WO2012108074A1 - インジウムターゲット及びその製造方法 - Google Patents

インジウムターゲット及びその製造方法 Download PDF

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Publication number
WO2012108074A1
WO2012108074A1 PCT/JP2011/070388 JP2011070388W WO2012108074A1 WO 2012108074 A1 WO2012108074 A1 WO 2012108074A1 JP 2011070388 W JP2011070388 W JP 2011070388W WO 2012108074 A1 WO2012108074 A1 WO 2012108074A1
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WO
WIPO (PCT)
Prior art keywords
target
indium
indium target
crystal structure
cross
Prior art date
Application number
PCT/JP2011/070388
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English (en)
French (fr)
Japanese (ja)
Inventor
瑶輔 遠藤
坂本　勝
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Jx日鉱日石金属株式会社
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Publication date
Application filed by Jx日鉱日石金属株式会社 filed Critical Jx日鉱日石金属株式会社
Priority to KR1020127015985A priority Critical patent/KR101261202B1/ko
Priority to CN201180004828.9A priority patent/CN102782181B/zh
Publication of WO2012108074A1 publication Critical patent/WO2012108074A1/ja

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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
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy

Definitions

  • the present invention relates to a sputtering target and a manufacturing method thereof, and more particularly to an indium target and a manufacturing method thereof.
  • Indium is used as a sputtering target for forming a light absorption layer of a Cu—In—Ga—Se (CIGS) thin film solar cell.
  • CGS Cu—In—Ga—Se
  • an indium target is produced by depositing indium or the like on a backing plate, then providing a mold on the backing plate, pouring indium into the mold, and casting it. Has been.
  • the indium target produced by such a conventional melt casting method still has room for improvement in the stability of the sputtering characteristics such as the deposition rate and discharge voltage from the start to the end of sputtering.
  • an object of the present invention is to provide an indium target having stable sputtering characteristics such as a film formation rate and a discharge voltage from the start to the end of sputtering and a method for manufacturing the indium target.
  • the present inventors have made extensive studies to solve the above problems, and found that the shape of the structure of the indium target greatly affects the stability of the sputtering characteristics such as the sputtering rate and discharge voltage from the start to the end of sputtering. It was. That is, an indium target in which a columnar crystal structure extending in the thickness direction of the target from one surface of the target to the other surface is formed is more sputtered than an indium target in which such a columnar crystal structure is not formed. It was found that the sputtering characteristics such as the film formation rate and discharge voltage from the end to the end become stable. In addition, in the conventional melt casting method, indium is poured into a mold and then cooled and cast to obtain an indium ingot.
  • the indium poured into the mold is cooled and cast, it grows. Focusing on the fact that the structure of indium becomes a mixed structure of granular crystals and columnar crystals, and that the particle size varies depending on the difference in cooling rate of each part, and by controlling the cooling rate at this time, the columnar crystals described above are controlled. It was found that an organization can be formed.
  • the present invention completed on the basis of the above knowledge has, in one aspect, a columnar crystal structure extending in the thickness direction of the target from one surface of the target to the other surface, and the volume content of the columnar crystal structure is 90-100. % Indium target.
  • the volume content of the columnar crystal structure is 95 to 100%.
  • the average grain size of the columnar crystal structure is 0.1 to 50 mm in a cross section in a direction perpendicular to the thickness direction of the target.
  • the indium target according to the present invention has a Cu, Ni or Fe concentration of 1000 wtppm or less.
  • the molten indium raw material is poured into a mold, and the entire surface of at least the upper surface of the indium raw material poured into the mold is uniformly cooled with a refrigerant to change from a molten state to a solid state. And completing the phase change within 15 minutes.
  • the completion of solidification is when the temperature of the point in the indium farthest from the part where the refrigerant is in direct or indirect contact is below the freezing point of indium of 156 ° C.
  • the temperature at the interface between the backing plate and indium is 156 ° C. or less, and measurement may be performed by inserting a thermocouple into the indium in a region that does not interfere with target production.
  • the temperature of the back surface of the backing plate which is a temperature above the target interface, may be measured.
  • the present invention is a method of heating an indium target, dividing the indium target immediately before melting, and observing and evaluating the exposed cross section.
  • the indium target is exposed immediately before melting. This is a method for evaluating a cross section of an indium target when the temperature of the cross-sectional site is 156 ° C.
  • an indium target having stable sputtering characteristics such as a film forming rate and a discharge voltage from the start to the end of sputtering and a method for manufacturing the indium target.
