US20040144204A1 - Airu spattering target and method for preparation thereof - Google Patents

Airu spattering target and method for preparation thereof Download PDF

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Publication number
US20040144204A1
US20040144204A1 US10/479,687 US47968703A US2004144204A1 US 20040144204 A1 US20040144204 A1 US 20040144204A1 US 47968703 A US47968703 A US 47968703A US 2004144204 A1 US2004144204 A1 US 2004144204A1
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United States
Prior art keywords
alru
sputtering target
sintering
intermetallic compound
manufacturing
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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.)
Abandoned
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US10/479,687
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English (en)
Inventor
Akira Hisano
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Nippon Mining Holdings Inc
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Individual
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Assigned to NIKKO MATERIALS COMPANY, LIMITED reassignment NIKKO MATERIALS COMPANY, LIMITED ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HISANO, AKIRA
Publication of US20040144204A1 publication Critical patent/US20040144204A1/en
Assigned to NIPPON MINING & METALS CO., LTD. reassignment NIPPON MINING & METALS CO., LTD. CHANGE OF NAME (SEE DOCUMENT FOR DETAILS). Assignors: NIKKO MATERIALS CO., LTD.
Priority to US11/733,016 priority Critical patent/US7767139B2/en
Abandoned legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C5/00—Alloys based on noble metals
    • C22C5/04—Alloys based on a platinum group metal
    • 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
    • C22C1/047—Making non-ferrous alloys by powder metallurgy comprising intermetallic compounds
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy

Definitions

  • the present invention pertains to an AlRu sputtering target, and particularly to an AlRu sputtering target favorable in forming films for hard disks, as well as the manufacturing method thereof.
  • targets composed of a positive electrode and a negative electrode are made to face each other, and high voltage is applied between the substrate and target under an inert gas atmosphere in order to generate an electric field.
  • sputtering method there are the high frequency sputtering (RF) method, magnetron sputtering method, DC (direct current) sputtering method, among others, and these methods are suitably used in accordance with the target material or conditions for forming the film.
  • RF high frequency sputtering
  • magnetron sputtering method magnetron sputtering method
  • DC (direct current) sputtering method among others, and these methods are suitably used in accordance with the target material or conditions for forming the film.
  • Al—50 at % Ru is employed compositionally, but since the dissolution temperature of this composition is 2000° C. or higher, it is difficult to employ a dissolution casting product as a target from the perspective of manufacturing costs.
  • FIG. 5 The SEM image, Ru distribution image, Al distribution image and O distribution image of a conventional Al—50 at % Ru sintered body target surface are shown in FIG. 5, FIG. 6, FIG. 7 and FIG. 8, respectively.
  • An object of the present invention is to enable the stable and low-cost manufacture of an AlRu sputtering target having an even texture and capable of significantly reducing oxygen, and to prevent or suppress the generation of particles and improve the yield ratio of deposition goods.
  • the present inventors discovered that the oxygen content can be reduced, generation of particles can be prevented or suppressed, and the yield ratio of manufacture can be significantly improved by improving the manufacturing process and sintering process of powder.
  • An AlRu sputtering target characterized in that it is a sintered body composed of an AlRu intermetallic compound of 95 vol. % or more;
  • a manufacturing method of an AlRu sputtering target characterized in performing high frequency dissolution to raw materials Al and Ru, preparing powder having as its principal component an Al 13 Ru 4 intermetallic compound by pulverizing the ingot after dissolution or with the atomization method, and, after mixing Ru powder to this powder having as its principal component an Al 13 Ru 4 intermetallic compound, performing sintering by hot pressing or hot isostatic pressing (HIP);
  • FIG. 1 is a diagram showing the SEM image of the AlRu intermetallic compound sintered body sputtering target of the present invention
  • FIG. 2 is a diagram showing the Ru distribution image of the AlRu intermetallic compound sintered body sputtering target of the present invention
  • FIG. 3 is a diagram showing the Al distribution image of the AlRu intermetallic compound sintered body sputtering target of the present invention
  • FIG. 4 is a diagram showing the O distribution image of the AlRu intermetallic compound sintered body sputtering target of the present invention.
  • FIG. 5 is a diagram showing the SEM image of a conventional Al—50 at % Ru sintered body target
  • FIG. 6 is a diagram showing the Ru distribution image of a conventional Al—50 at % Ru sintered body target
  • FIG. 7 is a diagram showing the Al distribution image of a conventional Al—50 at % Ru sintered body target.
  • FIG. 8 is a diagram showing the O distribution image of a conventional Al—50 at % Ru sintered body target.
  • the AlRu sputtering target of the present invention has a significant characteristic in that it is a sintered body composed of an AlRu intermetallic compound of 95 vol. % or more. Since an even texture of an AlRu intermetallic compound can be obtained, there is a significant effect in that an even film can be formed during sputtering deposition.
  • the texture is formed only of an AlRu intermetallic compound, the existence of free Al, Ru or other intermetallic compounds less than 45 vol. % will not significantly affect the quality of deposition, and this degree of content is tolerable.
  • the oxygen content of the AlRu sputtering target of the present invention is 1500 wtppm or less, thus having an oxygen content that is extremely reduced, and the target surface is therefore even. Further, it is also possible to obtain an AlRu sputtering target having a relative density of 90% or more.
  • FIG. 1 shows an SEM image, which is an example of the AlRu sputtering target of the present invention. As shown in FIG. 1, an even surface is obtained.
  • FIG. 2 and FIG. 3 show the distribution images of Ru and Al, and it is evident that there is no significant segregation within the target and that it is superior in evenness.
  • FIG. 4 shows the distribution image of oxygen. It is clear from FIG. 4 that the oxygen content is extremely low and dispersed.
  • the target of the present invention Upon manufacturing the target of the present invention, after the Al and Ru raw materials are cast or prepared such as the target composition of atomized powder becomes Al 13 Ru 4 (the molar ratio of Al and Ru is approximately 3 to 4:1), this is dissolved at a high frequency.
  • the oxygen content in the hot metal or ingot as a result of this high frequency dissolution can be made 100 wtppm or less.
  • An ingot is obtained after dissolving and casting the above, and this is pulverized to obtain powder having as its principal component an Al 13 Ru 4 intermetallic compound.
  • the dissolution of this component ratio can be carried out at a relatively low temperature of roughly 1400 to 1450° C., and a high temperature such as 2000° C. described above is not necessary.
  • the obtained Al 13 Ru 4 intermetallic compound can easily be crushed, there is a characteristic in that the manufacture of powder is facilitated.
