JP2002371325A - High purity metal, sputtering target consisting of high purity metal, thin film formed by sputtering, and method for manufacturing high purity metal - Google Patents
High purity metal, sputtering target consisting of high purity metal, thin film formed by sputtering, and method for manufacturing high purity metalInfo
- Publication number
- JP2002371325A JP2002371325A JP2001182735A JP2001182735A JP2002371325A JP 2002371325 A JP2002371325 A JP 2002371325A JP 2001182735 A JP2001182735 A JP 2001182735A JP 2001182735 A JP2001182735 A JP 2001182735A JP 2002371325 A JP2002371325 A JP 2002371325A
- Authority
- JP
- Japan
- Prior art keywords
- metal
- high purity
- purity
- chromium
- purity metal
- 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.)
- Granted
Links
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、Ｏ、Ｃ、Ｎ、Ｈ、
Ｆ、Ｓ等（以下、特に記載しない限り、「ガス成分」と
記載する。）を多量に含有する粗金属から、該ガス成分
を大幅に減少させることのできる高純度金属の製造方法
並びに高純度金属、高純度金属からなるスパッタリング
ターゲット及びスパッタリングにより形成した薄膜に関
する。TECHNICAL FIELD The present invention relates to O, C, N, H,
From a crude metal containing a large amount of F, S, and the like (hereinafter, referred to as a “gas component” unless otherwise specified), a method for producing a high-purity metal capable of significantly reducing the gas component, and a high-purity metal The present invention relates to a sputtering target made of metal and high-purity metal, and a thin film formed by sputtering.
【０００２】[0002]
【従来の技術】最近、磁性材料、磁気記録材料、高弾性
材料、半導体材料等に高純度クロム、マンガン等の高純
度金属が使用されるようになってきたが、これらの粗金
属には、Ｏ、Ｃ、Ｎ、Ｈ、Ｆ、Ｓ等のガス成分を多量に
含有されている。したがって、上記のような用途に使用
する場合には、このような不純物を含有する粗金属から
該ガス成分等を減少させることが要求される。例えば、
高純度クロムを製造する方法として、通常６価の粗クロ
ムを電解精製して高純度クロムを得る方法や水素や炭素
等の還元剤あるいは脱硫剤を添加して高純度化する方法
が提案されているが、６価の粗クロムは有毒であり取扱
いに危険が伴うという問題があり、また還元剤及び脱硫
剤を使用する方法は工程が煩雑となりコスト高となる欠
点があった。2. Description of the Related Art Recently, high-purity metals such as high-purity chromium and manganese have been used for magnetic materials, magnetic recording materials, high-elastic materials, and semiconductor materials. It contains a large amount of gas components such as O, C, N, H, F, and S. Therefore, when used in the above applications, it is required to reduce such gas components and the like from crude metals containing such impurities. For example,
As a method of producing high-purity chromium, a method of obtaining high-purity chromium by electrolytically refining crude hexavalent chromium or a method of adding a reducing agent such as hydrogen or carbon or a desulfurizing agent to achieve high purity has been proposed. However, there is a problem that crude hexavalent chromium is toxic and involves a risk of handling, and the method using a reducing agent and a desulfurizing agent has the disadvantage that the steps are complicated and the cost is high.
【０００３】このようなことから、安全にかつ低コスト
で製造できる方法の検討がなされてきた。そこでクロム
等の金属特有の蒸気圧が高いことを利用して、高周波溶
解炉を使用して真空蒸留を行った。しかし、クロム等を
真空蒸留する場合、２０００°Ｃ程度まで高温に加熱す
る必要がある。溶解する坩堝を２０００°Ｃに上げるた
めには、坩堝材料や溶解装置を耐熱性に優れた特別なも
のを使用しなければならず、また坩堝材料からの汚染の
問題もあり、かえってコスト高になるという問題があ
り、高周波溶解炉を使用して真空蒸留する高純度化は断
念せざるを得なかった。[0003] In view of the above, a method for manufacturing the semiconductor device safely and at low cost has been studied. Therefore, utilizing the high vapor pressure specific to metals such as chromium, vacuum distillation was performed using a high-frequency melting furnace. However, in the case of vacuum distillation of chromium or the like, it is necessary to heat it to a high temperature of about 2000 ° C. In order to raise the melting crucible to 2000 ° C, special crucible materials and melting equipment with excellent heat resistance must be used, and there is also a problem of contamination from the crucible material, which increases the cost. Therefore, there was no other choice but to give up high-purity vacuum distillation using a high-frequency melting furnace.
