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US20060060268A1 - Method of making high strength bainite article, and article made thereby - Google Patents

Method of making high strength bainite article, and article made thereby Download PDF

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Publication number
US20060060268A1
US20060060268A1 US11/227,354 US22735405A US2006060268A1 US 20060060268 A1 US20060060268 A1 US 20060060268A1 US 22735405 A US22735405 A US 22735405A US 2006060268 A1 US2006060268 A1 US 2006060268A1
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US
United States
Prior art keywords
workpiece
temperature
quenching medium
heat
heating
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Abandoned
Application number
US11/227,354
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English (en)
Inventor
Tad Machrowicz
Brandon Landino
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Noble Advanced Technologies Inc
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to US11/227,354 priority Critical patent/US20060060268A1/en
Priority to KR1020077007958A priority patent/KR20070099539A/ko
Priority to BRPI0515674-2A priority patent/BRPI0515674A/pt
Priority to JP2007532551A priority patent/JP2008519154A/ja
Priority to US11/575,343 priority patent/US20080053579A1/en
Priority to EP05858151A priority patent/EP1797205A2/fr
Priority to PCT/US2005/033336 priority patent/WO2007001374A2/fr
Assigned to PULLMAN INDUSTRIES, INC. reassignment PULLMAN INDUSTRIES, INC. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: LANDINO, BRANDON, MACHROWICZ, TAD
Publication of US20060060268A1 publication Critical patent/US20060060268A1/en
Assigned to COMERICA BANK, AS AGENT reassignment COMERICA BANK, AS AGENT SECURITY AGREEMENT Assignors: NOBLE ADVANCED TECHNOLOGIES, INC., NOBLE COMPONENTS & SYSTEMS, INC., NOBLE INTERNATIONAL, LTD., NOBLE LAND HOLDINGS, INC., NOBLE LOGISTIC SERVICES, INC., NOBLE MANUFACTURING GROUP, INC., NOBLE METAL PROCESSING, INC., NOBLE METAL PROCESSING-KENTUCKY, G.P., NOBLE METAL PROCESSING-OHIO, LLC, NOBLE SWISS HOLDINGS, LLC, NOBLE TUBE TECHNOLOGIES, LLC, PROTOTECH LASER WELDING INC., PULLMAN INDUSTRIES OF INDIANA, INC., PULLMAN INDUSTRIES, INC., PULLMAN INVESTMENTS LLC
Assigned to NOBLE ADVANCED TECHNOLOGIES, INC. reassignment NOBLE ADVANCED TECHNOLOGIES, INC. CHANGE OF NAME (SEE DOCUMENT FOR DETAILS). Assignors: PULLMAN INDUSTRIES, INC.
Abandoned legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/18—Hardening; Quenching with or without subsequent tempering
    • C21D1/19—Hardening; Quenching with or without subsequent tempering by interrupted quenching
    • C21D1/20—Isothermal quenching, e.g. bainitic hardening
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/56—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering characterised by the quenching agents
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D11/00—Process control or regulation for heat treatments
    • C21D11/005—Process control or regulation for heat treatments for cooling
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D2211/00—Microstructure comprising significant phases
    • C21D2211/002—Bainite