  • Ru powder is mixed with this powder having as its principal component an Al 13 Ru 4 intermetallic compound, and this is sintered by hot pressing or hot isostatic pressing (HIP).
  • the amount of Ru powder to be mixed shall be the ultimately obtained amount of AlRu intermetallic compound. It is desirable that sintering is performed with powder having an average particle size of 50 to 100 ⁇ m. Further, in accordance with the sintering conditions, it would also be possible to employ powder other than the average particle size described above.
  • the sintering temperature is set between 1300 and 1500° C., and sintering is performed at a sintering pressure of 150 Kgf/cm 2 or more. In order to reduce oxygen even further, it is desirable that sintering is performed in a vacuum. As a result, it is possible to obtain a sputtering target composed of an AlRu intermetallic compound in which the oxygen content is 1500 wtppm or less, and having a relative density of 90% or more.
  • the Al and Ru raw materials were prepared to be a 20 Kg raw material where Al 3.25 mol:Ru 1 mol, respectively, and this was dissolved at a high frequency (in a vacuum).
  • the dissolution temperature was 1650° C. As a result of this high frequency vacuum dissolution, it was possible to suppress the oxygen content in the hot metal to 50 wtppm.
  • Ru powder having the same particle size as the powder having as its principal component Al 13 Ru 4 intermetallic compound was mixed thereto, and this mixed powder was filled in a graphite dice for sintering.
  • the amount of Ru powder to be mixed was made to be the ultimately obtained amount of AlRu intermetallic compound.
  • a sintered body block was obtained by sintering at a sintering temperature of 1350° C. and a sintering pressure of 200 Kgf/cm 2 . A block of this was further cut out and processed into a target upon performing surface grinding or the like.
  • the Al and Ru raw materials were prepared to be a 20 Kg raw material where Al 3.25 mol:Ru 1 mol, respectively, and this was dissolved at a high frequency (in a vacuum).
  • the dissolution temperature was 1650° C. As a result of this high frequency vacuum dissolution, it was possible to suppress the oxygen content in the hot metal to 50 wtppm.
  • Ru powder having the same particle size as the powder having as its principal component Al 13 Ru 4 intermetallic compound was mixed thereto, and this mixed powder was filled in a graphite dice for sintering.
  • the amount of Ru powder to be mixed was made to be the ultimately obtained amount of AlRu intermetallic compound.
  • a sintered body block was obtained by sintering at a sintering temperature of 1450° C. and a sintering pressure of 200 Kgf/cm 2 . A block of this was further cut out and processed into a target upon performing surface grinding or the like.
  • the Al and Ru raw materials were prepared to be a 20 Kg raw material where Al 3.25 mol: Ru 1 mol, respectively, and this was dissolved at a high frequency (in a vacuum).
  • the dissolution temperature was 1650° C. As a result of this high frequency vacuum dissolution, it was possible to suppress the oxygen content in the hot metal to 50 wtppm.
  • Ru powder having the same particle size as the powder having as its principal component Al 13 Ru 4 intermetallic compound was mixed thereto, and this mixed powder was filled in a graphite dice for sintering.
  • the amount of Ru powder to be mixed was made to be the ultimately obtained amount of AlRu intermetallic compound.
  • a sintered body block was obtained by sintering at a sintering temperature of 1550° C. and a sintering pressure of 200 Kgf/cm 2 . A block of this was further cut out and processed into a target upon performing surface grinding or the like.
  • the Al and Ru raw material powders having an average particle size of 75 ⁇ m were prepared to be a mixed powder where Al 1 mol:Ru 1 mol, respectively, and this was filled in a graphite dice for sintering.
  • a sintered body block was obtained by sintering at a sintering temperature of 600° C. and a sintering pressure of 200 Kgf/cm 2 . A block of this was further cut out and processed into a target upon performing surface grinding or the like.
  • the AlRu sputtering target falling within the scope of the present invention disclosed in the Examples is capable of obtaining an even texture of AlRu intermetallic compound.
  • an even film can be formed.
  • the oxygen content of the AlRu intermetallic compound sputtering target of the present invention is 1500 wtppm or less, thus having an oxygen content that is extremely reduced, and the target surface (erosion face) is therefore even. Further, it is also possible to obtain an AlRu sputtering target having a relative density of 90% or more. In addition, there is no significant segregation within the target and the evenness is superior.
  • the oxygen content in the hot metal or ingot can be made 100 wtppm or less by performing high frequency dissolution to the Al and Ru raw materials.
  • An ingot is obtained after dissolving and casting the above, and this is pulverized to obtain powder having as its principal component an Al 13 Ru 4 intermetallic compound.
  • the dissolution of this component ratio can be carried out at a relatively low temperature of roughly 1400 to 1450° C., and a characteristic is yielded in that the manufacturing cost can be reduced.
  • cost can be reduced for the pulverizing process since the obtained Al 13 Ru 4 intermetallic compound can easily be crushed, and pulverization is facilitated thereby.
  • the sintering temperature is set between 1300 and 1500° C., and sintering is performed at a sintering pressure of 150 Kgf/cm 2 or more. And, by performing sintering in a vacuum, the oxygen content can be reduced even more.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Vapour Deposition (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Manufacturing Of Magnetic Record Carriers (AREA)
US10/479,687 2002-06-24 2003-05-08 Airu spattering target and method for preparation thereof Abandoned US20040144204A1 (en)