【０００４】[0004]
【発明が解決しょうとする課題】以上から、本発明は
Ｏ、Ｃ、Ｎ、Ｈ、Ｆ、Ｓ等のガス成分を多量に含有する
粗金属から、該ガス成分を大幅に減少させることのでき
る高純度金属の製造に際し、クロム等の金属特有の蒸気
圧が高いことを利用するとともに、低コストでかつ安全
性が高い金属の製造方法を提供するものであり、さら
に、これによって得られた高純度金属、高純度金属から
なるスパッタリングターゲット及びスパッタリングによ
り形成した薄膜を提供するものである。As described above, the present invention can greatly reduce the amount of a gas component such as O, C, N, H, F, and S from a crude metal containing a large amount of the gas component. In the production of high-purity metals, it utilizes the high vapor pressure specific to metals such as chromium, and provides a low-cost and highly safe method for producing metals. An object of the present invention is to provide a sputtering target composed of a high-purity metal and a high-purity metal, and a thin film formed by sputtering.
【０００５】[0005]
【課題を解決するための手段】本発明は、 １．Ｏ、Ｃ、Ｎ、Ｈ、Ｆ、Ｓ等のガス成分含有量が総量
で２００ｐｐｍ以下であることを特徴とする高純度クロ
ム又は高純度マンガンからなる高純度金属。 ２．上記１記載の高純度金属からなるスパッタリングタ
ーゲット及び該ターゲットを用いてスパッタリングによ
り形成した薄膜。 ３．Ｏ、Ｃ、Ｎ、Ｈ、Ｆ、Ｓ等のガス成分を多量に含有
する粗金属を電子ビーム溶解し、揮発した金属を凝縮し
て高純度金属を得ることを特徴とする高純度金属の製造
方法。 ４．金属がクロム又はマンガン、カルシウムであること
を特徴とする上記３記載の高純度金属の製造方法。 ５．坩堝中に粗金属を入れ、該粗金属に電子ビームを照
射して金属を溶解揮発させ、凝縮容器の天井等に凝縮し
た高純度金属を回収することを特徴とする上記３又は４
記載の高純度金属の製造方法。 に関する。The present invention provides: A high-purity metal comprising high-purity chromium or high-purity manganese, wherein the total content of gas components such as O, C, N, H, F, and S is 200 ppm or less. 2. 2. A sputtering target comprising the high-purity metal according to 1 above, and a thin film formed by sputtering using the target. 3. Production of high-purity metal, characterized in that a crude metal containing a large amount of gas components such as O, C, N, H, F, and S is melted by an electron beam, and the volatilized metal is condensed to obtain a high-purity metal. Method. 4. 4. The method for producing a high-purity metal according to the above item 3, wherein the metal is chromium, manganese, or calcium. 5. The above-mentioned item 3 or 4, wherein the coarse metal is put into a crucible, the coarse metal is irradiated with an electron beam to dissolve and volatilize the metal, and the high-purity metal condensed on the ceiling or the like of the condensation vessel is recovered.
The method for producing a high-purity metal according to the above. About.
【０００６】[0006]
【発明の実施の形態】本発明の一例について、図を使用
して説明する。図１は本発明に使用する電子ビーム溶解
装置の断面概念説明図であり、銅製等の水冷坩堝１に精
製前のＯ、Ｃ、Ｎ、Ｈ、Ｆ、Ｓ等のガス成分を多量に含
有する粗金属２を導入する。坩堝１の上部に凝縮容器３
を設置する。凝縮容器３の材料としては、鉄、ステンレ
ス、グラファイト等の材料を使用することができる。し
かし、特に汚染物質が存在しない限り、特に上記材料に
制限される必要がなく、他の材料を使用することもでき
る。該凝縮容器３の一部には粗金属２に電子ビーム４等
を照射する窓５が開けられている。電子ビーム溶解装置
の真空度は１×１０−２〜１×１０−５ｍｍＨｇ程度に
維持する。電子ビームによる溶解は０．１Ａ〜１０Ａで
実施する。なお、この電子ビーム溶解の出力は、溶解蒸
発させ精製する金属の種類等に応じて適宜制御すること
ができ、必ずしも上記に制限される必要はない。DESCRIPTION OF THE PREFERRED EMBODIMENTS One example of the present invention will be described with reference to the drawings. FIG. 1 is a conceptual explanatory view of a cross section of an electron beam melting apparatus used in the present invention. A water-cooled crucible 1 made of copper or the like contains a large amount of gas components such as O, C, N, H, F, and S before purification. The crude metal 2 is introduced. Condensing container 3 on top of crucible 1
Is installed. As a material of the condensation container 3, a material such as iron, stainless steel, and graphite can be used. However, as long as no contaminants are present, there is no need to be particularly limited to the above materials, and other materials can be used. A window 5 for irradiating the coarse metal 2 with an electron beam 4 or the like is opened in a part of the condensation vessel 3. The degree of vacuum of the electron beam melting apparatus is maintained at about 1 × 10 −2 to 1 × 10 −5 mmHg. Melting by an electron beam is performed at 0.1 A to 10 A. The output of the electron beam melting can be appropriately controlled according to the type of metal to be dissolved and evaporated and purified, and is not necessarily limited to the above.
