WO2012144655A1 - スパッタリングターゲット及びその製造方法 - Google Patents
スパッタリングターゲット及びその製造方法 Download PDFInfo
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- WO2012144655A1 WO2012144655A1 PCT/JP2012/061301 JP2012061301W WO2012144655A1 WO 2012144655 A1 WO2012144655 A1 WO 2012144655A1 JP 2012061301 W JP2012061301 W JP 2012061301W WO 2012144655 A1 WO2012144655 A1 WO 2012144655A1
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- sputtering target
- powder
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- material powder
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- 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
-
- 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
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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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
-
- 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
-
- 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
- C22C1/0425—Copper-based alloys
-
- 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
- C22C1/0483—Alloys based on the low melting point metals Zn, Pb, Sn, Cd, In or Ga
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
-
- 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
- a fifth invention is a method for producing a sputtering target according to any one of the first to fourth inventions, wherein at least each element of Cu, Ga and Sb is a single element or two or more of these elements
- a raw material powder made as a powder containing an alloy and a step of hot working the raw material powder in a vacuum, an inert atmosphere, or a reducing atmosphere, and the Ga contained in the raw material powder is a CuGa alloy or GaSb. It is contained as an alloy. That is, in the fifth invention, since Ga is contained as a raw material powder as a CuGa alloy or a GaSb alloy, Ga in the sintered body structure is more reliably alloyed than when only Ga is added to the raw material powder. It is possible to improve the machinability of the sintered body made of Cu, Ga, Sb.
- the sintering using the HIP method is preferably performed within the range of 400 ° C. to 620 ° C. of the HIP temperature (the holding temperature during HIP).
- the reason why the HIP temperature is set in the above range is that if the temperature is less than 400 ° C., the density of the sintered body is low and chipping is likely to occur during cutting, and if it exceeds 620 ° C., Sb dissolves in the HIP and burns. This is because it causes a compositional deviation in the body.
- the raw material powder produced by any of the above methods (a) to (d) is hot-pressed or HIP (hot isostatic pressing), or the raw material powder is pressure-molded, and then the compact is sintered, etc.
- the hot working is performed in a vacuum, an inert gas atmosphere, or a reducing gas atmosphere in order to prevent oxidation of the Cu—Ga alloy or Cu.
- the preferable pressure in the hot pressing is set to 100 to 500 kgf / cm 2 .
- a preferable pressure during HIP is 500-1500 kgf / cm 2 .
- the pressurization may be performed before the start of sintering temperature rise, or may be performed after reaching a certain temperature.
- the entire amount of Cu, Ga, Sb metal was charged into an atomizing device so as to be Cu 63.75 Ga 35 Sb 0.5 Na 0.5 S 0.25 (at%).
- the temperature is raised to 1150 ° C., and it is confirmed that all the metal is in a molten metal, and atomizing is performed to prepare a CuGaSb atomized powder.
- the obtained CuGaSb atomized powder has an average particle size of 1 ⁇ m or less.
- Na 2 S powder was added and mixed in a dry ball mill for 4 hours to produce mixed powders shown in Table 1.
- Example 18 As the raw material powder of Example 18, the entire amount of Cu, Ga, Sb metal was charged into an atomizing device so that Cu 63.75 Ga 35 Sb 0.5 Na 0.5 Se 0.25 (at%) was obtained. The temperature is raised to 1150 ° C., and it is confirmed that all the metal is in a molten metal, and atomizing is performed to prepare a CuGaSb atomized powder. Next, the obtained CuGaSb atomized powder has an average particle size of 1 ⁇ m or less. Na 2 Se powder was added and mixed in a dry ball mill for 4 hours to prepare mixed powders shown in Table 1.
- the mixed powder of Table 2 was produced by mixing for 4 hours in a ball mill.
- Comparative Example 4 the entire amount of Cu and Ga metals was charged into a vacuum melting apparatus so as to be Cu 75 Ga 25 (at%) in Table 2, and the temperature was raised to 1150 ° C., so that all the metal was molten. After confirming this, the hot water was poured out into a graphite mold to produce an ingot. The obtained ingot was further heated to 800 ° C. in nitrogen and held for 1 hour, and then rolled at a reduction rate of 5% / pass for a total of 4 passes. As the raw material powder of Comparative Example 5, the whole amount of Cu, Sb, and Ga metal was charged into an atomizer so as to be Cu 69.98 Ga 30 Sb 0.02 (at%), and the temperature was raised to 1150 ° C. After confirming that all the metal was melted, atomization was performed to prepare CuGaSb atomized powders in Table 2.
- Comparative Example 7 the entire amount of Cu, Ga, Sb metal was charged into a vacuum melting apparatus so as to be Cu 69.98 Ga 30 Sb 0.02 (at%) in Table 2, and the temperature was raised to 1150 ° C. After confirming that all the metal was melted, it was poured out into a graphite mold to prepare an ingot. The obtained ingot was further heated to 600 ° C. in nitrogen and maintained for 1 hour, and then rolled at a reduction rate of 5% / pass for a total of 4 passes.
