US20040245099A1 - Sputtering target and production method therefor - Google Patents

Sputtering target and production method therefor Download PDF

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Publication number
US20040245099A1
US20040245099A1 US10/492,310 US49231004A US2004245099A1 US 20040245099 A1 US20040245099 A1 US 20040245099A1 US 49231004 A US49231004 A US 49231004A US 2004245099 A1 US2004245099 A1 US 2004245099A1
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grain size
crystal grain
target
average crystal
average
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US10/492,310
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Atsushi Hukushima
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Nippon Mining Holdings Inc
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Assigned to NIKKO MATERIALS COMPANY, LIMITED reassignment NIKKO MATERIALS COMPANY, LIMITED ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HUKUSHIMA, ATSUSHI
Publication of US20040245099A1 publication Critical patent/US20040245099A1/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 US12/617,966 priority Critical patent/US8029629B2/en
Abandoned legal-status Critical Current

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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
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • 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
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18—High-melting or refractory metals or alloys based thereon
    • C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon

Definitions

  • the present invention pertains to a sputtering target having a complex three-dimensional (stereoscopic) structure formed by die forging, and the manufacturing method thereof.
  • a sputtering target suitable for forming films of complex shapes and forming circuits is in demand.
  • a target having a three-dimensional (stereoscopic) structure in which the cross section is of a hat shape or dome shape, or a combination thereof is now being used.
  • a target having this kind of three-dimensional structure is manufactured by performing hot forging to an ingot or billet formed by dissolving and casting metal, thereafter performing annealing thereto, and further performing die forging thereto.
  • the hot forging performed to the ingot or billet will destroy the cast structure, disperse or eliminate the pores and segregations, and, by further annealing this, recrystallization will occur, and the precision and strength of the structure can be improved to a certain degree.
  • this forged, recrystallized and annealed material is formed into a target shape having a prescribed three-dimensional structure via die forging, and, thereafter, recrystallization annealing and straightening annealing are performed thereto and surface treatment is ultimately performed thereto in order to manufacture the target.
  • portions facing the forging direction will merely be subject to compressive force
  • portions along the forging direction; that is, the sidewall of the three-dimensional structure will be subject to harsh, strong processing.
  • the grain size of the recrystallized grains upon annealing will significantly differ at portions that are strongly subject to plastic deformation and portions that are weakly subject to plastic deformation.
  • crystals become fine grains at portions that are strongly subject to plastic deformation
  • crystals become coarse grains at portions that are weakly subject to plastic deformation.
  • the boundary area of such portions that are strongly and weakly subject to plastic deformation will become a crystal structure in which the fine grains and coarse grains exist at random, or in which the fine grains and coarse grains change in a phased manner.
  • an object of the present invention is to provide a method capable of constantly manufacturing a sputtering target excellent in characteristics by improving and elaborating forging and heat treatment processes to render a crystal size fine and uniform, and a sputtering target excellent in quality obtained by this method.
  • the present invention provides:
  • a sputtering target manufactured by die forging wherein the average crystal grain size D at a portion where an average crystal grain size is the largest and an average grain size d at a portion where an average crystal grain size is the smallest are related as 1.0 ⁇ D/d ⁇ 2.0;
  • a manufacturing method of a sputtering target by die forging comprising the steps of performing hot kneading or cold kneading and straightening annealing to an ingot or billet material; adjusting the crystal grains by performing cold preforming and recrystallization
  • FIG. 1 is an explanatory diagram showing the structure of a target stamp forged into a hat shaped target
  • FIG. 2 is an explanatory diagram showing the structure of a target stamp forged into a shape in which the cross section thereof appears to be a connection of two hat shaped targets;
  • FIG. 3 is a diagram showing the measurement position of the face orientation.
  • the sputtering target of the present invention is manufactured with the following steps. specifically, foremost, a metal material such as copper, titanium, aluminum, nickel, cobalt, tantalum, or the alloys thereof is dissolved and cast to manufacture an ingot or billet. Next, his ingot or billet is subject to hot forging or cold forging and straightening annealing.
  • a metal material such as copper, titanium, aluminum, nickel, cobalt, tantalum, or the alloys thereof is dissolved and cast to manufacture an ingot or billet.