【０００７】電子ビーム４の粗金属２への照射により、
電子ビームスポットに金属の溶融プールが形成される
が、クロムやマンガン等の金属は蒸気圧が極めて高いの
で直ちに蒸発し、主として１５００°Ｃ以下に保持され
た凝縮容器３の天井や側壁に金属クロム、金属マンガン
等の蒸留金属６が付着する。この凝縮容器３の保持温度
は高純度化する粗原料金属材料によって、適宜調節す
る。上記のように、蒸気圧が極めて高いクロム、マンガ
ン等の金属は直ちに蒸発するので、粗原料を保持する坩
堝は上記のように、銅製等の水冷坩堝１を使用すること
ができる。したがって、高周波溶解等で使用するような
高耐熱性の坩堝材料を使用する必要はない。そして、粗
原料中に含まれる酸化クロム、二酸化マンガンやその他
の酸化物、硫化物、炭化物、窒化物等の蒸発し難い物質
は坩堝１内に残存し、また揮発するガス成分は凝縮容器
３外に排出される。以上の結果、凝縮容器３の天井や側
壁に付着した金属クロム、金属マンガン等の蒸留金属６
は蒸気圧の差異から優先的かつ選択的に、Ｏ、Ｃ、Ｎ、
Ｈ、Ｆ、Ｓ等のガス成分含有量が総量で２００ｐｐｍ以
下の極めて純度の高い５Ｎレベルの高純度クロム、金属
マンガン等の金属が得られる。なお、凝縮容器３の坩堝
に近い側壁にはスプラッシュによる低純度の物質が付着
する場合があるが、その場合にはその部分は回収高純度
クロム、高純度マンガン等の金属から除外する必要があ
る。By irradiating the coarse metal 2 with the electron beam 4,
A molten pool of metal is formed at the electron beam spot, but metals such as chromium and manganese evaporate immediately due to the extremely high vapor pressure, and mainly chromium metal is formed on the ceiling and side walls of the condensation vessel 3 maintained at 1500 ° C or lower. , Metal manganese or other distilled metal 6 adheres. The holding temperature of the condensing container 3 is appropriately adjusted depending on the crude metal material to be purified. As described above, since metals such as chromium and manganese having an extremely high vapor pressure evaporate immediately, the water-cooled crucible 1 made of copper or the like can be used as the crucible for holding the crude material as described above. Therefore, it is not necessary to use a high heat-resistant crucible material used for high-frequency melting or the like. In addition, hardly evaporable substances such as chromium oxide, manganese dioxide and other oxides, sulfides, carbides, and nitrides contained in the crude material remain in the crucible 1, and the gas components that evaporate are removed from the condensing vessel 3. Is discharged. As a result, the distillation metal 6 such as chromium metal or manganese metal adhered to the ceiling or side wall of the condensation vessel 3
Is preferentially and selectively based on the difference in vapor pressure, and O, C, N,
Metals such as 5N-level high-purity chromium and metal manganese having extremely high purity, having a total content of gas components such as H, F and S of 200 ppm or less, can be obtained. In addition, a low-purity substance due to splash may adhere to the side wall near the crucible of the condensing container 3, and in that case, that part must be excluded from metals such as recovered high-purity chromium and high-purity manganese. .