  • the indium target according to the present invention is formed in a rectangular or circular plate shape having a thickness of 5 to 20 mm. As shown in FIGS. 1 and 2 and FIGS. 4 and 5, the indium target according to the present invention has a columnar crystal structure extending in the thickness direction of the target from one surface of the target to the other surface.
  • FIG. 1 is a cross-sectional photograph of an indium target produced by solidifying in 20 seconds using water as a coolant from the surface of the target in a casting process of the indium target described later.
  • FIG. 2 is a cross-sectional photograph of an indium target produced by solidifying in 10 seconds using ice as a coolant from the surface of the target in the casting process of the indium target.
  • FIG. 1 is a cross-sectional photograph of an indium target produced by solidifying in 20 seconds using water as a coolant from the surface of the target in a casting process of the indium target described later.
  • FIG. 2 is a cross-sectional photograph of an indium target produced by solid
  • FIG. 3 is a cross-sectional photograph of an indium target produced by solidifying over 17 minutes by cooling without using a refrigerant in the indium target casting process.
  • 4 to 6 are schematic cross-sectional views of the indium target corresponding to FIGS. 1 to 3, respectively.
  • the indium target prepared by rapidly cooling the entire surface at least from the surface direction of the target at a predetermined cooling rate using a coolant in the casting process is the thickness of the target from one surface of the target to the other surface.
  • a columnar crystal structure extending in the direction is formed. Therefore, the surface to be sputtered from the start to the end of the sputtering always has the same crystal distribution, and it is possible to maintain the same characteristics as the initial stage of sputtering even after the sputtering progresses and the erosion becomes deep.
  • the indium target produced by cooling in the casting process is a mixture of a granular structure and a columnar structure, and the columnar structure does not reach the other surface from one surface of the target.
  • the volume content of the columnar structure is also small.
  • a target has a columnar crystal structure extending from the surface and side surfaces in the target, and further has a granular crystal in the center of the target. For this reason, as sputtering progresses and erosion deepens, each crystal on the sputtered surface shows a distribution different from that in the initial stage of sputtering. For this reason, from the start to the end of sputtering, the erosion method becomes non-uniform and the sputtering characteristics become unstable.
  • the volume content of the columnar crystal structure is 90 to 100%.
  • a granular structure and a columnar structure are not mixed, but a columnar crystal structure extending in the thickness direction of the target from one surface of the target to the other surface, and its volume.
  • the sputtering characteristics such as the film formation rate and discharge voltage from the end to the end become stable.
  • the volume content of the columnar crystal structure is preferably 92 to 100%, more preferably 95 to 100%. When the volume content of the columnar crystal structure is less than 90%, variations in sputtering characteristics begin to be observed.
  • the average grain size of the columnar crystal structure may be 0.1 to 50 mm in the cross section in the direction perpendicular to the thickness direction of the target. According to such a form, the total number of particles existing in the sputter surface increases, so that variations in sputter characteristics depending on the crystal plane to be sputtered can be offset, and the entire sputter surface exhibits uniform characteristics.
  • the average particle size of the columnar crystal structure is preferably 0.1 to 10 mm, more preferably 0.1 to 5 mm.
  • the concentration of Cu, Ni, or Fe which is a metal derived from the backing plate, is 1000 wtppm or less. According to the present invention, since the cooling rate is made faster than the cooling rate, the amount of impurities mixed into the target is reduced accordingly, and the reduction in conversion efficiency of the finally produced solar cell can be suppressed.
  • the concentration of Cu, Ni or Fe is preferably 500 wtppm or less, more preferably 300 wtppm or less.
  • the indium raw material is melted and poured into a mold provided on a backing plate.
  • the indium raw material to be used preferably has a high purity because the conversion efficiency of the solar cell produced by the raw material is reduced when impurities are contained. For example, the purity is 99.99.
  • An indium raw material having a mass% or more can be used.
  • the phase change from the molten state to the solidified state is completed within 15 minutes to form an indium target.
  • the refrigerant used at this time include cold air, water, oil, alcohol and the like.
  • cold air the indium raw material is cooled directly or indirectly.
  • water, oil, alcohol or the like the indium raw material is indirectly cooled. Cooling with a refrigerant may be performed not only from the upper surface side of the indium raw material poured into the mold, but also from the side surface side and / or the bottom surface side in order to improve the efficiency of the process.
  • the columnar crystal structure grows well by quenching the indium raw material poured into the mold. Further, the contact time with the backing plate in the casting process is shortened, and the contamination of impurities such as Cu, Ni or Fe derived from the backing plate is suppressed accordingly.
  • the time required for the phase change of the indium raw material is preferably within 5 minutes, more preferably within 1 minute.