  • his ingot or billet is subject to hot forging or cold forging and straightening annealing.
  • cold preforming is performed.
  • the melting point of the material is Tm
  • this cold performing is controlled to be 0.3 Tm or less, preferably 0.2 Tm or less.
  • the degree of processing will differ depending on the ultimately demanded crystal grain size, it is preferable that the degree of processing is 20% or more. It is particularly preferable to perform processing at a processing ratio of 50 to 90%. Thereby, intense processing strain can be yielded in the material.
  • the reason for performing cold preforming is to introduce a larger processing strain, and to maintain a fixed temperature of the material during the preforming step as much as possible. As a result, the stain to be introduced can be enlarged sufficiently, and be made uniform.
  • the crystal grain size is adjusted by performing recrystallization annealing.
  • the melting point of the material is Tm
  • this recrystallization annealing after the cold preforming is performed at 0.6 Tm or less, preferably 0.4 Tm or less.
  • the average crystal grain size D 0 at a portion where an average crystal grain size is the largest and an average grain size d 0 at a portion where an average crystal grain size is the smallest will be related as 1.0 ⁇ D 0 /d 0 ⁇ 1.5.
  • Cold preforming is an important step in the present invention, and, with this, it is possible to obtain a target having fine and uniform crystals in the final step.
  • this cold preformed material having fine and uniform crystals is subject to die forging.
  • spinning processing is included in the die forging. In other words, spinning processing shall be included in every die forging described in this specification.
  • crystal homogenization annealing or straightening annealing is performed in order to make the average crystal grain size to be within a range of 1 to 500 ⁇ m.
  • the internal strain can be eliminated, and a target having an overall approximately uniform crystal grain size can be obtained.
  • a sputtering target in which the average crystal grain size D at a portion where an average crystal grain size is the largest and an average grain size d at a portion where an average crystal grain size is the smallest will be related as 1.0 ⁇ D/d ⁇ 2.0 can be obtained.
  • a hexagonal sputtering target of titanium in particular, it is possible to obtain a sputtering target wherein, in the erosion face of the target, the total intensity ratio of the (002) face, and the (103) face, (014) face and (015) face within a 30° angle against such (002) face is 30% or more, and the variation is within ⁇ 10% of the average value.
  • This type of face orientation centered around the (002) face is effective in realizing uniform sputtering, and yields evenness in the deposition.
  • a copper (6N) material was dissolved and cast to prepare an ingot. Next, this ingot was subject to hot kneading at 800° C. This hot kneading destroyed the cast structure, as well as dispersed and eliminated pores and segregations, and a forged product having a uniform structure was obtained thereby.
  • preforming was performed at room temperature and a processing ratio of 50%. After performing this preforming step, recrystallization annealing was performed at 300° C. for 2 hours in order to adjust the crystal grains. As a result, it was possible to adjust the average crystal grain size to be a fine and uniform crystal grain size of 85 ⁇ m.
  • the preformed material having this kind of fine and uniform crystals was stamp forged into a hat shaped target. Die forging was performed at 280° C. After die forging, crystal grain homogenization annealing and straightening annealing were performed at 300° C. for 2 hours.
  • FIG. 1 is a cross section of the hat shaped target prepared in the foregoing step.
  • Symbol C in FIG. 1 represents the hat ceiling portion
  • a and E represent the flange portion
  • B and D represent the side portion, and all of these portions are on the target side (side subject to erosion upon sputtering).
  • the crystal grain size has been adjusted to be fine in the prior cold preforming and recrystallization annealing steps.
  • the annealing of the present invention it is possible to avoid significant differences in the crystal grain size in portions strongly subject to strain and portions weakly subject to strain without having to encounter considerable grain growth.
  • Example 2 Similar to Example 1, a copper (6N) material was dissolved and cast to prepare an ingot. Next, this ingot was subject to cold kneading, cold preforming was performed at a processing ratio of 50%, and recrystallization annealing was further performed at 300° C. for 2 hours. This preformed material was similarly stamp forged into a hat shaped target at 400° C.
  • symbol C represents the hat ceiling portion
  • a and E represent the flange portion
  • B and D represent the side portion, and all of these portions are on the target side (side subject to erosion upon sputtering).
  • the average grain size was respectively A: 344 ⁇ m, B: 184 ⁇ m, C: 211 ⁇ m, D: 192 ⁇ m and E: 379 ⁇ m, and coarse on the whole.
  • Example 2 Similar to Example 1, a copper (6N) material was dissolved and cast to prepare an ingot. Next, this ingot was subject to preforming with hot forging at 750° C. As with Example 1, this preformed material was stamp forged into a hat shaped target at 280° C., and, after such die forging, crystal grain homogenization annealing and straightening annealing were performed at 300° C. for 2 hours. The average crystal grain size of portions A to E at such time is similarly shown in Table 1. Here, the recrystallization annealing subsequent to the preforming step was not performed.