【０００８】この凝縮容器３の天井や側壁に付着した金
属クロム、金属マンガン等の金属６は電子ビーム溶解
後、冷却して取り外す。この金属クロム、金属マンガン
等の蒸留金属６は容易に剥がすことができる。このよう
にして得たＯ、Ｃ、Ｎ、Ｈ、Ｆ、Ｓ等のガス成分含有量
が総量で２００ｐｐｍ以下である高純度クロム、金属マ
ンガン等の蒸留金属を、真空溶解、鋳造等の工程を経て
電子部品等に使用するクロム、マンガン等の薄膜を形成
するスパッタリングターゲットに加工することができ
る。このような高純度ターゲットは薄膜の特性を改善す
るだけでなく、Ｏ、Ｃ、Ｎ、Ｈ、Ｆ、Ｓ等のガス成分に
起因するスパッタリング中のスプラッシュ、異常放電、
パーティクル等の発生が減少するという著しい特長を有
する。以上については、主としてクロム及びマンガンの
高純度化について説明したが、本発明の電子ビームによ
る精製によるＯ、Ｃ、Ｎ、Ｈ、Ｆ、Ｓ等のガス成分の除
去、すなわちクロムやマンガンと同様に蒸気圧の高いＣ
ａ、Ｐｂ、Ｓｎ、Ｂｅ、Ｎｉ、Ｓｉ等の金属の精製に有
効である。The metal 6 such as chromium metal or manganese metal adhered to the ceiling or side wall of the condensing container 3 is cooled and removed after melting by electron beam. The distilled metal 6 such as metal chromium and metal manganese can be easily peeled off. Vapor melting, casting, etc. of the thus obtained distilled metals such as high purity chromium and metallic manganese having a total content of gas components of 200 ppm or less such as O, C, N, H, F, S, etc. After that, it can be processed into a sputtering target for forming a thin film of chromium, manganese or the like used for electronic parts and the like. Such a high-purity target not only improves the properties of the thin film, but also includes a splash during sputtering due to gas components such as O, C, N, H, F, and S, abnormal discharge,
It has a remarkable feature that generation of particles and the like is reduced. In the above, the description has been given mainly of the purification of chromium and manganese. However, the removal of gas components such as O, C, N, H, F, and S by the refining by the electron beam of the present invention, that is, similar to the case of chromium and manganese, C with high vapor pressure
It is effective for refining metals such as a, Pb, Sn, Be, Ni, and Si.
【０００９】[0009]
【実施例】次に、実施例に基づいて説明する。なお、こ
れらは本発明の理解を容易にするためのものであり、本
発明はこれらに制限されるものではない。Next, an embodiment will be described. Note that these are intended to facilitate understanding of the present invention, and the present invention is not limited to these.
【００１０】（実施例１）図１に示すような電子ビーム
溶解装置を使用し、銅製の水冷坩堝に精製前のＯ、Ｃ、
Ｎ、Ｈ、Ｆ、Ｓ等のガス成分を多量に含有する３Ｎレベ
ルの粗クロム（原料）５ｋｇを導入した。この原料の化
学分析値を表１に示す。坩堝の上部に位置する凝縮容器
の材料としては、純鉄を使用した。該凝縮容器の一部に
開口した窓から原料粗クロムに電子ビームを照射した。
電子ビーム溶解装置の真空度は１〜２×１０−４ｍｍＨ
ｇ（≒１．３３〜２．６６×１０−２Ｐａ）に維持し
た。電子ビームによる溶解を１．２Ａで１時間、実施し
た。(Embodiment 1) Using an electron beam melting apparatus as shown in FIG. 1, O, C,
5 kg of 3N-level crude chromium (raw material) containing a large amount of gas components such as N, H, F, and S were introduced. Table 1 shows the chemical analysis values of this raw material. Pure iron was used as a material for the condensation vessel located at the top of the crucible. The raw material crude chromium was irradiated with an electron beam through a window opened in a part of the condensation vessel.
The degree of vacuum of the electron beam melting device is 1-2 × 10 −4 mmH
g (≒ 1.33 to 2.66 × 10 −2 Pa). Dissolution by electron beam was performed at 1.2 A for 1 hour.