  • the obtained indium target is processed to a desired thickness and shape by a machining center, a milling cutter, or a scraper, and if necessary, pickling or degreasing is performed.
  • the indium target thus obtained can be suitably used as a sputtering target for the light absorption layer for CIGS thin film solar cells.
  • Example 1 A cylindrical mold having an inner diameter of 205 mm and a height of 15 mm was fixed on a copper backing plate having a diameter of 250 mm and a thickness of 5 mm, and an indium raw material (purity 4N) melted at 180 ° C. was poured into the inside to a depth of 10 mm. After that, ice water was used as a coolant from the upper surface, and the phase change from the molten state to the solid state was completed in 10 seconds. Further, the mold was removed and the lathe was processed to form a disk-shaped indium target (diameter 204 mm ⁇ thickness 5 mm). .
  • an indium raw material purity 4N
  • Example 2 An indium target was produced under the same conditions as in Example 1 except that water was used as a refrigerant and the phase change from the indium molten state to the solid state was completed in 20 seconds.
  • Example 3 An indium target was produced under the same conditions as in Example 1 except that cold air was used as the refrigerant and the phase change from the indium molten state to the solid state was completed in 300 seconds.
  • Example 4 An indium target was produced under the same conditions as in Example 1 except that the phase change from the indium molten state to the solid state was completed in 500 seconds using the atmosphere (air blowing) as the refrigerant.
  • Example 1 An indium target was produced under the same conditions as in Example 1 except that the indium raw material of the mold was cooled to the atmosphere and the phase change from the indium molten state to the solid state was completed in 1000 seconds.
  • Example 2 The indium raw material was melted at 250 ° C., the indium raw material of the mold was cooled by air cooling, and the phase change from the molten state to the solid state was completed in 1800 seconds under the same conditions as in Example 1. A target was produced.
  • the indium targets obtained in the examples and the comparative examples are each evaluated by observing the exposed cross section by heating the indium target and splitting the indium target immediately before melting. “Just before melting” is when the temperature of the cross-sectional portion where the indium target is exposed reaches 156 ° C.
  • the target may be folded or bent by holding both sides of the cross-sectional portion of the target to be observed immediately before melting. Indium that has reached 156 ° C is very easy to break along the grain boundaries.
  • the method of applying the force of folding or bending is used. May be.
  • the target may be held by hand and the aforementioned force may be applied, or the target may be applied by grasping the target with a tool such as pliers.
  • the crystal structure of this cross section was photographed with a digital camera, and the volume content of the columnar crystal structure was evaluated. Note that the crystal structure of the above-mentioned cross section of the indium target cannot be observed accurately by the conventional observation method.
  • the conventional method of exposing the cross section by cutting since the surface is licked as it is, the crystal grain boundary cannot be observed, and etching is performed to expose the crystal grain boundary. become. In such a method, at the stage of cutting, the cross section is distorted and recrystallized, and the original crystal grain boundary cannot be observed.
  • the exposure of the cross section includes exposure due to breakage after cooling with liquid nitrogen, but the indium target in the present invention cannot be broken even by cooling with liquid nitrogen, and thus such a method cannot be adopted.
  • the crystal structure of the cross section of the indium target is observed by the method as described above, the original crystal grain boundary can be accurately observed.
  • the average particle diameter of the columnar crystal structure of the cross section in the direction perpendicular to the thickness direction of the indium target obtained in the examples and comparative examples was evaluated by the following method.
  • the cross section was photographed with a digital camera, and the number (N) of crystal grains existing in an arbitrary region (rectangle, area Smm 2 ) of the cross section of the image was counted.
  • the number of crystal grains existing across the boundary of the region was 0.5
  • the number of crystal grains present in the square was 0.25.
  • the average area (s) of the crystal grains was calculated by dividing the area (S) of the measurement target region by N. Assuming that the crystal grains are spheres, the average crystal grain size (A) was calculated by the following formula.
  • A 2 (s / ⁇ ) 1/2
  • the impurity concentration (copper concentration derived from the backing plate) of the indium target obtained in the examples and comparative examples was evaluated by ICP emission analysis (manufactured by Seiko Instrument Inc., SPS3000 ICP emission spectrometer).
  • Sputtering device Canon Anelva, SPF-313H ⁇ Target size: ⁇ 8 inch x 5mmt ⁇ Sputtering gas: Ar ⁇ Sputtering gas pressure: 0.5Pa ⁇ Sputtering gas flow rate: 50 SCCM Sputtering temperature: T.A. (No heating) ⁇ Sputtering power density: 2.0 W / cm 2 -Substrate: Corning Eagle 2000, ⁇ 4 inch x 0.7 mmt Each measurement result is shown in Tables 1 and 2. Moreover, the evaluation result of the film-forming rate and discharge voltage in Table 2 is shown in FIGS. 7 and 8, respectively.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)
PCT/JP2011/070388 2011-02-09 2011-09-07 インジウムターゲット及びその製造方法 WO2012108074A1 (ja)

