴とする高純
度Ｙの製造装置。(1) An apparatus having an electrolytic device at the bottom and a removable electrodeposited Y storage device at the top of the electrolytic device, in which the Y recovered by the electrolytic device is stored in the electrodeposited Y storage device. 1. An apparatus for producing high-purity Y, characterized in that the cathode electrode rod has a structure that can be stored.
（２）上記（１）における電析Ｙ装置が、電析Ｙを収納
後、真空蒸留装置に設置可能な構造としている事を特徴
とする高純度Ｙの製造装置。(2) An apparatus for producing high-purity Y, characterized in that the electrodeposition Y apparatus according to (1) above has a structure that can be installed in a vacuum distillation apparatus after storing the electrodeposition Y.
濃１υＵ（眞１１−
本発明は、高純度Ｙの溶融塩電解装置に係るものである
。The present invention relates to a high-purity Y molten salt electrolysis device.
電解装置の本体は、外容器はステンレス類である。The main body and outer container of the electrolyzer are made of stainless steel.
溶融塩用の容器は、Ｎｉルツボの内側にグラファイトル
ツボを入れる。あるいは、高価ではあるが、Ｗ。As a container for molten salt, a graphite crucible is placed inside the Ni crucible. Or W, although it is expensive.
Ｍｏ、Ｔａ等の高融点金属製ルツボを用いても良い。A crucible made of a high melting point metal such as Mo or Ta may also be used.
グラファイトルツボには、溶融塩となるもの、例えば、
ＮａＣ１，ＮａＣ１−ＫＣｌ、ＬｉＣ１−ＫＣｌ等をい
れる。グラファイトルツボは、アノード用の容器として
用いる。アノードのリード線は、電解装置の本体と上部
のＹ収納装置の接続部（ボルトとナツト）に接続する。Graphite crucibles contain substances that become molten salts, e.g.
Add NaCl, NaCl-KCl, LiCl-KCl, etc. A graphite crucible is used as a container for the anode. The anode lead wire is connected to the connection part (bolt and nut) between the main body of the electrolyzer and the upper Y storage device.
電解装置には、上下２つのバルブがあり下のバルブは、
溶融塩の蒸気の遮断及び外気からの湿気の混入の防止の
ためであり、上のバルブは、別の電気炉に移動可能とし
、かつ外気からの湿気混入による電析物及び付着塩の酸
化防止のためである。The electrolyzer has two valves, upper and lower, and the lower valve is
This is to shut off molten salt vapor and prevent moisture from entering from outside air.The upper valve can be moved to another electric furnace, and prevents oxidation of deposits and deposited salt due to moisture entering from outside air. This is for the sake of
カソードは、Ｎ ｉ 、 Ｗ、 ＭＯ等を用いる。For the cathode, Ni, W, MO, etc. are used.
移動後の電解装置は、ただちにもう一つの電析）′収納
装置とカソード棒を取り付け、前記と同様の電解を操業
することかできる。After being moved, the electrolyzer can be immediately fitted with another electrodeposition storage device and a cathode rod, and can be operated for electrolysis in the same manner as described above.
［実施例］
第１図に示す溶融塩電解装置を用いて、粗Ｙを溶融塩電
解精製する実施例を示す。[Example] An example will be shown in which crude Y is subjected to molten salt electrolysis refining using the molten salt electrolysis apparatus shown in FIG.
Ｎｌ製ルツボ３にグラファイトルツボ４を挿入し、その
中に粉状無水塩化リチウム及び塩化カリウムを各々９，
１１ｋｇ入れ、そしてこれを電解槽容器２に入れ、電気
炉４にセットする。A graphite crucible 4 is inserted into a crucible 3 made of Nl, and powdered anhydrous lithium chloride and potassium chloride are each placed in the crucible 4.
11 kg was placed in the electrolytic cell container 2 and set in the electric furnace 4.
前操作としてＬｉｃｋ、ＫＣ］を真空ポンプで内部を出
ロアより排気しながら約５００℃まで加熱した。さらに
、Ａｒガスを入口６より導入し大気圧塩′上にする。Ａ
ｒ雰囲気下で表１に示すような粗Ｙメタル１１を約２ｋ
ｇ挿入し、さらに、Ａｒガスと同時にＹＣ１，を約２０
００ｇ洛中に導入する。この時の電解浴Ｓ中のＹ１１度
は約４％であった。導入終了後、浴温を７００℃とし、
さらにＷ電極棒８を入れる。初期カソード電流密度を１
．ＯＡ／ｃｍ’とし電解を実施した。約２０ｈｒ通電し
たところで、第一回の電解操作を停止した。電析Ｙ収納
装置１３内をＡｒ雰囲気にするため、導入口１６よりＡ
ｒを導入し、排出口１７より排出してＡｒ置換を行う。[Lick, KC] was heated to about 500° C. as a pre-operation while evacuating the inside from the outlet lower with a vacuum pump. Furthermore, Ar gas is introduced from the inlet 6 to bring it above the atmospheric pressure salt. A
Approximately 2k of rough Y metal 11 as shown in Table 1 is heated under r atmosphere.
Insert about 20 g of YC1, and then add about 20 g of YC1 at the same time as Ar gas.