【００１１】粗クロム原料への電子ビーム照射により、
電子ビームスポットに金属クロムの溶融プールが形成さ
れたが、その範囲は小さく、クロムは直ちに蒸発し、１
５００°Ｃ以下に保持された凝縮容器の天井や側壁に金
属クロムが付着した。上記のように、金属クロムは蒸気
圧が極めて高く直ちに蒸発するので、原料を保持する銅
製の水冷坩堝が溶損や破壊することは全くなかった。そ
して、粗原料中に含まれる酸化クロムやその他の酸化
物、硫化物、炭化物、窒化物等の蒸発し難い物質は坩堝
内に残存した。またその他の揮発したガス成分は凝縮容
器外に排出された。凝縮容器の天井や側壁に付着した金
属クロムは蒸気圧の差異から、Ｏ、Ｃ、Ｎ、Ｈ、Ｆ、Ｓ
等のガス成分含有量が総量で２００ｐｐｍ以下の極めて
純度の高い５Ｎレベルの高純度クロムが約１ｋｇ得られ
た。By irradiating the crude chromium raw material with an electron beam,
A molten pool of chromium metal was formed in the electron beam spot, but the area was small, and chromium evaporated immediately and 1
Metal chromium adhered to the ceiling and side walls of the condensation container maintained at 500 ° C. or lower. As described above, the metal chromium has an extremely high vapor pressure and evaporates immediately, so that the copper water-cooled crucible holding the raw material was not melted or broken at all. Then, hardly evaporable substances such as chromium oxide and other oxides, sulfides, carbides, and nitrides contained in the crude material remained in the crucible. Further, other volatile gas components were discharged out of the condensation vessel. The metallic chromium adhering to the ceiling and side walls of the condensing vessel is O, C, N, H, F, S
Approximately 1 kg of 5N-level high-purity chromium having extremely high purity and a total content of gas components such as 200 ppm or less was obtained.
【００１２】電子ビーム溶解後冷却し、凝縮容器の天井
や側壁に付着した金属クロムを剥がした。この剥離は極
めて容易であった。このようにして得た金属クロムの化
学分析により測定した。その結果を同様に表１に示す。
表１に示すように、酸素の低減が著しく、またＯ、Ｃ、
Ｎ、Ｈ、Ｆ、Ｓ等のガス成分の総量は２００ｐｐｍ以下
の４Ｎレベル以上の高純度クロムが得られた。このよう
にして得た高純度クロムを、真空溶解、鋳造等の工程を
経てスパッタリングターゲットに加工した。このターゲ
ットを使用してスパッタリングを実施したところ、３Ｎ
レベルの粗クロムに比べ、Ｏ、Ｃ、Ｎ、Ｈ、Ｆ、Ｓ等の
ガス成分に起因するスパッタリング中のスプラッシュ、
異常放電、パーティクルの発生が著しく減少した。After cooling by electron beam melting, the metal chromium adhering to the ceiling and side walls of the condensation vessel was peeled off. This peeling was extremely easy. The metal chromium thus obtained was measured by chemical analysis. Table 1 also shows the results.
As shown in Table 1, the oxygen reduction was remarkable, and O, C,
High purity chromium having a total amount of gas components such as N, H, F, and S of not more than 200 ppm and not less than 4N was obtained. The high-purity chromium thus obtained was processed into a sputtering target through steps such as vacuum melting and casting. When sputtering was performed using this target, 3N
Splash during sputtering due to gas components such as O, C, N, H, F, S, etc.
Abnormal discharge and generation of particles were significantly reduced.
【００１３】[0013]
【表１】 [Table 1]
【００１４】（実施例２）実施例１と同様に、図１に示
すような電子ビーム溶解装置を使用し、銅製の水冷坩堝
に精製前のＯ、Ｃ、Ｎ、Ｈ、Ｆ、Ｓ等のガス成分を多量
に含有する粗マンガン（原料）５ｋｇを導入した。この
原料の化学分析値を表２に示す。実施例１と同様に、坩
堝の上部に位置する凝縮容器の材料として純鉄を使用し
た。該凝縮容器の一部に開口した窓から原料粗マンガン
に電子ビームを照射した。電子ビーム溶解装置の真空度
は１〜２×１０−４ｍｍＨｇ（≒１．３３〜２．６６×
１０−２Ｐａ）に維持した。電子ビームによる溶解を
１．２Ａで１時間、実施した。Example 2 In the same manner as in Example 1, an electron beam melting apparatus as shown in FIG. 1 was used to place O, C, N, H, F, S, etc. before purification into a water-cooled copper crucible. 5 kg of crude manganese (raw material) containing a large amount of gas components was introduced. Table 2 shows the chemical analysis values of this raw material. As in the case of Example 1, pure iron was used as a material for the condensation vessel located at the top of the crucible. The raw material crude manganese was irradiated with an electron beam through a window opened in a part of the condensation vessel. The degree of vacuum of the electron beam melting apparatus is 1 to 2 × 10 −4 mmHg (≒ 1.33 to 2.66 ×
10 -2 Pa). Dissolution by electron beam was performed at 1.2 A for 1 hour.