Definitions

  • This invention relates generally to the fabrication of articles from ferrous metals. More specifically, the invention relates to the fabrication of articles from ferrous alloys having high concentrations of lower bainite. Most specifically, the invention relates to the fabrication of structural members for motor vehicles, and other articles of manufacture, fabricated from high strength steel having a high concentration of lower bainite.
  • Ultra high strength steel is used to fabricate various components of motor vehicles, building structures, and other articles of fabrication.
  • such articles are fabricated directly from martensite steel or they are fabricated from a low carbon steel which is converted to martensite during the production process.
  • steel products produced thereby have tensile strengths up to and over 200 ksi.
  • martensite structures are compromised in elongation properties (typically 4-6%).
  • Bainite steels, particularly lower bainite steels have very high strength but also have very good elongation properties, typically approaching 15%. The superior elongation properties greatly enhance the utility of such articles and/or simplify their fabrication.
  • bainite steels are advantageous in many applications, the preparation of steels having a significant bainite phase, and in particular a lower bainite phase, is difficult.
  • the steel alloys In order to form the bainite phase, the steel alloys must be first heated to a temperature above their austenizing temperature then quenched to a particular holding temperature which is above the temperature at which the martensite phase forms, and they must be held at this temperature for relatively long periods of time so that the bainite phase may form.
  • Lower bainite is formed when the steel is held at a temperature close to, but above, the temperature at which martensite forms.
  • the holding step requires both the combination of fairly high temperatures and very good temperature control. As a consequence, this step is typically carried out in relatively large volumes of high temperature fluids such as molten salts or heated oils. These high temperature baths present significant hazards, consume relatively large amounts of energy, and occupy relatively large areas.
  • the present invention provides a process whereby bainite and in particular lower bainite containing articles may be fabricated in a process having a highly simplified holding step which eliminates the use of high temperature baths and the like, but still promotes the formation of the bainite phase. Accordingly, the process of the present invention may be readily adapted to the large volume, high speed fabrication of high strength steel alloys articles such as intrusion beams, frame members, body members and the like for motor vehicles, as well as components of building structures and other articles of manufacture.
  • a method for preparing a body of a ferrous alloy containing a high percentage of a bainite phase In a first step of the method, a workpiece comprised of a ferrous alloy is heated to a temperature above an austenizing temperature of the alloy. Thereafter, the workpiece is contacted with a quenching medium. Heat is input to the workpiece at least during a portion of the time that it is in contact with the quenching medium so that the combination of the input heat and the quenching medium cooperate to maintain the workpiece at a holding temperature which is below 350° C. but above the martensite phase formation temperature of the alloy.
  • the workpiece is maintained at this holding temperature for a period of time sufficient to form a bainite phase therein and thereafter the workpiece is cooled to ambient temperature.
  • the combination of the holding temperature and time are selected so that a lower bainite phase is formed in the workpiece.
  • the thickness of the workpiece is no greater than 5 millimeters, and in some certain instances it is no greater than 3 millimeters.
  • the workpiece can be heated by resistance heating wherein an electrical current is flowed therethrough.
  • the quenching medium may comprise a gas or a liquid, and it may be flowed across, sprayed onto, or flowed through the workpiece, while in other instances, the workpiece may be immersed in a bath of the quenchant fluid.
  • the workpiece may be subjected to a forming operation which either changes or maintains its shape. This forming operation may be implemented either prior to heating above the austenizing temperature, while the workpiece is at the austenizing temperature, while the workpiece is at the hold temperature, or after the process is complete. Also disclosed herein are articles made by the process of the present invention as well as apparatus for carrying out the invention.
  • FIG. 1 is a graph showing one heating profile which may be implemented in accord with the present invention to produce a lower bainite phase in a workpiece;
  • FIG. 2 is a diagram of a temperature control circuit which may be utilized in the practice of the present invention.
  • the present invention is a metallurgical process which greatly simplifies the formation of bainite, and in particular lower bainite, containing articles by decoupling the function of the quench medium from that of the hold medium heretofore employed. As such, the present invention eliminates the need to utilize large, high temperature, liquid baths for holding articles at an elevated temperature during the formation of the bainite phase.
  • the present invention relies upon a combination of input heat and a quench medium to dynamically balance the temperature of a workpiece so as to effectively hold that workpiece at an elevated temperature sufficient to promote the formation of a bainite phase.
  • a workpiece comprised of a ferrous alloy is first heated to a temperature above its austenizing temperature.
  • This heating may be accomplished by any means known in the art. For example, heating may be carried out in a furnace, by an inductive heater or by resistive heating where an electrical current is flowed through an article.
  • a quench medium may comprise a simple fluid such as water or a water-based liquid, an oil or the like, or in some instances it may be a liquefied or vaporized gas.
  • the quench fluid may be in the form of a bath in which the article is immersed, or it may comprise a sprayed volume of fluid.
  • the fluid need not be at a very high temperature since heat will also be input to the workpiece.
  • the quench fluid may comprise a gas including ambient air, an inert gas such as nitrogen, argon or the like, or a reactive gas such as a nitriding or carburizing gas.
  • the input of heat working in combination with the quench medium establishes a dynamic equilibrium which maintains the workpiece at a selected temperature.
  • the workpiece may be very accurately maintained at a holding temperature selected so as to promote the formation of the bainite phase.
  • the balance of heat and cooling is maintained for a period of time sufficient to form this phase, after which the heat input is terminated and the workpiece cooled below a transition temperature so as to preserve the bainite phase.
  • this process is highly controllable.
  • the workpiece is maintained at a holding temperature which is no greater than 350° C. but above the temperature at which the martensite phase begins to form. The precise temperature ranges will depend upon the specific alloys being treated.
  • Heat input during the hold phase may be implemented by various processes known in the art.