00g will be introduced into Rakuchu. At this time, the Y11 degree in the electrolytic bath S was about 4%. After the introduction, the bath temperature was set to 700℃,
Furthermore, insert the W electrode rod 8. The initial cathode current density is 1
．． Electrolysis was carried out at OA/cm'. After about 20 hours of electricity, the first electrolysis operation was stopped. In order to create an Ar atmosphere inside the electrodeposited Y storage device 13, A is introduced from the inlet 16.
Ar is introduced and discharged from the exhaust port 17 to perform Ar substitution.
電析したＹを上部の筒１３の中に引き上げ、上下】４．
１５二つのバルブを閉める。筒１３をカソード棒ととも
に別の電気炉に移動する。さらに、別のＹ収納装置をバ
ルブ１５の上にとりつけることにより、連続操業が可能
となる。Pull the electrodeposited Y into the upper cylinder 13 and move it up and down]4.
15 Close the two valves. The tube 13 is moved together with the cathode rod to another electric furnace. Furthermore, by attaching another Y storage device above the valve 15, continuous operation is possible.
１班しガ呈 溶融塩電解が連続的に操業可能となる。1st group presentation Molten salt electrolysis can be operated continuously.
第１図は、本発明の高純度Ｙを得るための製造装置の概
略図である。
ｌ・電気炉、２・ステンレス裂電解槽容器、３・Ｎｉ製
ルツボ、４・・グラファイトルツボ、５・電解浴、６・
・−Ａｒ導入口、７ 排気口、８・カソード電極棒、１
］・−Ｙメタル、１３・電析Ｙ収納装置、１４・上バル
ブ１５・下バルブ、１６−Ａｒ導入口、
１７・・Ａｒ排出口
特許呂願人 日本鉱業株式会社
代 理 人 弁理士（７５６９）並川啓志第１図
平成３年 ２月 ２日FIG. 1 is a schematic diagram of a manufacturing apparatus for obtaining high purity Y of the present invention. 1. Electric furnace, 2. Stainless steel cracked electrolytic tank container, 3. Ni crucible, 4. Graphite crucible, 5. Electrolytic bath, 6.
・-Ar inlet, 7 Exhaust port, 8・Cathode electrode rod, 1
] - Y metal, 13 - Electrodeposition Y storage device, 14 - Upper valve 15 - Lower valve, 16 - Ar inlet, 17 - Ar outlet Patent attorney: Japan Mining Co., Ltd. Patent attorney (7569) ) Keishi Namikawa Figure 1 February 2, 1991
Claims (2)
可能な電析Ｙ収納装置を有する装置で、該電析Ｙ収納装
置に前記電解装置で回収したＹを有するカソード電極棒
が、収納しうるような構造としたことを特徴とする高純
度Ｙの製造装置。(1) An apparatus having an electrolytic device at the bottom and a removable electrodeposited Y storage device at the top of the electrolytic device, in which the cathode electrode rod containing the Y recovered by the electrolytic device is placed in the electrolytic Y storage device. 1. An apparatus for producing high-purity Y, characterized in that it has a structure that allows it to be stored.
真空蒸留装置に設置可能な構造としている事を特徴とす
る高純度Ｙの製造装置。(2) After the electrodeposition Y device in the first paragraph stores the electrodeposition Y,
A high-purity Y production device characterized by a structure that can be installed in a vacuum distillation device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30379990A JPH04176886A (en) | 1990-11-13 | 1990-11-13 | Apparatus for producing high-purity y |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30379990A JPH04176886A (en) | 1990-11-13 | 1990-11-13 | Apparatus for producing high-purity y |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04176886A true JPH04176886A (en) | 1992-06-24 |
Family
ID=17925442
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP30379990A Pending JPH04176886A (en) | 1990-11-13 | 1990-11-13 | Apparatus for producing high-purity y |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04176886A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013005349A1 (en) | 2011-07-06 | 2013-01-10 | Jx日鉱日石金属株式会社 | High-purity yttrium, process for producing high-purity yttrium, high-purity yttrium sputtering target, metal gate film deposited with high-purity yttrium sputtering target, and semiconductor element and device equipped with said metal gate film |
-
1990
- 1990-11-13 JP JP30379990A patent/JPH04176886A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013005349A1 (en) | 2011-07-06 | 2013-01-10 | Jx日鉱日石金属株式会社 | High-purity yttrium, process for producing high-purity yttrium, high-purity yttrium sputtering target, metal gate film deposited with high-purity yttrium sputtering target, and semiconductor element and device equipped with said metal gate film |
| KR20140012190A (en) | 2011-07-06 | 2014-01-29 | 제이엑스 닛코 닛세키 킨조쿠 가부시키가이샤 | High-purity yttrium, process for producing high-purity yttrium, high-purity yttrium sputtering target, metal gate film deposited with high-purity yttrium sputtering target, and semiconductor element and device equipped with said metal gate film |
| US10041155B2 (en) | 2011-07-06 | 2018-08-07 | Jx Nippon Mining & Metals Corporation | High-purity yttrium, process of producing high-purity yttrium, high-purity yttrium sputtering target, metal gate film deposited with high-purity yttrium sputtering target, and semiconductor element and device equipped with the metal gate film |
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