【００１５】粗マンガン原料への電子ビーム照射によ
り、電子ビームスポットに金属マンガンの溶融プールが
形成されたが、その範囲は小さく、マンガンは直ちに蒸
発し、１５００°Ｃ以下に保持された凝縮容器の天井や
側壁に金属マンガンが付着した。実施例１と同様に、金
属マンガンは蒸気圧が極めて高く直ちに蒸発するので、
原料を保持する銅製の水冷坩堝が溶損や破壊することは
全くなかった。そして、粗原料中に含まれる二酸化マン
ガンやその他の酸化物、硫化物、炭化物、窒化物等の蒸
発し難い物質は坩堝内に残存した。またその他の揮発し
たガス成分は凝縮容器外に排出された。凝縮容器の天井
や側壁に付着した金属マンガンは蒸気圧の差異から、
Ｏ、Ｃ、Ｎ、Ｈ、Ｆ、Ｓ等のガス成分含有量が総量で１
００ｐｐｍ以下の極めて純度の高い５Ｎレベルの高純度
マンガンが約１ｋｇ得られた。Although the molten pool of metallic manganese was formed in the electron beam spot by the electron beam irradiation on the raw material of crude manganese, the range was small, the manganese was immediately evaporated, and the temperature of the condensation vessel maintained at 1500 ° C. or lower. Metal manganese adhered to the ceiling and side walls. As in Example 1, the metal manganese has an extremely high vapor pressure and evaporates immediately, so that
The copper water-cooled crucible holding the raw material was not melted or broken at all. Then, hardly evaporable substances such as manganese dioxide and other oxides, sulfides, carbides and nitrides contained in the crude material remained in the crucible. Further, other volatile gas components were discharged out of the condensation vessel. Metal manganese adhering to the ceiling and side walls of the condensation vessel, due to the difference in vapor pressure,
The total content of gas components such as O, C, N, H, F, and S is 1
About 1 kg of highly pure manganese of 5N level having a very high purity of not more than 00 ppm was obtained.
【００１６】電子ビーム溶解後冷却し、凝縮容器の天井
や側壁に付着した金属マンガンを剥がした。実施例１と
同様に、この剥離は極めて容易であった。このようにし
て得た金属マンガンの化学分析により測定した。その結
果を、同様に表２に示す。表２に示すように、酸素の低
減が著しく、またＯ、Ｃ、Ｎ、Ｈ、Ｆ、Ｓ等のガス成分
の総量は１００ｐｐｍ以下の４Ｎレベル以上の高純度マ
ンガンが得られた。実施例１と同様に、このようにして
得た高純度マンガンを、真空溶解、鋳造等の工程を経て
スパッタリングターゲットに加工した。このターゲット
を使用してスパッタリングを実施したところ、粗マンガ
ンに比べ、Ｏ、Ｃ、Ｎ、Ｈ、Ｆ、Ｓ等のガス成分に起因
するスパッタリング中のスプラッシュ、異常放電、パー
ティクルの発生が著しく減少した。After cooling by electron beam melting, metal manganese adhering to the ceiling and side walls of the condensation vessel was peeled off. As in Example 1, this peeling was extremely easy. The metal manganese thus obtained was measured by chemical analysis. The results are similarly shown in Table 2. As shown in Table 2, high-purity manganese with a remarkable reduction in oxygen and a total content of gas components such as O, C, N, H, F, and S of 100 ppm or less and 4N or more was obtained. As in Example 1, the high-purity manganese thus obtained was processed into a sputtering target through steps such as vacuum melting and casting. When sputtering was performed using this target, splash, abnormal discharge, and generation of particles during sputtering caused by gas components such as O, C, N, H, F, and S were significantly reduced as compared with crude manganese. .