  • the average grain size was respectively A: 724 ⁇ m, B: 235 ⁇ m, C: 257 ⁇ m, D: 244 ⁇ m and E: 773 ⁇ m, and even more coarse on the whole.
  • D average crystal grain size
  • E average grain size
  • Example 2 Similar to Example 1, a copper (6N) material was dissolved and cast to prepare an ingot. Next, this ingot was subject to preforming with hot forging at 750° C. This preformed material was similarly stamp forged into a hat shaped target at 650° C., and, after such die forging, crystal grain homogenization annealing and straightening annealing were performed at 700° C. for 2 hours. The average crystal grain size of portions A to E at such time is similarly shown in Table 1. Here, the recrystallization annealing subsequent to the preforming step was not performed.
  • symbol C represents the hat ceiling portion
  • a and E represent the flange portion
  • B and D represent the side portion, and all of these portions are on the target side (side subject to erosion upon sputtering).
  • the average grain size was respectively A: 2755 ⁇ m, B: 654 ⁇ m, C: 775 ⁇ m, D: 688 ⁇ m and E: 2911 ⁇ m, and abnormally coarse on the whole.
  • Example 2 Similar to Example 1, a copper (6N) material was dissolved and cast to prepare an ingot. Next, this ingot was subject to preforming with hot forging at 400° C. As with Example 1, this preformed material was stamp forged into a hat shaped target at 280° C., and, after such die forging, crystal grain homogenization annealing and straightening annealing were performed at 300° C. for 2 hours. The average crystal grain size of portions A to E at such time is similarly shown in Table 1. Here, the recrystallization annealing subsequent to the preforming step was not performed.
  • symbol C represents the hat ceiling portion
  • a and E represent the flange portion
  • B and D represent the side portion, and all of these portions are on the target side (side subject to erosion upon sputtering).
  • a titanium (4N5) material was dissolved and cast to prepare an ingot. Next, this ingot was subject to cylindrical forging at 650° C. to prepare a billet. Here, the total absolute value of the true strain was 4.
  • the cold preformed material having this kind of fine and uniform crystals was stamp forged into a hat shaped target. Die forging was performed at 450° C. After die forging, crystal grain homogenization annealing and straightening annealing were performed at 500 ° C. for2 hours.
  • FIG. 1 represents the hat ceiling portion
  • a and E represent the flange portion
  • B and D represent the side portion, and all of these portions are on the target side (side subject to erosion upon sputtering).
  • the total intensity ratio of the (002) face in the erosion face of the hat shaped target, and the (103) face, (014) face and (015) face within a 30° angle thereof was sought here, this shall be the (002) face orientation rate.
  • the measured portions are the respective measurement positions depicted in FIG. 3 described later.
  • I(hkl) is the intensity of the diffraction peak of the (hkl) face sought with X-ray diffraction.
  • I*(hkl) is the relative intensity (meaning the intensity when the orientation is entirely random) of the JCPDS (Joint Committee of Diffraction Standard) card. Therefore, I(hkl)/I*(hkl) shows the normalized orientation intensity of the (hkl) face in comparison to the random orientation.
  • ⁇ [I(hkl)/I*(hkl)] is the total normalized intensity ratio. Therefore, the (002) face orientation rate can be calculated with [I(002)/I*(002)+I(103)/I*(103)+I(014)/I*(014)+I(015)/I*(015)]/ ⁇ [I(hkl)/I * (hkl)].
  • results of the total intensity ratio measured respectively at the positions of a, b (as indicated above), c, d, e, f and g of the hat shaped target illustrated in FIG. 3 were as follows: position a: 34.3%, position b (as indicated above): 34.3%, position c: 44.0%, position d: 43.2%, position e: 44.9%, position f: 37.1% and position g: 43.3%.
  • the total intensity ratio of the (002) face, and the (103) face, (014) face and (015) face within a 30° angle against this (002) face at the respective positions was 40 ⁇ 10%, and a favorable target having minimal variations in the orientation and superior evenness was obtained thereby.
  • Example 2 As with Example 2, a cylindrical forged billet was used to perform cold preforming at a processing ratio of 50%. This preformed material was stamp forged into a target at 700° C., and, after die forging, crystal grain homogenization annealing and straightening annealing were performed at 750° C. The average crystal grain size of portions A to E at such time is similarly shown in Table 2.
  • symbol C represents the hat ceiling portion
  • a and E represent the flange portion
  • B and D represent the side portion, and all of these portions are on the target side (side subject to erosion upon sputtering).
  • the average grain size was respectively A: 346 ⁇ m, B: 140 ⁇ m, C: 199 ⁇ m, D: 156 ⁇ m and E: 325 ⁇ m, and coarse on the whole.
  • D average crystal grain size
  • E average grain size