  • One particular process which may be advantageously employed in the present invention comprises a resistive heating wherein an electrical current is flowed through the article so as to generate heat.
  • the resistive heating process is economical and simple to implement and control.
  • the article may be initially heated to a temperature above the austenizing temperature by a resistive heating process preferably carried out in the absence of a quench medium and thereafter contacted with a quench medium so as to cool it to the hold temperature.
  • Such heating and holding may be advantageously carried out in a single workstation and can be coordinated with further forming processes carried out before, during or after the hold step.
  • heating processes such as inductive heating, flame heating, radiant energy heating and the like may also be employed in the practice of the present invention.
  • temperature information obtained thereby may be utilized to control the input of heat and/or parameters of the quench medium such as temperature, velocity, pressure and the like as appropriate, so as to allow for accurate temperature control.
  • control may be carried out in a feedback mode or in an indirect mode.
  • FIG. 1 there is shown a time versus temperature profile for one process in accord with the present invention as operable to form a lower bainite phase in a ferrous body.
  • the graph of FIG. 1 plots time along the horizontal axis and temperature along the vertical axis.
  • the workpiece is at ambient temperature, which is understood to be a normal room temperature encountered in the workplace; and in any instance, an ambient temperature is a temperature which is sufficiently low so that significant metallurgical transitions will not occur in the workpiece. Typically, ambient temperatures are below 50° C.
  • the workpiece is heated to a temperature which is above the austenizing temperature of the alloy comprising the workpiece.
  • This temperature will vary dependent upon the particular alloy employed; however, one of ordinary skill in the art could readily determine what this temperature should be.
  • This first stage heating is typically carried out fairly rapidly, although this is not a requirement of the invention. Heating may be in a furnace, in which instance parts may be maintained therein until further processed. In other instances, heating may be carried out on individual parts immediately before processing. Heating can be by flame, induction, resistance heating or any other method available to those of skill in the art.
  • a holding temperature which is typically below 350° C. but above the temperature at which a martensite phase will form in the alloy. The part is cooled from the austenizing temperature to the holding temperature by application of a quenchant fluid thereto.
  • heat is applied thereto in conjunction with the quenchant fluid.
  • This heating may be by any means known in the art; however, because of ease of application and control, resistance heating is one preferred heating method. Induction heating is another.
  • the combination of heat input and quenchant will establish a dynamic equilibrium, as noted above, which maintains the workpiece at the hold temperature.
  • the application of heat may be continuous or it may be intermittent as is necessary.
  • the workpiece is held at the hold temperature for a period of time sufficient to form desirable amounts of the bainite phase; and thereafter, it is cooled to an ambient temperature thereby locking in the bainite phase. Cooling is typically accomplished by the quenchant fluid, and additional heat is not input in most instances.
  • the aforedescribed heating profile may be modified depending upon the specific metallurgy of the alloy being employed and/or in accordance with desired processing parameters. For example, the rate at which the workpiece is heated or cooled may be varied. Likewise, the hold phase, while shown as being a single horizontal line, may be a stepped line or a gradually sloping line. In some instances, temperature spikes may be selectively incorporated into the profile.
  • the present invention allows for very good spatial control of the metallurgical properties of a workpiece.
  • portions of a workpiece may be selectably heated, held and cooled so as to preferentially form a bainite phase in certain portions of a workpiece.
  • physical parameters of a workpiece such as deformability may be optimized for particular applications.
  • FIG. 2 there is shown a schematic depiction of one temperature control circuit which may be implemented in the present invention.
  • the circuit of FIG. 2 operates to maintain a workpiece 10 at a preselected temperature.
  • a temperature sensor 12 is in communication with the workpiece and is operative to produce an output signal indicative of its temperature.
  • the temperature sensor 12 may comprise a thermocouple, a thermometer, a thermistor or some other such contact device. Also, it may comprise a non-contact device such as an optical pyrometer. In any instance, the temperature sensor 12 produces a control signal which is communicated to a quench controller 14 and/or a heater controller 16 .
  • the temperature sensor communicates with both the quench controller and the heater controller; but in some instances, sufficient temperature control can be obtained in the workpiece by controlling only a single one of the controllers.
  • the quench controller 14 controls a quench fluid delivery system 18 which supplies a quench fluid to the workpiece 10 .
  • the heater controller 16 controls a heater 20 which inputs heat to the workpiece.
  • the controllers 14 , 16 can cooperate to heat and cool the workpiece 10 in accord with a preselected profile.
  • One of skill in the art can readily incorporate other embodiments of controller in the system of the present invention.
  • the methods of the present invention are implemented utilizing workpieces which are relatively thin, and in that regard have a thickness of no more than 5 millimeters; and in some particular instances, the thickness of the articles is no more than 3 millimeters. It has been found that very good temperature control, and uniform metallurgical properties can be obtained utilizing articles of this dimension. However, thicker articles may be fabricated by appropriately adjusting the temperature and heat transfer capacity of the quench medium.
  • the method of the present invention is very well adapted to the fabrication of relatively thin sheet metal articles such as bumper beams, intrusion beams, frame members, body panels and the like for motor vehicles. It may also be utilized to fabricate panels, beams, braces and similar components of building structures.
  • the method of the present invention may be implemented in conjunction with other forming processes such as roll forming, stamping, bending, die forming and the like.
  • stations and systems for the formation of the bainite phase may be incorporated directly into various apparatus, particularly in those instances where processes are carried out at elevated temperatures.
  • a bainite formation step may be readily incorporated into hot forming operations such as die forming, heat treating and the like.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Heat Treatment Of Articles (AREA)
  • Heat Treatments In General, Especially Conveying And Cooling (AREA)
  • Control Of Heat Treatment Processes (AREA)
  • Heat Treatment Of Steel (AREA)
US11/227,354 2004-09-17 2005-09-15 Method of making high strength bainite article, and article made thereby Abandoned US20060060268A1 (en)

