USRE39893E1 - Cemented carbide insert - Google Patents

Cemented carbide insert Download PDF

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Publication number
USRE39893E1
USRE39893E1 US11/449,014 US44901406A USRE39893E US RE39893 E1 USRE39893 E1 US RE39893E1 US 44901406 A US44901406 A US 44901406A US RE39893 E USRE39893 E US RE39893E
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United States
Prior art keywords
coated
coated body
ratio
content
cemented carbide
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Expired - Lifetime
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US11/449,014
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English (en)
Inventor
Anders Lenander
Mikael Lindholm
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Sandvik Intellectual Property AB
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Sandvik Intellectual Property AB
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Publication date
Priority claimed from US09/545,448 external-priority patent/US6344264B1/en
Application filed by Sandvik Intellectual Property AB filed Critical Sandvik Intellectual Property AB
Priority to US11/449,014 priority Critical patent/USRE39893E1/en
Application granted granted Critical
Publication of USRE39893E1 publication Critical patent/USRE39893E1/en
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Expired - Lifetime 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
    • C23C30/00—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process
    • C23C30/005—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process on hard metal substrates
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
    • C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
    • C22C29/08—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds based on tungsten carbide
    • 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
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/247—Removing material: carving, cleaning, grinding, hobbing, honing, lapping, polishing, milling, shaving, skiving, turning the surface
    • 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
    • B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B22F2005/001—Cutting tools, earth boring or grinding tool other than table ware
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
    • Y10T428/24802—Discontinuous or differential coating, impregnation or bond [e.g., artwork, printing, retouched photograph, etc.]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
    • Y10T428/24942—Structurally defined web or sheet [e.g., overall dimension, etc.] including components having same physical characteristic in differing degree
    • Y10T428/2495—Thickness [relative or absolute]
    • Y10T428/24967—Absolute thicknesses specified
    • Y10T428/24975—No layer or component greater than 5 mils thick
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
    • Y10T428/252—Glass or ceramic [i.e., fired or glazed clay, cement, etc.] [porcelain, quartz, etc.]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
    • Y10T428/263—Coating layer not in excess of 5 mils thick or equivalent
    • Y10T428/264—Up to 3 mils
    • Y10T428/265—1 mil or less