  • Example 2 As with Example 2, a cylindrical forged billet was used to perform hot preforming at 500° C. As with Comparative Example 2, this preformed material was stamp forged into a hat shaped target at 450° C., and, after die forging, crystal grain homogenization annealing and straightening annealing were performed at 500° C. The average crystal grain size of portions A to E at such time is similarly shown in Table 2. Here, the recrystallization annealing subsequent to the preforming step was not performed.
  • symbol C represents the hat ceiling portion
  • a and E represent the flange portion
  • B and D represent the side portion, and all of these portions are on the target side (side subject to erosion upon sputtering).
  • a cylindrical forged billet was used to perform hot preforming at 750° C.
  • This preformed material was stamp forged into a hat shaped target at 450° C., and, after die forging, crystal grain homogenization annealing and straightening annealing were performed at 500° C.
  • the average crystal grain size of portions A to E at such time is similarly shown in Table 2.
  • the recrystallization annealing subsequent to the preforming step was not performed.
  • symbol C represents the hat ceiling portion
  • a and E represent the flange portion
  • B and D represent the side portion, and all of these portions are on the target side (side subject to erosion upon sputtering).
  • the average grain size was respectively A: 156 ⁇ m, B: 56 ⁇ m, C: 87 ⁇ m, D: 61 ⁇ m and E: 177 ⁇ m, and was coarser than Comparative Example 6.
  • a copper (6N) material was dissolved and cast to prepare an ingot. Next, this ingot was subject to hot kneading at 800° C. This hot kneading destroyed the cast structure, as well as dispersed and eliminated pores and segregations, and a forged product having a uniform structure was obtained thereby.
  • the preformed material having this kind of fine and uniform crystals was stamp forged into a target shape in which the cross section thereof appears to be a connection of two hat shaped targets. Die forging was performed at 280° C. After die forging, crystal grain homogenization annealing and straightening annealing were performed at 300° C. for 2 hours.
  • FIG. 2 is a cross section of the target prepared in the foregoing step.
  • Symbol C in FIG. 2 represents the hat ceiling portion
  • A represents the flange portion
  • B and D represent the side portion
  • E represents the hat connection portion
  • all of these portions are on the target side (side subject to erosion upon sputtering).
  • Example 3 Similar to Example 3, a copper (6N) ingot was prepared. This ingot was then subject to preforming via hot forging at 400° C. Similar to Example 4, this preformed material was stamp forged into a target shape in which the cross section thereof appears to be a connection of two hat shaped targets. After die forging, crystal grain homogenization annealing and straightening annealing were performed at 300° C.
  • symbol C represents the hat ceiling portion
  • A represents the flange portion
  • B and D represent the side portion
  • E represents the hat connection portion
  • all of these portions are on the target side (side subject to erosion upon sputtering).
  • a tantalum (5N) material was dissolved and EB cast to prepare an ingot. Next, this ingot was repeatedly subject to kneading at room temperature and straightening annealing at 1200° C., and a billet in which the total absolute value of the true strain is 8 was prepared.
  • the preformed material having this kind of fine and uniform crystals was subject to spinning processing so as to form a target shape in which the cross section thereof appears to be a connection of two hat shaped targets.
  • Spinning processing was performed at room temperature. Thereafter, crystal grain homogenization annealing and straightening annealing were performed at 925° C. for 2 hours.
  • FIG. 1 represents the hat ceiling portion
  • A represents the flange portion
  • B and D represent the side portion
  • E represents the hat connection portion
  • all of these portions are on the target side (side subject to erosion upon sputtering).
  • the cold rolled, preformed material was subject to spinning processing so as to form a target shape in which the cross section thereof appears to be a connection of two hat shaped targets.
  • Spinning processing was performed at room temperature. Thereafter, crystal grain homogenization annealing and straightening annealing were performed at 925° C. for 2 hours.
  • symbol C represents the hat ceiling portion
  • A represents the flange portion
  • B and D represent the side portion
  • E represents the hat connection portion
  • all of these portions are on the target side (side subject to erosion upon sputtering).
  • the partial enlargement of the crystal grain size could be considered a result of insufficient kneading at the time of knead forging. As a result, the cast primary crystals could not be completely destroyed, and the target was formed into its final shape while retaining the distribution of the primary crystals.
  • the present invention provides a manufacturing method of a sputtering target having a three-dimensional structure by die forging, and is characterized in that an average crystal grain size D at a portion where an average crystal grain size is the largest and an average crystal grain size d at a portion where an average crystal grain size is the smallest are related as 1.0 ⁇ D/d ⁇ 2.0.
  • an average crystal grain size D at a portion where an average crystal grain size is the largest and an average crystal grain size d at a portion where an average crystal grain size is the smallest are related as 1.0 ⁇ D/d ⁇ 2.0.

