US20140123810A1 - Preparation method of Ruthenium(Ru) powder for preparation of Ruthenium target - Google Patents
Preparation method of Ruthenium(Ru) powder for preparation of Ruthenium target Download PDFInfo
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- US20140123810A1 US20140123810A1 US14/115,597 US201214115597A US2014123810A1 US 20140123810 A1 US20140123810 A1 US 20140123810A1 US 201214115597 A US201214115597 A US 201214115597A US 2014123810 A1 US2014123810 A1 US 2014123810A1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0466—Alloys based on noble metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F2009/001—Making metallic powder or suspensions thereof from scrap particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Definitions
- the present invention is related to a producing method of Ruthenium (Ru) raw material powder used in manufacturing a target or other Ru compound.
- the present invention is related to a producing method of Ru powder material, wherein Ruthenium (Ru) oxide is produced by applying a heat process to high purity powder produced by plasma, Ru oxide is changed into a refined shape through pulverization, high purity Ru powder is produced through an atmospheric heat process and thereby, a production yield and purity of powder can be improved.
- Ruthenium (Ru) oxide is produced by applying a heat process to high purity powder produced by plasma, Ru oxide is changed into a refined shape through pulverization, high purity Ru powder is produced through an atmospheric heat process and thereby, a production yield and purity of powder can be improved.
- a large capacity and a high integrity related to a magnetic recording medium or next-generation memory are required very eagerly.
- the present invention provides a producing method of Ru powder material which is widely used in a seed layer for forming a magnetic layer.
- the present invention is related to a producing method of high purity Ru powder, wherein coarse powder is produced by applying plasma to a waste Ru target, Ru oxide is generated through a heat process, refined powder is finally acquired through a pulverization process, and high purity powder is produced through an atmospheric heat process.
- the present invention is related to a producing method of refined powder, wherein a production time is reduced, content of impure substances in powder can be controlled, Ru powder is produced by using plasma, and refined powder having a particle size of below 5 ⁇ m through a pulverization process is produced.
- a Ru thin film is frequently used. Further, since Ru powder for manufacturing a Ru sputtering target for a thin film molding is very expensive, Ru powder is produced by recycling a waste Ru target. A degree of purity is deteriorated due to continuous recycling of Ru. In order to prevent deterioration of purity and to easily control a thickness of a thin film, a technology for refining a crystal particle of a target and for producing high purity powder is required eagerly. A Ru target having refined crystal particles and high functionality is produced through a sintering process, and refined and high purity Ru powder is demanded in order to control crystal particles.
- a Ru target requires high purity and this requirement is to be satisfied to improve a degree of uniformity of a thin film.
- simplification of processes are required and gas content is also controlled so as to prevent impure substances not to be introduced during the whole processes.
- gas content is also controlled so as to prevent impure substances not to be introduced during the whole processes.
- wet method using acids employs a post heat process for selectively removing carbon which is mixed with Ru by using mainly a carbon mold. The oxygen content is increased through this heat process. Particling is formed on the properties of a thin film because of increase of oxygen and thus, fatal defects are generated.
- Japanese Patent Laid-Open Publication No. 2009-108400 discloses a manufacturing method using a waste Ru target, wherein powder is produced through a rough pulverization, a hammer milling, deposition and extraction, a magnetic selection, a dry process, deoxidizing and a heat process.
- the method of the above-mentioned patent it can solve the problems that much quantity of acid solution is used in a conventional wet method and oxygen content increases in the dry method. Further, the production time of powder can be shortened.
- the present invention is related to a manufacturing method of high purity and refined Ru powder by using waste Ru target.
- the present invention employs an eco-friendly dry method instead of a conventional wet method. That is, the object of the present invention is to produce high purity powder by using plasma, and to finally produce high purity and refined Ru powder by increasing a production yield of powder when a refined pulverization process is executed, and preventing a degree of purity of powder from being deteriorated. When powder is produced in this way, it is possible to produce high purity and refined Ru powder on a large scale.
- the object of the present invention is to produce coarse powder through a forced dispersing process, instead of evaporated/condensed powder of Nano Scale when producing high purity of powder by using a plasma device, and to finally produce ultra high purity and refined Ru powder by applying a refined pulverization process and a heat process to the produced powder.