- the processability and cutting effect were evaluated by first dry-processing the sintered CuGa sintered body or CuGaSb sintered body of the example or comparative example using a lathe manufactured by Mori Seiki Seisakusho: MS850G.
- the size of the sintered body was a diameter: ⁇ 80 mm and a thickness: 6 mm. Further, the rotational speed during processing was 140 rpm, the cutting amount of the cutting tool was 0.3 mm, and the feed speed was 0.097 mm / rev.
- the used processing bead (manufactured by Mitsubishi Materials) was a shape model number: STFER1616H16, an insert shape model number: TEGX160302L, and a material type was HTi10.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Powder Metallurgy (AREA)
- Physical Vapour Deposition (AREA)
Abstract
Description
すなわち、第2の発明では、Cu−Ga合金を主とする合金相の結晶粒中またはその粒界(以下、粒界等と略記する場合がある)に、Sb単体またはSbとCuとを含む化合物を含む組織を有するので、粒界等にあるSb単体またはSbとCuとを含む化合物によって快削性を発揮することができ、被切削性を向上させることができる。
上記各金属元素の組成評価は、スパッタリングターゲットを粉砕し、ICP法(高周波誘導結合プラズマ法)を用いて含有量を定量分析する。
成形後、真空または気圧0.01kgf/cm2~10kgf/cm2の不活性ガス雰囲気、または還元性雰囲気中にて非加圧状態で焼結する等の熱間加工する工程を有している。なお、上記原料粉末に含まれるGaがCuGa合金またはGaSb合金として含有されていることが好ましい。
実施例9の原料粉末としては、まずCu57Ga40Sb3(at%)になるように、Cu,Ga,Sbをアトマイズ装置に装入し、1150℃に昇温し、金属が全部溶湯になっていることを確認して、アトマイズを行うことでCu57Ga40Sb3(at%)のアトマイズ粉末を作製した。次に、Cu67Ga30Sb3(at%)になるように、Cu,Ga,Sbをアトマイズ装置に装入し、1150℃に昇温し、金属が全部溶湯になっていることを確認して、アトマイズを行うことでCu67Ga30Sb3(at%)のアトマイズ粉末を作製した。さらに、表1の組成になるように、得られた2組成のCuGaSbアトマイズ粉を乾式ボールミルにて4時間混合して、表1の所定の組成となるCu,Ga,Sb混合粉を作製した。
施例17の原料粉末としては、Cu63.75Ga35Sb0.5Na0.5S0.25(at%)となるようにCu,Ga,Sb金属の全量をアトマイズ装置に装入し、1150℃に昇温し、金属が全部溶湯になっていることを確認して、アトマイズを行うことでCuGaSbアトマイズ粉末を作製し、次に、得られたCuGaSbアトマイズ粉に、平均粒径1μm以下のNa2S粉末を投入し、乾式ボールミルにて4時間混合して表1の混合粉末を作製した。 実施例18の原料粉末としては、Cu63.75Ga35Sb0.5Na0.5Se0.25(at%)となるようにCu,Ga,Sb金属の全量をアトマイズ装置に装入し、1150℃に昇温し、金属が全部溶湯になっていることを確認して、アトマイズを行うことでCuGaSbアトマイズ粉末を作製し、次に、得られたCuGaSbアトマイズ粉に、平均粒径1μm以下のNa2Se粉末を投入し、乾式ボールミルにて4時間混合して表1の混合粉末を作製した。
、いずれも加工後チッピングが無く、面粗さRaが0.85以下、Rzが8.1以下と小さく優れた被切削性が得られている。なお、一例としてCu69Ga30Sb1(at%)とした本発明の実施例とCu69.9Ga30Sb0.01(at%)とした本発明の比較例との加工後におけるターゲット表面の写真を図1および図2に示す。
Claims (6)
- Ga:20~40at%、Sb:0.1~3at%、残部がCu及び不可避不純物からなる成分組成を有することを特徴とするスパッタリングターゲット。
- 請求項1に記載のスパッタリングターゲットにおいて、 Cu−Ga合金を主とする合金相の結晶粒内または粒界に、Sb単体またはSbとCuとを含む化合物の少なくとも一方を含む組織を有することを特徴とするスパッタリングターゲット。
- 請求項1に記載のスパッタリングターゲットにおいて、 スパッタリングターゲット素地中のGaがCu−Ga二元合金の形態で含有されていることを特徴とするスパッタリングターゲット。
- 請求項1に記載のスパッタリングターゲットにおいて、 さらに、Naが、NaF化合物、Na2S化合物またはNa2Se化合物として含有され、スパッタリングターゲット中の全金属元素に対し、Naが0.05~2at%含有されていることを特徴とするスパッタリングターゲット。
- 請求項1に記載のスパッタリングターゲットを作製する方法であって、 少なくともCu,GaおよびSbの各元素を単体またはこれらのうち2種以上の元素を含む合金として粉末とした原料粉末を作製する工程と、 前記原料粉末を真空、不活性雰囲気、または還元性雰囲気で熱間加工する工程を含み、 前記原料粉末に含まれるGaがCuGa合金またはGaSb合金として含有されていることを特徴とするスパッタリングターゲットの製造方法。
- 請求項4に記載のスパッタリングターゲットを作製する方法であって、 少なくともCu,GaおよびSbの各元素を単体またはこれらのうち2種以上の元素を含む合金として金属粉末とし、前記金属粉末にNaF粉末、Na2S粉末またはNa2Se粉末を混合して原料粉末を作製する工程と、 前記原料粉末を真空、不活性雰囲気、または還元性雰囲気で熱間加工する工程を含み、 前記原料粉末に含まれるGaがCuGa合金またはGaSb合金として含有されていることを特徴とするスパッタリングターゲットの製造方法。
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
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CN201280003518.XA CN103261473B (zh) | 2011-04-22 | 2012-04-20 | 溅射靶及其制造方法 |