Priority Applications (2)

Application Number Priority Date Filing Date Title
KR1020127015985A KR101261202B1 (ko) 2011-02-09 2011-09-07 인듐 타깃 및 그 제조 방법
CN201180004828.9A CN102782181B (zh) 2011-02-09 2011-09-07 铟靶材及其制造方法

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JP2011026090A JP5086452B2 (ja) 2011-02-09 2011-02-09 インジウムターゲット及びその製造方法
JP2011-026090 2011-02-09

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104583452A (zh) * 2012-08-22 2015-04-29 Jx日矿日石金属株式会社 铟制圆筒型溅射靶及其制造方法
US9490108B2 (en) 2010-09-01 2016-11-08 Jx Nippon Mining & Metals Corporation Indium target and method for manufacturing same
US9758860B2 (en) 2012-01-05 2017-09-12 Jx Nippon Mining & Metals Corporation Indium sputtering target and method for manufacturing same
US9922807B2 (en) 2013-07-08 2018-03-20 Jx Nippon Mining & Metals Corporation Sputtering target and method for production thereof

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Publication number Priority date Publication date Assignee Title
CN102925868B (zh) * 2012-11-29 2014-12-10 研创应用材料（赣州）有限公司 一种制备铟靶材金属薄膜的方法
JP5746252B2 (ja) * 2013-03-28 2015-07-08 光洋應用材料科技股▲分▼有限公司 正方晶系結晶構造を有するインジウムターゲット
CN108165936A (zh) * 2017-12-21 2018-06-15 清远先导材料有限公司 制备铟靶材的方法
CN113652652B (zh) * 2021-07-20 2023-04-07 先导薄膜材料（广东）有限公司 一种铟靶材及其制备方法

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JPS63241167A (ja) * 1987-03-30 1988-10-06 Seiko Epson Corp スパツタリング用タ−ゲツト
JPS63262461A (ja) * 1987-04-21 1988-10-28 Mitsubishi Kasei Corp スパツタリングタ−ゲツト
JPS6411968A (en) * 1987-07-06 1989-01-17 Seiko Epson Corp Manufacture of sputtering target
JPH01289562A (ja) * 1988-05-17 1989-11-21 Hitachi Ltd スパツタリング用ターゲットの製造方法
JPH05125523A (ja) * 1991-11-06 1993-05-21 Daido Steel Co Ltd ターゲツト材とその製造方法
JPH11158612A (ja) * 1997-12-01 1999-06-15 Mitsubishi Materials Corp 溶解ルテニウムスパッタリングターゲット
WO1999066099A1 (fr) * 1998-06-17 1999-12-23 Tanaka Kikinzoku Kogyo K.K. Materiau cible pour projection
JP2003286565A (ja) * 2002-03-27 2003-10-10 Mitsubishi Materials Corp スパッタリング用ターゲット及びその製造方法
JP2004091819A (ja) * 2002-08-29 2004-03-25 Mitsubishi Materials Corp スパッタリング用ターゲット、その製造方法及びターゲット部材
JP2005113174A (ja) * 2003-10-03 2005-04-28 Tanaka Kikinzoku Kogyo Kk スパッタリング用ルテニウムターゲット及びスパッタリング用ルテニウムターゲットの製造方法
JP2009203499A (ja) * 2008-02-26 2009-09-10 Mitsubishi Materials Corp ターゲット材およびその製造方法
JP2010024474A (ja) * 2008-07-16 2010-02-04 Sumitomo Metal Mining Co Ltd インジウムターゲットの製造方法