- the present invention is characterized in that it produces coarse powder by forcibly dispersing a waste Ru target by using a plasma device, Ru oxide is acquired through an oxidation process at the same time carbon is removed for easily performing a refined pulverization process, and ultra high purity powder can be produced by applying an atmospheric heat process to the finally oxidized powder.
- the present invention has the merits as follows.
- powder is produced by forcibly dispersing ingots by using plasma.
- a wet process can be omitted and pulverization can be easily performed by oxidizing coarse powder into a metal oxide.
- a production time of the final powder can be reduced and refined and high purity Ru powder can also be produced.
- functional improvement of a Ru sputtering target material produced by a sintering method is expected.
- FIG. 1 is a diagram illustrating a working procedure for producing Ru powder by using a waste Ru target of the present invention.
- FIG. 2 is a diagram illustrating FESEM image of final Ru powder produced according to the present invention.
- the present invention provides a manufacturing method of Ru powder comprising a step for removing pollutants remaining on a surface of a waste Ru target and washing the surface; a step for forming a plasma atmosphere by decompressing an inside of a plasma device, injecting a reaction gas, and applying electricity after introducing the washed waste Ru target into the plasma device; a step for producing Ru powder by increasing a plasma electricity and then, forcibly dispersing ingots; a step for selectively removing carbon by applying an atmospheric heat process to the produced Ru powder in order to produce Ru oxide (RuOx) powder; a step for pulverizing the produced Ru oxide (RuOx) powder into refined shape for producing refined Ru powder; and a step for producing high purity Ru powder by applying a hydrogen atmospheric heat process to the produced Ru oxide (RuOx) powder.
- the present invention is characterized in that when producing Ru powder, powder is produced by forcibly dispersing ingots by using plasma and thereby, coarse high purity powder is produced, a metal oxide is produced through a heat process, carbon which is mixed with Ru is selectively removed and simultaneously, pulverization can be easily executed, powder is pulverized into refined powder having an average particle size of 5 ⁇ m through a refined pulverization process, and a final refined and high purity Ru powder is produced through an atmospheric heat process.
- the processing time is reduced remarkably and condensation generated due to a heat process is suppressed as compared with a conventional plasma method. Therefore, it is possible to produce Ru powder which is suitable for refined and high purity sinter. Further, it is also possible to realize a production yield more than 95% and to produce powder having an average particle size of 5 ⁇ m.
- FIG. 1 a production method of the final powder is illustrated in FIG. 1 .
- the present invention is characterized in that it includes a step (S 10 ) for removing pollutants remaining on a surface of a waste Ru target by using a chemical method and washing the surface; a step (S 20 ) for forming a plasma atmosphere by decompressing an inside of a plasma device, injecting a reaction gas, and applying electricity after introducing the washed waste Ru target into the plasma device; a step (S 30 ) for producing Ru powder by increasing a plasma electricity and then, forcibly dispersing ingots; a step (S 40 ) for selectively removing carbon by applying an atmospheric heat process to the produced Ru powder in order to produce Ru oxide (RuOx) powder; a step (S 50 ) for pulverizing the produced Ru oxide (RuOx) powder into refined shape for producing refined Ru powder; and a step (S 60 ) for producing high purity Ru powder by applying a hydrogen atmospheric heat process to the produced Ru oxide (RuOx) powder.
- a chemical method wherein a waste Ru target is deposited in a solvent for a short time, and a surface side is cut by several tens of ⁇ m is employed, or a physical method including the mechanical processing methods such as a lathe or a grinding machine or MCT and the like. Thereby, a constant thickness layer is removed.
- pollutants are removed by the mechanical processing methods, it is possible to remove a thickness of approximately 10 ⁇ m. The main reason of it is that an oxidation layer may not be removed completely if the thickness to be removed is too thin and yield of the final powder may be reduced if the thickness to be removed is too thick.
- a plasma atmosphere is formed by decompressing an inside of a plasma device, injecting a reaction gas, and applying electricity after introducing the waste Ru target in which pollutants are removed into the plasma device (S 20 ).
- a waste Ru target is mounted on the mold of the washed inside of the chamber and the distance between a plasma torch and a target is adjusted.
- the material of an electrode used for forming plasma is very important and it is also important to minimize contamination.