【００１７】[0017]
【表２】 [Table 2]
【００１８】[0018]
【発明の効果】Ｏ、Ｃ、Ｎ、Ｈ、Ｆ、Ｓ等のガス成分を
多量に含有する粗金属から、電子ビームによりクロム、
マンガン等の金属特有の蒸気圧が高いことを利用し、高
純度化を目的とするクロム、マンガン等の金属を選択的
に蒸発・凝縮させて該ガス成分を大幅に減少させ、低コ
ストでかつ安全性が高い金属の製造方法を提供するもの
であり、さらに、これによって得られた高純度金属、高
純度金属からなるスパッタリングターゲット及びスパッ
タリングにより形成した薄膜を提供することができると
いう優れた効果を有する。また、これによって得られた
高純度ターゲットは、薄膜の電気・磁気的特性又は化学
的特性を改善するだけでなく、Ｏ、Ｃ、Ｎ、Ｈ、Ｆ、Ｓ
等のガス成分に起因するスパッタリング中のスプラッシ
ュ、異常放電、パーティクル等の発生が減少するという
著しい特長を有する。According to the present invention, from a crude metal containing a large amount of gas components such as O, C, N, H, F, and S, chromium,
Utilizing the high vapor pressure peculiar to metals such as manganese, the metals such as chromium and manganese for the purpose of high purification are selectively evaporated and condensed to significantly reduce the gas components, and at low cost and It is intended to provide a method for manufacturing a highly safe metal, and furthermore, to obtain an excellent effect of being able to provide a high-purity metal obtained thereby, a sputtering target composed of a high-purity metal, and a thin film formed by sputtering. Have. The high-purity target obtained thereby not only improves the electrical / magnetic or chemical properties of the thin film, but also improves the O, C, N, H, F, S
It has a remarkable feature that generation of splash, abnormal discharge, particles and the like during sputtering caused by gas components such as the above is reduced.
【図１】本発明に使用する電子ビーム溶解装置の断面概
念説明図である。FIG. 1 is a conceptual explanatory view of a cross section of an electron beam melting apparatus used in the present invention.
１ 坩堝 ２ 粗金属 ３ 凝縮容器 ４ 電子ビーム ５ 窓 ６ 金属クロム、金属マンガン等の蒸留金属 DESCRIPTION OF SYMBOLS 1 Crucible 2 Crude metal 3 Condensing container 4 Electron beam 5 Window 6 Distilled metal, such as metal chromium and metal manganese
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｃ２２Ｃ 27/06 Ｃ２２Ｃ 27/06 Ｃ２３Ｃ 14/34 Ｃ２３Ｃ 14/34 Ａ Ｆターム(参考） 4K001 AA08 AA16 BA23 DA06 DA07 EA13 FA12 GA16 4K029 BA02 BA07 CA05 DC08 ──────────────────────────────────────────────────の Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme coat ゛ (Reference) C22C 27/06 C22C 27/06 C23C 14/34 C23C 14/34 A F term (Reference) 4K001 AA08 AA16 BA23 DA06 DA07 EA13 FA12 GA16 4K029 BA02 BA07 CA05 DC08
Claims (5)
有量が総量で２００ｐｐｍ以下であることを特徴とする
高純度クロム又は高純度マンガンからなる高純度金属。1. A high-purity metal comprising high-purity chromium or high-purity manganese, wherein the total content of gas components such as O, C, N, H, F, and S is 200 ppm or less.
ッタリングターゲット及び該ターゲットを用いてスパッ
タリングにより形成した薄膜。2. A sputtering target comprising the high-purity metal according to claim 1, and a thin film formed by sputtering using the target.
多量に含有する粗金属を電子ビーム溶解し、揮発した金
属を凝縮して高純度金属を得ることを特徴とする高純度
金属の製造方法。3. A high-purity metal is obtained by electron beam melting a crude metal containing a large amount of gas components such as O, C, N, H, F, and S, and condensing a volatile metal. Production method of high purity metal.
特徴とする請求項３記載の高純度金属の製造方法。4. The method according to claim 3, wherein the metal is chromium or manganese.