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DE10063383C1 (de) * 2000-12-19 2002-03-14 Heraeus Gmbh W C Verfahren zur Herstellung eines Rohrtargets und Verwendung
JP4528995B2 (ja) * 2007-08-02 2010-08-25 国立大学法人東北大学 Ｓｉバルク多結晶インゴットの製造方法

Patent Citations (12)

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Publication number Priority date Publication date Assignee Title
JPS63241167A (ja) * 1987-03-30 1988-10-06 Seiko Epson Corp スパツタリング用タ−ゲツト
JPS63262461A (ja) * 1987-04-21 1988-10-28 Mitsubishi Kasei Corp スパツタリングタ−ゲツト
JPS6411968A (en) * 1987-07-06 1989-01-17 Seiko Epson Corp Manufacture of sputtering target
JPH01289562A (ja) * 1988-05-17 1989-11-21 Hitachi Ltd スパツタリング用ターゲットの製造方法
JPH05125523A (ja) * 1991-11-06 1993-05-21 Daido Steel Co Ltd ターゲツト材とその製造方法
JPH11158612A (ja) * 1997-12-01 1999-06-15 Mitsubishi Materials Corp 溶解ルテニウムスパッタリングターゲット
WO1999066099A1 (fr) * 1998-06-17 1999-12-23 Tanaka Kikinzoku Kogyo K.K. Materiau cible pour projection
JP2003286565A (ja) * 2002-03-27 2003-10-10 Mitsubishi Materials Corp スパッタリング用ターゲット及びその製造方法
JP2004091819A (ja) * 2002-08-29 2004-03-25 Mitsubishi Materials Corp スパッタリング用ターゲット、その製造方法及びターゲット部材
JP2005113174A (ja) * 2003-10-03 2005-04-28 Tanaka Kikinzoku Kogyo Kk スパッタリング用ルテニウムターゲット及びスパッタリング用ルテニウムターゲットの製造方法
JP2009203499A (ja) * 2008-02-26 2009-09-10 Mitsubishi Materials Corp ターゲット材およびその製造方法
JP2010024474A (ja) * 2008-07-16 2010-02-04 Sumitomo Metal Mining Co Ltd インジウムターゲットの製造方法

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9490108B2 (en) 2010-09-01 2016-11-08 Jx Nippon Mining & Metals Corporation Indium target and method for manufacturing same
US9758860B2 (en) 2012-01-05 2017-09-12 Jx Nippon Mining & Metals Corporation Indium sputtering target and method for manufacturing same
CN104583452A (zh) * 2012-08-22 2015-04-29 Jx日矿日石金属株式会社 铟制圆筒型溅射靶及其制造方法
EP2818575A4 (en) * 2012-08-22 2016-01-20 Jx Nippon Mining & Metals Corp INDIUM CYLINDRICAL CATHODIC SPUTTERING TARGET AND METHOD OF MANUFACTURING SAME
US9761421B2 (en) 2012-08-22 2017-09-12 Jx Nippon Mining & Metals Corporation Indium cylindrical sputtering target and manufacturing method thereof
US9922807B2 (en) 2013-07-08 2018-03-20 Jx Nippon Mining & Metals Corporation Sputtering target and method for production thereof

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TWI398409B (zh) 2013-06-11
CN102782181B (zh) 2015-11-25
JP5086452B2 (ja) 2012-11-28
KR20120115971A (ko) 2012-10-19
JP2012162792A (ja) 2012-08-30
CN102782181A (zh) 2012-11-14
KR101261202B1 (ko) 2013-05-10
TW201233632A (en) 2012-08-16

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