- Molybdenum (Mo), Tungsten (W), Copper (Cu), Graphite, and Ruthenium (Ru) can be used as an anode mold material. It is important to minimize contamination due to a mold in order to prevent a degree of purity of a final powder from being deteriorated. Even if contamination is generated due to a mold, it is very essential to select a mold in which pollution can be easily removed. For realizing this purpose, it is possible that a carbon for which pollution can be easily removed is very advantageous. More preferably, even if pollution is generated, it is possible to use a high purity Ru mold which does not affect a degree of purity at all.
- Molybdenum (Mo), Tungsten (W) and Ruthenium (Ru) can be used as a cathode mold material used in a plasma process. It is possible to use Ru of the same material for producing high purity powder.
- Plasma is formed by decompressing an inside of a plasma device, injecting a reaction gas, and applying electricity.
- a pressure is reduced to 10 ⁇ 1 torr by a vacuum pump in order to form plasma, a reaction gas is injected and a working vacuum degree is adjusted. Then, electricity is provided.
- Ar, H 2 , N 2 , CH 4 , or the mixed gases such as Ar+H 2 , and Ar+N 2 can be used as a reaction gas.
- H 2 , N 2 , and O 2 remain in a final Ru powder.
- H 2 , N 2 , O 2 are manufactured as a target for use in a semiconductor line, they affect a process for forming particles during a film forming process.
- the working vacuum level is set at approximately 100-300 torr. If the level is below 100 torr, the amount of inert gas required for forming plasma is very small. Thus, a direct transfer of heat is difficult. If the level is above 300 torr, a forced dispersing due to plasma is not almost formed.
- a vacuum level is adjusted through other cooling gas element attached to a device or a vacuum level control valve.
- Ru is produced by increasing electricity and forcibly dispersing ingot. Then, Ru oxide (RuOx) powder is produced by selectively removing carbon through a heat process (S 30 , S 40 ).
- the object of the atmospheric heat process is to remove carbon and to easily pulverize powder into refined shape by forming a Ru oxide.
- a heat process condition in case of the atmospheric heat process, it is possible that a heat process is performed at a temperature of 800-1200° C. for 1-5 hours. There is a high possibility that the remaining carbon may not be removed sufficiently and sufficient oxidization may not be realized if a temperature is below 800° C. and the process time is below 1 hour. There is a high possibility that produced powder may be condensed if a temperature is above 1200° C. and the process time is above 5 hours.
- Refined Ru powder is produced by pulverizing the produced Ru oxide (RuOx) powder (S 50 ). Ru powder undergoing the atmospheric heat process are pulverized into refined shape. At this time, it is possible to employ Jet-Mill, Planetary Mill and Ball Mill as a pulverization method. It is to be understood that Jet-Mill can be used as a pulverization method. The main reason of it is that Jet-Mill method has the most strong pulverization power and introduction of impure substances can be easily and most importantly controlled. Pure Ru metal is not pulverized even by Jet-Mill, but pulverization is performed very smoothly and easily in case of Ru oxide (RuOx).
- the rotation speed of an inside classifier of Jet-Mill ranges from 1500 RPM to 15,000 RPM. If the speed becomes below 1,500 RPM, the particle size of powder is becoming too coarse. If the speed becomes above 15,000 RPM, the production yield of powder is reduced tremendously and remarkably. In particular, if the particle size of powder is too refined during a subsequent atmospheric heat process, inert energy is reduced and thus, condensation of powder is generated. If the particle size of powder is too coarse, the crystal particle size of a final target increases. Therefore, it is most possible that a particle size of powder becomes approximately 5 ⁇ m according to the experiment results.
- High purity Ru powder is produced by applying a hydrogen atmosphere heat process to the refined Ru oxide powder (S 60 ).
- the minutely pulverized Ru oxide powder is deoxidized and becomes high purity Ru powder through a hydrogen atmosphere heat process.
- a heat process is performed at the temperature of 800-1200° C. for 1-5 hours.
- the main reason of it is as follows. In a case that a heat process is performed at temperature below 800° C. and for less than 1 hour, deoxidization of Ru oxide is not realized sufficiently. In a case that a heat process is performed at temperature above 1,200° C. and for more than 5 hours, there is a high possibility that powders may be condensed. At this time, it is possible that oxygen content contained in the deoxidized Ru powder becomes below 600 ppm.