Definitions

  • the present invention relates to a coated cemented carbide cutting tool insert particularly useful for turning operations in steels or stainless steels, and is especially suited for operations with high demands regarding toughness properties of the insert.
  • High performance cutting tools must nowadays possess high wear resistance, high toughness properties and good resistance to plastic deformation. Improved toughness behaviour of a cutting insert can be obtained by increasing the WC grain size and/or by raising the overall binder phase content, but such changes will simultaneously result in significant loss of the plastic deformation resistance.
  • a first aspect of the present invention provides a cutting tool insert for machining steel comprising a cemented carbide body comprising WC, 5-12 wt. % Co, 3-11 wt. % of cubic carbides of the metals Ta and Ti, and less than 0.1 wt. % of Nb where the ratio of Ta/Ti is 1.0-4.0, and the Co-binder phase is highly alloyed with W, having a CW-ratio of 0.75-0.95, the body also comprising a binder phase enriched and essentially gamma phase free surface zone with a thickness of 5-50 ⁇ m; and a coating.
  • a second aspect of the present invention provides a method of making a coated cemented carbide body having a gamma phase-free and binder rich surface zone comprising the steps of:
  • FIG. 1 is a plot showing the level of Co enrichment near the surface of an insert formed according to the present invention.
  • a coated cemented carbide insert with a 5-50 ⁇ thick, preferably 10-30 ⁇ m thick, essentially gamma phase free and binder phase-enriched surface zone with an average binder phase content (by volume) preferably in the range 1.2-2.0 times the bulk binder phase content.
  • the gamma phase consists essentially of TaC and TiC and of any WC that dissolves into the gamma phase during sintering.
  • the ratio Ta/Ti is between 1.0 and 4.0, preferably 2.0-3.0.
  • the binder phase is highly W-alloyed.
  • the CW-ratio takes a value less than or equal to 1. The lower the CW-ratio, the higher the W-content in the binder phase. It has now-been found according to the invention that an improved cutting performance is achieved if the CW-ratio is in the range 0.75-0.95, preferably 0.80-0.85.
  • the present invention is applicable to cemented carbides with a composition of 5-12, preferably 9-11, weight percent of Co binder phase, and 3-11, preferably 7-10, weight percent TaC+TiC, and the balance being WC.
  • the Nb content should not exceed 0.1 weight percent.
  • the weight ratio Ta/Ti should be 1.0-4.0, preferably 2.0-3.0.
  • the WC preferably has an average grain size of 1.0 to 4.0 ⁇ m, more preferably 1.5 to 3.0 ⁇ m.
  • the cemented carbide body may contain less than 1 volume % of ⁇ -phase (M 6 C).
  • Inserts according to the invention are further provided with a coating preferably comprising 3-12 ⁇ m columnar TiCN-layer followed by a 1-8 ⁇ m thick Al 2 O 3 -layer deposited, for example, according to any of the patents U.S. Pat. No. 5,766,782, U.S. Pat. No. 5,654,035, U.S. Pat. No. 5,974,564, U.S. Pat. No. 5,702,808, preferably a ⁇ -Al 2 O 3 -layer and preferably with an outermost thin layer of TiN which preferably is removed in the edge line by brushing or by blasting.
  • the property of the coated insert can be optimised to suit specific cutting conditions.
  • a cemented carbide insert produced according to the invention is provided with a coating of: 6 ⁇ m TiCN, 5 ⁇ m Al 2 O 3 and 1 ⁇ m TiN. This coated insert is particularly suited for cutting operation in steel.
  • a cemented carbide insert produced according to the invention is provided with a coating of: 4 ⁇ m TiN, 2 ⁇ m Al 2 O 3 and 1 ⁇ m TiN. This coating is particularly suited for cutting operations in stainless steels.
  • the invention also relates to a method of making cutting inserts comprising a cemented carbide substrate of a binder phase of Co, WC, a gamma phase of Ta and Ti, a binder phase enriched surface zone essentially free of gamma phase, and a coating.
  • a powder mixture containing 5-12, preferably 9-11, weight percent of binder phase consisting of Co, and 3-11, preferably 7-10, weight percent TaC+TiC, and the balance WC with an average grain size of 1.0-4.0 ⁇ m, more preferably 1.5-3.0 ⁇ m, is prepared.
  • the Nb content should not exceed 0.1 weight percent.
  • the weight ratio Ta/Ti should be 1.0-4.0, preferably 2.0-3.0.
  • the raw materials are mixed with pressing agent and, optionally W, such that the desired CW-ratio is obtained.
  • the mixture is milled and spray dried to obtain a powder material with the desired properties.
  • the powder material is compacted and sintered. Sintering is performed at a temperature of 1300-1500° C., in a controlled atmosphere of about 50 mbar followed by cooling. After conventional post sintering treatments, including edge rounding, a hard, wear resistant coating according to above is deposited by CVD- or MT-CVD-technique.
  • Cemented carbide turning inserts of the style CNMG 120408-PM and SNMG120412-PR with the composition 9.9 wt % Co, 6.0 wt % TaC, 2.5 wt % TiC, and 0.3 wt % TiN, with the balance WC having an average grain size of 2.0 ⁇ m were produced according to the invention.
  • the nitrogen was added to the carbide powder as TiCN. Sintering was done at 1450° C. in a atmosphere of Ar at a total pressure of about 50 mbar.
  • FIG. 1 shows a plot of the Co enrichment near the surface measured by an image analysis technique.
  • the Co is enriched to a peak level of 1.3 times the bulk content.
  • Magnetic saturation values were recorded and used for calculating CW-values.
  • An average CW-value of 0.81 was obtained.
  • the inserts were coated in a CVD-process comprising a first thin layer (less than 1 ⁇ m) of TiN followed by 6 ⁇ m thick layer of TICN with columnar grains by using MTCVD-techniques (process temperature 850° C. and CH 3 CN as the carbon/nitrogen source).
  • MTCVD-techniques process temperature 850° C. and CH 3 CN as the carbon/nitrogen source.
  • a 5 ⁇ m thick ⁇ -Al 2 O 3 layer was deposited according to U.S. Pat. No. 5,974,564.
  • a 1.0 ⁇ m TiN layer was deposited.
  • the coated inserts were brushed in order to smoothly remove the TiN coating from the edge line.
  • Cemented carbide turning inserts of the style CNMG 120408-PM and SNMG120412-PR with the composition 10.0 wt % Co, 2.9 wt % TaC, 3.4 wt % TiC, 0.5 wt % NbC and 0.2 wt % TiN and the balance WC with an average grain size of 2.1 ⁇ m were produced.
  • the inserts were sintered in the same process as A.
  • Metallographic investigation showed that the produced inserts had a gamma phase free zone of 15 ⁇ m. Magnetic saturation values were recorded and used for calculating CW-values. An average CW-value of 0.81 was obtained.
  • the inserts were subject to the same pre-coating treatment as A, coated in the same coating process and also brushed in the saute way as A.
  • Cemented carbide turning inserts of the style CNGM 120408-PM and SNMG120412-PR with the composition 10.0 wt % Co, 3.0 wt % TaC, 6.3 wt % ZrC and balance WC with an average grain size of 2.5 ⁇ m were produced.
  • Inserts from A, B and C were tested with respect to toughness in a longitudinal turning operation with interrupted cuts.
  • Cutting data Cutting speed 130 m/min Depth of cut 1.5 mm
  • Feed Starting with 0.15 mm and gradually increased by 0.10 mm/min until breakage of the edge
  • the plastic deformation was measured as the edge depression at the nose of the inserts.
  • Examples 2, 3 and 4 show that the inserts A according to the invention surprisingly exhibit much better toughness in combination with somewhat better plastic deformation resistance in comparison to conventional inserts B and C.