ビームを照射して金属を溶解揮発させ、凝縮容器の天井
等に凝縮した高純度金属を回収することを特徴とする請
求項３又は４記載の高純度金属の製造方法。5. The method according to claim 1, wherein the coarse metal is put into a crucible, and the coarse metal is irradiated with an electron beam to dissolve and volatilize the metal, and recover the high-purity metal condensed on the ceiling of the condensing vessel. 5. The method for producing a high-purity metal according to 3 or 4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001182735A JP3979518B2 (en) | 2001-06-18 | 2001-06-18 | Manufacturing method of high purity metal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001182735A JP3979518B2 (en) | 2001-06-18 | 2001-06-18 | Manufacturing method of high purity metal |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2005102415A Division JP2005220444A (en) | 2005-03-31 | 2005-03-31 | High purity metal, sputtering target composed of high purity metal, thin film deposited by sputtering, and method for producing high purity metal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2002371325A true JP2002371325A (en) | 2002-12-26 |
| JP3979518B2 JP3979518B2 (en) | 2007-09-19 |
Family
ID=19022769
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2001182735A Expired - Fee Related JP3979518B2 (en) | 2001-06-18 | 2001-06-18 | Manufacturing method of high purity metal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3979518B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102994851A (en) * | 2012-10-29 | 2013-03-27 | 海门市金易焊接材料有限公司 | Low-carbon ferrochromium |
| CN107385240A (en) * | 2017-07-25 | 2017-11-24 | 北京兴荣源科技有限公司 | It is a kind of can mass production electrolysis chromium piece degasification technique |
-
2001
- 2001-06-18 JP JP2001182735A patent/JP3979518B2/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102994851A (en) * | 2012-10-29 | 2013-03-27 | 海门市金易焊接材料有限公司 | Low-carbon ferrochromium |
| CN107385240A (en) * | 2017-07-25 | 2017-11-24 | 北京兴荣源科技有限公司 | It is a kind of can mass production electrolysis chromium piece degasification technique |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3979518B2 (en) | 2007-09-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| TWI511926B (en) | High purity lanthanum, a high purity lanthanum, a sputtering target composed of high purity lanthanum, and a metal gate film having a high purity lanthanum as a main component | |
| US8926727B2 (en) | Apparatus and method for condensing metal vapor | |
| JP2002348621A (en) | Apparatus for collecting pure magnesium in magnesium alloy material, and method for recycling magnesium alloy material | |
| Shao et al. | Effect of La on the wettability of Al2O3 by molten aluminum | |
| JP2023107868A (en) | Method for producing high purity manganese and high purity manganese | |
| JP2615124B2 (en) | Lithium purification method | |
| JP2005220444A (en) | High purity metal, sputtering target composed of high purity metal, thin film deposited by sputtering, and method for producing high purity metal | |
| JP4900350B2 (en) | Manufacturing method to obtain high purity manganese | |
| JP2002371325A (en) | High purity metal, sputtering target consisting of high purity metal, thin film formed by sputtering, and method for manufacturing high purity metal | |
| JP5406157B2 (en) | Manufacturing method of high purity chromium, manufacturing method of sputtering target made of high purity chromium, and manufacturing method of thin film made of high purity chromium | |
| US4518421A (en) | Process for producing solid metal particles from a bath of metal | |
| JP4722403B2 (en) | Silicon purification apparatus and silicon purification method | |
| JP4007447B2 (en) | Method for producing high purity chromium | |
| JP2002206160A (en) | Thin film manufacturing apparatus thin film deposition method, and member for thin film manufacturing apparatus | |
| US3762911A (en) | Method of refining scrap especially of copper nickel alloy | |
| JPH0798980B2 (en) | Distillation purification method | |
| JP3673919B2 (en) | High-purity titanium recovery method | |
| JP2012072498A (en) | Sputtering target consisting of high purity manganese and thin film consisting of high purity manganese which is formed by sputtering | |
| Kroll | Vacuum metallurgy: its characteristics and its scope | |
| Vutova et al. | Electron-Beam Melting and Reuse of Metallic Materials | |
| KR100526039B1 (en) | Method for purifying magnesium scrap with vacuum distillation | |
| US3985551A (en) | Process for removing carbon from uranium | |
| JP6179699B1 (en) | Method for separating both from an alloy containing Dy and Tb | |
| WO2017170347A1 (en) | METHOD FOR SEPARATING Dy AND Tb FROM ALLOY CONTAINING BOTH | |
| CN113774241A (en) | Purification method of lanthanum-cerium alloy |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20041222 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20050215 |
|
| A521 | Written amendment |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20050331 |
|
| TRDD | Decision of grant or rejection written | ||
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20070619 |
|
| A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20070621 |
|
| R150 | Certificate of patent or registration of utility model |
Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20100706 Year of fee payment: 3 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20100706 Year of fee payment: 3 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20110706 Year of fee payment: 4 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20110706 Year of fee payment: 4 |
|
| S111 | Request for change of ownership or part of ownership |
Free format text: JAPANESE INTERMEDIATE CODE: R313111 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20110706 Year of fee payment: 4 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20110706 Year of fee payment: 4 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20120706 Year of fee payment: 5 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20120706 Year of fee payment: 5 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20130706 Year of fee payment: 6 |
|
| LAPS | Cancellation because of no payment of annual fees |