- target of high density can be produced when sintering is performed if the oxygen content is below 400 ppm.
- a reaction surface space is increased by performing a hydrogen atmosphere heat process and thus, the oxygen content in Ru powder is controlled so that high purity Ru powder can be produced.
- Ru powder 1 kg of a Ru target having a degree of purity of 3N5 was prepared in order to produce Ru powder.
- a chemical process was applied to a waste Ru target from which foreign substances were removed by using a heat plasma device of 100 kw class, and thereby, Ru powder of 800 g was produced.
- the process procedures and the conditions are as follows.
- a target is placed on a carbon mold and then, is mounted on an equipment. Subsequently, a pressured is reduced to 1 ⁇ 10 ⁇ 1 torr by using a rotary pump and then, an atmosphere is formed by N 2 gas. Plasma of 20 kw is applied to the atmosphere by using plasma of a mixed gas including Ar+N 2 .
- Ru powder produced in this way has a shape of a hollow center and has a particle size of 10-300 ⁇ m. Carbon contained in powder is removed through an atmospheric heat process at 850° C. for producing a Ru oxide. The Ru oxide powder is produced by Jet-Mill under a condition such as 300 g/hr and thereby, the average particle size of 5.2 ⁇ m is acquired.
- the powder acquired in this way is processed through a hydrogen atmosphere heat process at 850° C. for 4 hours and thus, a pure Ru powder can be produced.
- ICP Induction Coupled Plasma
- an oxygen content is 380 ppm.
- purity of powder is improved as a whole.
- Ru powder having a shape of a hollow center is produced by applying plasma to the target which is same as the specification described in the embodiment 1.
- An atmospheric heat process is applied to the powder acquired in this manner at 850° C. for 4 hours. Therefore, carbon is removed and Ru oxide is formed.
- a hydrogen atmosphere heat process is applied to the power at 850° C. for 4 hours, so that Ru deoxidization can be realized. It turned out that the final particle size of Ru powder acquired in this way is 10-300 ⁇ m and the oxygen content is 2,000 ppm. As is apparent from this fact, it is to be understood that deterioration of purity is generated.
- Ru powder having a shape of a hollow center is produced by applying plasma to the target which is same as the specification described in the embodiment 1. After pulverizing the Ru powder having a shape of a hollow center by using Jet-Mill under the condition same as that described in the embodiment 1, an atmospheric heat process is applied to the Ru powder at 850° C. for 4 hours. Then, a hydrogen atmosphere heat process is applied to the Ru power at 850° C. for 4 hours for acquiring final powder. It turned out that the particle size of Ru powder acquired in this way is 9.4 ⁇ m and the oxygen content is 1,500 ppm.
- ingot is forcibly dispersed by using plasma for producing powder. It is possible to omit a wet process and it is also possible to easily perform pulverization by changing coarse powder into a metal oxide. Through these processes, the production time of a final powder can be shortened. Further, high purity and refined Ru powder can be produced. Therefore, it is expected that a function of a Ru sputtering target material produced according to a sintering method is improved.