KR1020137011164A KR101358345B1 (ko) | 2011-04-22 | 2012-04-20 | 스퍼터링 타겟 및 그 제조방법 |
US14/111,504 US9528181B2 (en) | 2011-04-22 | 2012-04-20 | Sputtering target and method for producing same |
EP12774193.2A EP2700735B1 (en) | 2011-04-22 | 2012-04-20 | Sputtering target and method for producing same |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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JP2011096591A JP5153911B2 (ja) | 2011-04-22 | 2011-04-22 | スパッタリングターゲット及びその製造方法 |
JP2011-096591 | 2011-04-22 |
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WO2012144655A1 true WO2012144655A1 (ja) | 2012-10-26 |
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PCT/JP2012/061301 WO2012144655A1 (ja) | 2011-04-22 | 2012-04-20 | スパッタリングターゲット及びその製造方法 |
Country Status (7)
Country | Link |
---|---|
US (1) | US9528181B2 (ja) |
EP (1) | EP2700735B1 (ja) |
JP (1) | JP5153911B2 (ja) |
KR (1) | KR101358345B1 (ja) |
CN (1) | CN103261473B (ja) |
TW (1) | TWI438296B (ja) |
WO (1) | WO2012144655A1 (ja) |
Cited By (1)
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CN105008580A (zh) * | 2013-02-25 | 2015-10-28 | 三菱综合材料株式会社 | 溅射靶及其制造方法 |
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US9822430B2 (en) | 2012-02-29 | 2017-11-21 | The United States Of America As Represented By The Secretary Of The Army | High-density thermodynamically stable nanostructured copper-based bulk metallic systems, and methods of making the same |
JP6176535B2 (ja) * | 2013-02-25 | 2017-08-09 | 三菱マテリアル株式会社 | スパッタリングターゲット及びその製造方法 |
CN105579599A (zh) * | 2013-09-27 | 2016-05-11 | 攀时奥地利公司 | 铜镓溅射靶材 |
CN108772567A (zh) * | 2018-06-29 | 2018-11-09 | 米亚索乐装备集成(福建)有限公司 | 一种用于cig靶材打底层的合金材料、cig靶材及其制备方法 |
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2011
- 2011-04-22 JP JP2011096591A patent/JP5153911B2/ja not_active Expired - Fee Related
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2012
- 2012-04-20 US US14/111,504 patent/US9528181B2/en active Active
- 2012-04-20 CN CN201280003518.XA patent/CN103261473B/zh not_active Expired - Fee Related
- 2012-04-20 EP EP12774193.2A patent/EP2700735B1/en not_active Not-in-force
- 2012-04-20 TW TW101114153A patent/TWI438296B/zh not_active IP Right Cessation
- 2012-04-20 WO PCT/JP2012/061301 patent/WO2012144655A1/ja active Application Filing
- 2012-04-20 KR KR1020137011164A patent/KR101358345B1/ko active IP Right Grant
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105008580A (zh) * | 2013-02-25 | 2015-10-28 | 三菱综合材料株式会社 | 溅射靶及其制造方法 |
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EP2700735B1 (en) | 2016-08-17 |
TW201307593A (zh) | 2013-02-16 |
JP2012229454A (ja) | 2012-11-22 |
TWI438296B (zh) | 2014-05-21 |
US20140048414A1 (en) | 2014-02-20 |
EP2700735A4 (en) | 2014-10-01 |
CN103261473A (zh) | 2013-08-21 |
KR101358345B1 (ko) | 2014-02-06 |
CN103261473B (zh) | 2016-01-20 |
EP2700735A1 (en) | 2014-02-26 |
JP5153911B2 (ja) | 2013-02-27 |
KR20130059458A (ko) | 2013-06-05 |
US9528181B2 (en) | 2016-12-27 |
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