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US11/733,016 US7767139B2 (en) 2002-06-24 2007-04-09 AlRu sputtering target and manufacturing method thereof

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JP2002182713 2002-06-24
JP2002-182713 2002-06-24
PCT/JP2003/005757 WO2004001092A1 (fr) 2002-06-24 2003-05-08 Cible de pulverisation alru et son procede de preparation

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JP (2) JPWO2004001092A1 (fr)
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WO (1) WO2004001092A1 (fr)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007054256A1 (fr) * 2005-11-08 2007-05-18 Hansgrohe Ag Equipement sanitaire comportant un revetement
WO2007062089A1 (fr) * 2005-11-22 2007-05-31 Bodycote Imt, Inc. Fabrication de cibles d'electropulverisation au ruthenium ou en alliage au ruthenium a faible teneur en oxygene
US20070240992A1 (en) * 2004-03-01 2007-10-18 Nippon Mining & Metals Co., Ltd. High- Purity Ru Powder, Sputtering Target Obtained by Sintering the Same, Thin Film Obtained by Sputtering the Target and Process for Producing High-Purity Ru Powder
US20090114535A1 (en) * 2005-06-16 2009-05-07 Nippon Mining & Metals Co., Ltd. Ruthenium-Alloy Sputtering Target
US20090173627A1 (en) * 2006-02-22 2009-07-09 Nippon Mining & Metals Co., Ltd. Sintered Sputtering Target Made of Refractory Metals
US20090280025A1 (en) * 2005-10-14 2009-11-12 Nippon Mining & Metals Co., Ltd. High-Purity Ru Alloy Target, Process for Producing the Same, and Sputtered Film
US20110191706A1 (en) * 2004-08-17 2011-08-04 Dirtt Environmental Solutions Ltd. Automatically creating and modifying furniture layouts in design software
EP3106540A4 (fr) * 2014-03-27 2017-10-18 JX Nippon Mining & Metals Corp. CIBLE DE PULVÉRISATION CATHODIQUE COMPRENANT UN ALLIAGE Ni-P OU UN ALLIAGE Ni-Pt-P ET SON PROCÉDÉ DE PRODUCTION
US10319571B2 (en) 2012-07-30 2019-06-11 Jx Nippon Mining & Metals Corporation Ruthenium sputtering target and ruthenium alloy sputtering target

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JP5342810B2 (ja) * 2008-06-09 2013-11-13 株式会社コベルコ科研 Ａｌ基合金スパッタリングターゲット材の製造方法
JP5459494B2 (ja) * 2010-03-28 2014-04-02 三菱マテリアル株式会社 磁気記録媒体膜形成用スパッタリングターゲットおよびその製造方法
JP6461543B2 (ja) * 2013-10-08 2019-01-30 株式会社フルヤ金属 アルミニウムと希土類元素との合金ターゲット及びその製造方法
US9675796B2 (en) 2013-11-10 2017-06-13 Brainsgate Ltd. Implant and delivery system for neural stimulator
US10271907B2 (en) 2015-05-13 2019-04-30 Brainsgate Ltd. Implant and delivery system for neural stimulator
KR102150214B1 (ko) * 2019-12-03 2020-08-31 주식회사 이엠엘 물리증착용 고내식 컬러 합금 소재 및 고밀도 타겟 제조 방법
JPWO2022004354A1 (fr) * 2020-06-30 2022-01-06

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US5011554A (en) * 1989-12-26 1991-04-30 General Electric Company Ruthenium aluminum intermetallic compounds
US20020014406A1 (en) * 1998-05-21 2002-02-07 Hiroshi Takashima Aluminum target material for sputtering and method for producing same

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JP4058777B2 (ja) 1997-07-31 2008-03-12 日鉱金属株式会社 薄膜形成用高純度ルテニウム焼結体スパッタリングターゲット及び同ターゲットをスパッタリングすることによって形成される薄膜
JP2989169B2 (ja) * 1997-08-08 1999-12-13 日立金属株式会社 Ｎｉ−Ａｌ系金属間化合物ターゲットおよびその製造方法ならびに磁気記録媒体
US6736947B1 (en) 1997-12-24 2004-05-18 Kabushiki Kaisha Toshiba Sputtering target, A1 interconnection film, and electronic component
JPH11293454A (ja) * 1998-04-14 1999-10-26 Hitachi Metals Ltd Ａｌ系スパッタリング用ターゲット材及びその製造方法
JP2000017433A (ja) * 1998-07-07 2000-01-18 Hitachi Metals Ltd Ｂ２規則格子金属間化合物ターゲットおよび磁気記録媒体
JP2000034563A (ja) 1998-07-14 2000-02-02 Japan Energy Corp 高純度ルテニウムスパッタリングターゲットの製造方法及び高純度ルテニウムスパッタリングターゲット
EP1724364B1 (fr) 2004-03-01 2014-01-22 JX Nippon Mining & Metals Corporation Procédure de fabrication d'une poudre Ruthenium de grande pureté et une cible de pulvérisation de celui-ci.
JP5234735B2 (ja) 2005-06-16 2013-07-10 Ｊｘ日鉱日石金属株式会社 タンタル−ルテニウム合金スパッタリングターゲット
US7871564B2 (en) 2005-10-14 2011-01-18 Jx Nippon Mining & Metals Corporation High-purity Ru alloy target, process for producing the same, and sputtered film