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Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
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KR1020110042657A KR101206416B1 (ko) | 2011-05-04 | 2011-05-04 | 루테늄(Ru)타겟 제조를 위한 루테늄 분말 제조방법 |
KR10-2011-0042657 | 2011-05-04 | ||
PCT/KR2012/000741 WO2012150757A1 (ko) | 2011-05-04 | 2012-01-31 | 루테늄(Ru)타겟 제조를 위한 루테늄 분말 제조방법 |
Publications (1)
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US20140123810A1 true US20140123810A1 (en) | 2014-05-08 |
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US14/115,597 Abandoned US20140123810A1 (en) | 2011-05-04 | 2012-01-31 | Preparation method of Ruthenium(Ru) powder for preparation of Ruthenium target |
Country Status (5)
Country | Link |
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US (1) | US20140123810A1 (ja) |
JP (1) | JP5733732B2 (ja) |
KR (1) | KR101206416B1 (ja) |
SG (1) | SG194655A1 (ja) |
WO (1) | WO2012150757A1 (ja) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114289727A (zh) * | 2021-12-09 | 2022-04-08 | 贵研铂业股份有限公司 | 一种高均质微粒径高纯钌粉及其制备方法 |
Families Citing this family (6)
Publication number | Priority date | Publication date | Assignee | Title |
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KR20150003580A (ko) * | 2013-07-01 | 2015-01-09 | 희성금속 주식회사 | 루테늄 분말 및 루테늄 타겟의 제조방법 |
KR20150049883A (ko) * | 2013-10-31 | 2015-05-08 | 희성금속 주식회사 | 스퍼터링 폐 타겟의 재생방법 및 이에 의해 재생된 스퍼터링 타겟 |
KR20160050485A (ko) * | 2014-10-29 | 2016-05-11 | 희성금속 주식회사 | 루테늄 또는 루테늄 합금계 스퍼터링 타겟의 제조방법 및 이로부터 제조된 루테늄 또는 루테늄 합금계 스퍼터링 타겟 |
KR20160050491A (ko) * | 2014-10-29 | 2016-05-11 | 희성금속 주식회사 | 루테늄 또는 루테늄 합금계 스퍼터링 폐타겟의 재생방법 및 이로부터 제조된 균일한 결정립을 갖는 루테늄 또는 루테늄 합금계 재활용 스퍼터링 타겟 |
JP7296232B2 (ja) * | 2019-03-27 | 2023-06-22 | 株式会社フルヤ金属 | 中実球状粉末の製造方法及び造形製品の製造方法 |
CN114105228B (zh) * | 2021-11-25 | 2022-08-19 | 西北有色金属研究院 | 一种厚膜电阻用氧化钌的制备方法 |
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US20090229412A1 (en) * | 2006-04-14 | 2009-09-17 | Hiroshi Takashima | Process for producing low-oxygen metal powder |
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US20140105777A1 (en) * | 2011-04-26 | 2014-04-17 | Won Kyu Yoon | Production method for ultra-high-purity ruthenium(ru) powder and target by using waste ruthenium(ru) targets |
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JPH09227965A (ja) * | 1996-02-19 | 1997-09-02 | Mitsubishi Materials Corp | 精製金属ルテニウム粉末とその製造方法 |
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JP2007070650A (ja) * | 2005-09-02 | 2007-03-22 | Asahi Pretec Corp | ルテニウム酸化物の製法およびルテニウム粉末の製法 |
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KR101175676B1 (ko) * | 2010-03-25 | 2012-08-22 | 희성금속 주식회사 | 폐 루테늄(Ru) 타겟을 이용한 고순도화 및 미세화된 루테늄(Ru)분말 제조법 |
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2011
- 2011-05-04 KR KR1020110042657A patent/KR101206416B1/ko active IP Right Grant
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2012
- 2012-01-31 JP JP2014509236A patent/JP5733732B2/ja not_active Expired - Fee Related
- 2012-01-31 WO PCT/KR2012/000741 patent/WO2012150757A1/ko active Application Filing
- 2012-01-31 US US14/115,597 patent/US20140123810A1/en not_active Abandoned
- 2012-01-31 SG SG2013079744A patent/SG194655A1/en unknown
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US6589311B1 (en) * | 1999-07-07 | 2003-07-08 | Hitachi Metals Ltd. | Sputtering target, method of making same, and high-melting metal powder material |
US20090229412A1 (en) * | 2006-04-14 | 2009-09-17 | Hiroshi Takashima | Process for producing low-oxygen metal powder |
KR20110074168A (ko) * | 2009-12-24 | 2011-06-30 | 희성금속 주식회사 | 루테늄(Ru)폐타겟을 이용한 루테늄(Ru) 분말 및 루테늄(Ru) 타겟 재료 제조방법 |
US20140105777A1 (en) * | 2011-04-26 | 2014-04-17 | Won Kyu Yoon | Production method for ultra-high-purity ruthenium(ru) powder and target by using waste ruthenium(ru) targets |
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CN114289727A (zh) * | 2021-12-09 | 2022-04-08 | 贵研铂业股份有限公司 | 一种高均质微粒径高纯钌粉及其制备方法 |
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WO2012150757A1 (ko) | 2012-11-08 |
KR20120124803A (ko) | 2012-11-14 |
SG194655A1 (en) | 2013-12-30 |
KR101206416B1 (ko) | 2012-11-29 |
JP2014518939A (ja) | 2014-08-07 |
JP5733732B2 (ja) | 2015-06-10 |
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