Priority Applications (7)

Application Number Priority Date Filing Date Title
US11/227,354 US20060060268A1 (en) 2004-09-17 2005-09-15 Method of making high strength bainite article, and article made thereby
EP05858151A EP1797205A2 (fr) 2004-09-17 2005-09-19 Procede de fabrication d'un article ferreux haute resistance et article associe
BRPI0515674-2A BRPI0515674A (pt) 2004-09-17 2005-09-19 método para preparar um corpo de uma liga ferrosa, artigo e aparelho para preparar um corpo de uma liga ferrosa
JP2007532551A JP2008519154A (ja) 2004-09-17 2005-09-19 高強度の鉄物品の製造方法及びこれにより製造された物品
US11/575,343 US20080053579A1 (en) 2004-09-17 2005-09-19 Method of Making High Strength Ferrous Article, and Article Made Thereby
KR1020077007958A KR20070099539A (ko) 2004-09-17 2005-09-19 고강도 철제 물품의 제조 방법 및 그 방법으로 제조된 물품
PCT/US2005/033336 WO2007001374A2 (fr) 2004-09-17 2005-09-19 Procede de fabrication d'un article ferreux haute resistance et article associe

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US61072004P 2004-09-17 2004-09-17
US11/227,354 US20060060268A1 (en) 2004-09-17 2005-09-15 Method of making high strength bainite article, and article made thereby

Related Child Applications (1)

Application Number Title Priority Date Filing Date
US11575343 Continuation 2007-07-31

Publications (1)

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US20060060268A1 true US20060060268A1 (en) 2006-03-23

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US11/227,354 Abandoned US20060060268A1 (en) 2004-09-17 2005-09-15 Method of making high strength bainite article, and article made thereby
US11/575,343 Abandoned US20080053579A1 (en) 2004-09-17 2005-09-19 Method of Making High Strength Ferrous Article, and Article Made Thereby

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US11/575,343 Abandoned US20080053579A1 (en) 2004-09-17 2005-09-19 Method of Making High Strength Ferrous Article, and Article Made Thereby

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US (2) US20060060268A1 (fr)
EP (1) EP1797205A2 (fr)
JP (1) JP2008519154A (fr)
KR (1) KR20070099539A (fr)
BR (1) BRPI0515674A (fr)
WO (1) WO2007001374A2 (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060232038A1 (en) * 2005-04-14 2006-10-19 Benteler Automotive Corporation Vehicle suspension control arm and method
US7302821B1 (en) * 2004-12-27 2007-12-04 Emc Corporation Techniques for manufacturing a product using electric current during plastic deformation of material
US20100288009A1 (en) * 2007-12-13 2010-11-18 Aisin Takaoka Co., Ltd. Hot press forming apparatus and hot press forming method
US9869000B2 (en) 2013-12-10 2018-01-16 Battelle Energy Alliance, Llc Methods of making bainitic steel materials

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5493893B2 (ja) * 2010-01-14 2014-05-14 新日鐵住金株式会社 厚板鋼板の熱間プレス成形方法