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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)
  • Cutting Tools, Boring Holders, And Turrets (AREA)
  • Powder Metallurgy (AREA)
  • Chemical Vapour Deposition (AREA)
  • Carbon And Carbon Compounds (AREA)
US11/449,014 1999-04-08 2006-06-08 Cemented carbide insert Expired - Lifetime USRE39893E1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US11/449,014 USRE39893E1 (en) 1999-04-08 2006-06-08 Cemented carbide insert

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
SE9901243A SE519828C2 (sv) 1999-04-08 1999-04-08 Skär av en hårdmetallkropp med en bindefasanrikad ytzon och en beläggning och sätt att framställa denna
US09/545,448 US6344264B1 (en) 1999-04-08 2000-04-07 Cemented carbide insert
US11/449,014 USRE39893E1 (en) 1999-04-08 2006-06-08 Cemented carbide insert

Related Parent Applications (1)

Application Number Title Priority Date Filing Date
US09/545,448 Reissue US6344264B1 (en) 1999-04-08 2000-04-07 Cemented carbide insert

Publications (1)

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USRE39893E1 true USRE39893E1 (en) 2007-10-23

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US11/449,014 Expired - Lifetime USRE39893E1 (en) 1999-04-08 2006-06-08 Cemented carbide insert

Country Status (6)

Country Link
US (1) USRE39893E1 (de)
EP (1) EP1043416B1 (de)
JP (1) JP2000334608A (de)
AT (1) ATE276379T1 (de)
DE (1) DE60013675T2 (de)
SE (1) SE519828C2 (de)

Families Citing this family (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SE520253C2 (sv) 2000-12-19 2003-06-17 Sandvik Ab Belagt hårdmetallskär
SE0103970L (sv) 2001-11-27 2003-05-28 Seco Tools Ab Hårdmetall med bindefasanrikad ytzon
SE526604C2 (sv) * 2002-03-22 2005-10-18 Seco Tools Ab Belagt skärverktyg för svarvning i stål
SE526603C3 (sv) * 2003-01-24 2005-11-16 Sandvik Intellectual Property Belagt hårdmetallskär
SE527348C2 (sv) 2003-10-23 2006-02-14 Sandvik Intellectual Property Sätt att tillverka en hårdmetall
EP1609883B1 (de) * 2004-06-24 2017-09-20 Sandvik Intellectual Property AB Beschichtetes Schneidwerkzeug
SE528108C2 (sv) * 2004-07-13 2006-09-05 Sandvik Intellectual Property Belagt hårdmetallskär, speciellt för svarvning av stål, samt sätt att tillverka detsamma
SE529302C2 (sv) * 2005-04-20 2007-06-26 Sandvik Intellectual Property Sätt att tillverka en belagd submikron hårdmetall med bindefasanriktad ytzon
AT502703B1 (de) * 2005-10-28 2008-06-15 Boehlerit Gmbh & Co Kg Hartmetall für schneidplatten von kurbelwellenfräsern
SE531670C2 (sv) 2007-02-01 2009-06-30 Seco Tools Ab Texturerat alfa-aluminiumoxidbelagt skär för metallbearbetning
AT12293U1 (de) * 2009-10-05 2012-03-15 Ceratizit Austria Gmbh Schneidwerkzeug zur bearbeitung metallischer werkstoffe
DE102016107958A1 (de) * 2016-04-28 2017-11-02 Herrmann Ultraschalltechnik Gmbh & Co. Kg Stanz-Siegeleinheit und Ultraschallbearbeitungsvorrichtung mit einer solchen
EP3763840B1 (de) * 2019-07-10 2022-04-20 Sandvik Mining and Construction Tools AB Gradientenhartmetallkörper und verfahren zur herstellung davon