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US20070108046A1 (en) * 2003-09-12 2007-05-17 Nikko Materials Co., Ltd. Sputtering target and method for finishing surface of such target
US20070131545A1 (en) * 2003-10-15 2007-06-14 Nikko Materials Co., Ltd. Packaging device and packaging method for hollow cathode type sputtering target
US20070209741A1 (en) * 2006-03-07 2007-09-13 Carpenter Craig M Methods of producing deformed metal articles
US20090057139A1 (en) * 2005-03-28 2009-03-05 Nippon Mining & Metals Co., Ltd. Pot-Shaped Copper Sputtering Target and Manufacturing Method Thereof
US20110056828A1 (en) * 2009-01-22 2011-03-10 Tosoh Smd, Inc. Monolithic aluminum alloy target and method of manufacturing
US9382613B2 (en) 2010-03-11 2016-07-05 Kabushiki Kaisha Toshiba Sputtering target, manufacturing method thereof, and manufacturing method of semiconductor element
US11236416B2 (en) 2016-06-07 2022-02-01 Jx Nippon Mining & Metals Corporation Sputtering target and production method therefor

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US7892367B2 (en) * 2003-11-06 2011-02-22 Jx Nippon Mining & Metals Corporation Tantalum sputtering target
US20070251819A1 (en) * 2006-05-01 2007-11-01 Kardokus Janine K Hollow cathode magnetron sputtering targets and methods of forming hollow cathode magnetron sputtering targets
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US8702919B2 (en) 2007-08-13 2014-04-22 Honeywell International Inc. Target designs and related methods for coupled target assemblies, methods of production and uses thereof
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CN102424940A (zh) * 2011-12-20 2012-04-25 宁波江丰电子材料有限公司 高纯钴靶材的制备方法
CN103572225B (zh) * 2012-08-01 2016-05-04 宁波江丰电子材料股份有限公司 钽靶材及钽靶材组件的制造方法
CN103572223B (zh) * 2012-08-01 2016-01-27 宁波江丰电子材料股份有限公司 钽靶材及钽靶材组件的制造方法
CN104419901B (zh) * 2013-08-27 2017-06-30 宁波江丰电子材料股份有限公司 一种钽靶材的制造方法

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CN1578849A (zh) 2005-02-09
KR20040047893A (ko) 2004-06-05
WO2003046250A1 (fr) 2003-06-05
CN1329552C (zh) 2007-08-01
US20100058827A1 (en) 2010-03-11
EP1449935B1 (de) 2009-03-11
JP4110476B2 (ja) 2008-07-02
TW200301166A (en) 2003-07-01
US8029629B2 (en) 2011-10-04
JPWO2003046250A1 (ja) 2005-04-07
EP1449935A1 (de) 2004-08-25
DE60231538D1 (de) 2009-04-23
EP1449935A4 (de) 2005-01-19
KR100572263B1 (ko) 2006-04-24

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