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Publication number Priority date Publication date Assignee Title
US4343661A (en) * 1978-11-15 1982-08-10 Caterpillar Tractor Co. Method of making a low temperature bainite steel alloy gear
US4637844A (en) * 1985-07-08 1987-01-20 Tocco, Inc. Method for heat treating ferrous parts
US4715907A (en) * 1985-07-08 1987-12-29 Tocco, Inc. Method for heat treating ferrous parts
US5840136A (en) * 1996-03-05 1998-11-24 Aisin Aw Co., Ltd. Temperature-raising bainite forming process
US6187113B1 (en) * 1998-10-13 2001-02-13 Benteler Ag Steel alloy for manufacturing bumpers for motor vehicles
US20020100522A1 (en) * 2000-12-01 2002-08-01 Benton Rufus C. Method and apparatus for bainite blades
US20020113041A1 (en) * 2001-02-20 2002-08-22 Masashi Ozawa Method for partly reinforcing a workpiece
US20030190493A1 (en) * 2001-10-19 2003-10-09 Shigeki Nomura Method of manufacturing steel sheet having excellent workability and shape accuracy
US20040238080A1 (en) * 2001-08-29 2004-12-02 Sven Vandeputte Ultra high strength steel composition, the process of production of an ultra high strength steel product and the product obtained

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JPS6447812A (en) * 1987-08-18 1989-02-22 Daido Steel Co Ltd Vacuum heat treating furnace
JPH03253512A (ja) * 1990-03-02 1991-11-12 Komatsu Ltd 高温高圧ガス冷却によるオーステンパ処理方法
JP2685965B2 (ja) * 1990-06-18 1997-12-08 本田技研工業株式会社 球状黒鉛鋳鉄素材の熱処理方法
US6908963B2 (en) * 2001-10-09 2005-06-21 Nektar Therapeutics Al, Corporation Thioester polymer derivatives and method of modifying the N-terminus of a polypeptide therewith

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4343661A (en) * 1978-11-15 1982-08-10 Caterpillar Tractor Co. Method of making a low temperature bainite steel alloy gear
US4637844A (en) * 1985-07-08 1987-01-20 Tocco, Inc. Method for heat treating ferrous parts
US4715907A (en) * 1985-07-08 1987-12-29 Tocco, Inc. Method for heat treating ferrous parts
US5840136A (en) * 1996-03-05 1998-11-24 Aisin Aw Co., Ltd. Temperature-raising bainite forming process
US6187113B1 (en) * 1998-10-13 2001-02-13 Benteler Ag Steel alloy for manufacturing bumpers for motor vehicles
US20020100522A1 (en) * 2000-12-01 2002-08-01 Benton Rufus C. Method and apparatus for bainite blades
US20020113041A1 (en) * 2001-02-20 2002-08-22 Masashi Ozawa Method for partly reinforcing a workpiece
US20040238080A1 (en) * 2001-08-29 2004-12-02 Sven Vandeputte Ultra high strength steel composition, the process of production of an ultra high strength steel product and the product obtained
US20030190493A1 (en) * 2001-10-19 2003-10-09 Shigeki Nomura Method of manufacturing steel sheet having excellent workability and shape accuracy

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7302821B1 (en) * 2004-12-27 2007-12-04 Emc Corporation Techniques for manufacturing a product using electric current during plastic deformation of material
US20060232038A1 (en) * 2005-04-14 2006-10-19 Benteler Automotive Corporation Vehicle suspension control arm and method
US7506444B2 (en) * 2005-04-14 2009-03-24 Benteler Automotive Corporation Vehicle suspension control arm and method
US20100288009A1 (en) * 2007-12-13 2010-11-18 Aisin Takaoka Co., Ltd. Hot press forming apparatus and hot press forming method
US9206488B2 (en) * 2007-12-13 2015-12-08 Aisin Takaoka Co., Ltd. Hot press forming apparatus and hot press forming method
US9869000B2 (en) 2013-12-10 2018-01-16 Battelle Energy Alliance, Llc Methods of making bainitic steel materials

Also Published As

Publication number Publication date
BRPI0515674A (pt) 2008-07-29
JP2008519154A (ja) 2008-06-05
WO2007001374A2 (fr) 2007-01-04
US20080053579A1 (en) 2008-03-06
EP1797205A2 (fr) 2007-06-20
WO2007001374A3 (fr) 2008-08-21
KR20070099539A (ko) 2007-10-09

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