Citations (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4277283A (en) 1977-12-23 1981-07-07 Sumitomo Electric Industries, Ltd. Sintered hard metal and the method for producing the same
US4497874A (en) 1983-04-28 1985-02-05 General Electric Company Coated carbide cutting tool insert
US4610931A (en) 1981-03-27 1986-09-09 Kennametal Inc. Preferentially binder enriched cemented carbide bodies and method of manufacture
US4729823A (en) 1986-08-08 1988-03-08 Guevara-Kelley Scientific Products, Inc. Apparatus and methods for electrophoresis
US5484468A (en) 1993-02-05 1996-01-16 Sandvik Ab Cemented carbide with binder phase enriched surface zone and enhanced edge toughness behavior and process for making same
US5549980A (en) 1992-02-21 1996-08-27 Sandvik Ab Cemented carbide with binder phase enriched surface zone
US5649279A (en) 1992-12-18 1997-07-15 Sandvik Ab Cemented carbide with binder phase enriched surface zone
US5654035A (en) 1992-12-18 1997-08-05 Sandvik Ab Method of coating a body with an α-alumina coating
US5674564A (en) 1991-06-25 1997-10-07 Sandvik Ab Alumina-coated sintered body
US5702808A (en) 1994-11-15 1997-12-30 Sandvik Ab Al2 O2 -coated cutting tool preferably for near net shape machining
US5729823A (en) 1995-04-12 1998-03-17 Sandvik Ab Cemented carbide with binder phase enriched surface zone
US5766782A (en) 1994-01-14 1998-06-16 Sandvik Ab Aluminum oxide coated cutting tool and method of manufacturing thereof
US5786069A (en) 1995-09-01 1998-07-28 Sandvik Ab Coated turning insert

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
IL110663A (en) * 1994-08-15 1997-09-30 Iscar Ltd Tungsten-based cemented carbide powder mix and cemented carbide products made therefrom
SE509616C2 (sv) * 1996-07-19 1999-02-15 Sandvik Ab Hårdmetallskär med smal kornstorleksfördelning av WC
SE516017C2 (sv) * 1999-02-05 2001-11-12 Sandvik Ab Hårdmetallskär belagt med slitstark beläggning

Patent Citations (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4277283A (en) 1977-12-23 1981-07-07 Sumitomo Electric Industries, Ltd. Sintered hard metal and the method for producing the same
US4610931A (en) 1981-03-27 1986-09-09 Kennametal Inc. Preferentially binder enriched cemented carbide bodies and method of manufacture
US4497874A (en) 1983-04-28 1985-02-05 General Electric Company Coated carbide cutting tool insert
US4729823A (en) 1986-08-08 1988-03-08 Guevara-Kelley Scientific Products, Inc. Apparatus and methods for electrophoresis
US5674564A (en) 1991-06-25 1997-10-07 Sandvik Ab Alumina-coated sintered body
US5549980A (en) 1992-02-21 1996-08-27 Sandvik Ab Cemented carbide with binder phase enriched surface zone
US5649279A (en) 1992-12-18 1997-07-15 Sandvik Ab Cemented carbide with binder phase enriched surface zone
US5654035A (en) 1992-12-18 1997-08-05 Sandvik Ab Method of coating a body with an α-alumina coating
US5484468A (en) 1993-02-05 1996-01-16 Sandvik Ab Cemented carbide with binder phase enriched surface zone and enhanced edge toughness behavior and process for making same
US5766782A (en) 1994-01-14 1998-06-16 Sandvik Ab Aluminum oxide coated cutting tool and method of manufacturing thereof
US5702808A (en) 1994-11-15 1997-12-30 Sandvik Ab Al2 O2 -coated cutting tool preferably for near net shape machining
US5729823A (en) 1995-04-12 1998-03-17 Sandvik Ab Cemented carbide with binder phase enriched surface zone
US5786069A (en) 1995-09-01 1998-07-28 Sandvik Ab Coated turning insert

Also Published As

Publication number Publication date
SE9901243L (sv) 2000-10-09
SE9901243D0 (sv) 1999-04-08
SE519828C2 (sv) 2003-04-15
JP2000334608A (ja) 2000-12-05
DE60013675D1 (de) 2004-10-21
EP1043416A3 (de) 2002-08-14
EP1043416A2 (de) 2000-10-11
EP1043416B1 (de) 2004-09-15
DE60013675T2 (de) 2005-02-10
ATE276379T1 (de) 2004-10-15

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