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US5011554A (en) * 1989-12-26 1991-04-30 General Electric Company Ruthenium aluminum intermetallic compounds
US20020014406A1 (en) * 1998-05-21 2002-02-07 Hiroshi Takashima Aluminum target material for sputtering and method for producing same

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7578965B2 (en) 2004-03-01 2009-08-25 Nippon Mining & Metals Co., Ltd. High-purity Ru powder, sputtering target obtained by sintering the same, thin film obtained by sputtering the target and process for producing high-purity Ru powder
US20070240992A1 (en) * 2004-03-01 2007-10-18 Nippon Mining & Metals Co., Ltd. High- Purity Ru Powder, Sputtering Target Obtained by Sintering the Same, Thin Film Obtained by Sputtering the Target and Process for Producing High-Purity Ru Powder
US20110191706A1 (en) * 2004-08-17 2011-08-04 Dirtt Environmental Solutions Ltd. Automatically creating and modifying furniture layouts in design software
US9732413B2 (en) 2005-06-16 2017-08-15 Jx Nippon Mining & Metals Corporation Ruthenium-alloy sputtering target
US20090114535A1 (en) * 2005-06-16 2009-05-07 Nippon Mining & Metals Co., Ltd. Ruthenium-Alloy Sputtering Target
US20090280025A1 (en) * 2005-10-14 2009-11-12 Nippon Mining & Metals Co., Ltd. High-Purity Ru Alloy Target, Process for Producing the Same, and Sputtered Film
US7871564B2 (en) 2005-10-14 2011-01-18 Jx Nippon Mining & Metals Corporation High-purity Ru alloy target, process for producing the same, and sputtered film
US20080280158A1 (en) * 2005-11-08 2008-11-13 Hansgrophe Ag Coated Sanitaryware Item
DE102005054463B4 (de) * 2005-11-08 2016-10-27 Hansgrohe Se Beschichteter Gegenstand, Beschichtungsverfahren sowie Target für ein PVD-Verfahren
WO2007054256A1 (fr) * 2005-11-08 2007-05-18 Hansgrohe Ag Equipement sanitaire comportant un revetement
WO2007062089A1 (fr) * 2005-11-22 2007-05-31 Bodycote Imt, Inc. Fabrication de cibles d'electropulverisation au ruthenium ou en alliage au ruthenium a faible teneur en oxygene
US20090173627A1 (en) * 2006-02-22 2009-07-09 Nippon Mining & Metals Co., Ltd. Sintered Sputtering Target Made of Refractory Metals
US8118984B2 (en) 2006-02-22 2012-02-21 Jx Nippon Mining & Metals Corporation Sintered sputtering target made of refractory metals
US10319571B2 (en) 2012-07-30 2019-06-11 Jx Nippon Mining & Metals Corporation Ruthenium sputtering target and ruthenium alloy sputtering target
US10943773B2 (en) 2012-07-30 2021-03-09 Jx Nippon Mining & Metals Corporation Ruthenium sputtering target and ruthenium alloy sputtering target
EP3106540A4 (fr) * 2014-03-27 2017-10-18 JX Nippon Mining & Metals Corp. CIBLE DE PULVÉRISATION CATHODIQUE COMPRENANT UN ALLIAGE Ni-P OU UN ALLIAGE Ni-Pt-P ET SON PROCÉDÉ DE PRODUCTION

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US20070175753A1 (en) 2007-08-02
JP2008179892A (ja) 2008-08-07
WO2004001092A1 (fr) 2003-12-31
TW200400276A (en) 2004-01-01
US7767139B2 (en) 2010-08-03
JPWO2004001092A1 (ja) 2005-10-20
TWI225893B (en) 2005-01-01

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