EP1612299A1 - Procédé et appareil pour traitement de surface de matériaux de construction - Google Patents

Procédé et appareil pour traitement de surface de matériaux de construction Download PDF

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Publication number
EP1612299A1
EP1612299A1 EP04015424A EP04015424A EP1612299A1 EP 1612299 A1 EP1612299 A1 EP 1612299A1 EP 04015424 A EP04015424 A EP 04015424A EP 04015424 A EP04015424 A EP 04015424A EP 1612299 A1 EP1612299 A1 EP 1612299A1
Authority
EP
European Patent Office
Prior art keywords
voltage
treatment
component
pole
measuring
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.)
Granted
Application number
EP04015424A
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German (de)
English (en)
Other versions
EP1612299B1 (fr
Inventor
Ursus Dr. Krüger
Daniel Körtvelyessy
Ralph Reiche
Jan Dr. Steinbach
Gabriele Winkler
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.)
Siemens AG
Original Assignee
Siemens AG
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
Priority to AT04015424T priority Critical patent/ATE389739T1/de
Application filed by Siemens AG filed Critical Siemens AG
Priority to DE502004006578T priority patent/DE502004006578D1/de
Priority to EP04015424A priority patent/EP1612299B1/fr
Priority to PCT/DE2005/001090 priority patent/WO2006002610A1/fr
Priority to US11/630,137 priority patent/US20080277288A1/en
Priority to EP05770315A priority patent/EP1761660A1/fr
Priority to CNA2005100813633A priority patent/CN1721580A/zh
Priority to US11/170,662 priority patent/US7794581B2/en
Publication of EP1612299A1 publication Critical patent/EP1612299A1/fr
Application granted granted Critical
Publication of EP1612299B1 publication Critical patent/EP1612299B1/fr
Anticipated expiration legal-status Critical
Not-in-force legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F7/00—Constructional parts, or assemblies thereof, of cells for electrolytic removal of material from objects; Servicing or operating
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D21/00—Processes for servicing or operating cells for electrolytic coating
    • C25D21/12—Process control or regulation
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F5/00—Electrolytic stripping of metallic layers or coatings

Definitions

  • the invention relates to a method for the surface treatment of a component according to the preamble of claim 1 and to an apparatus for carrying out a method for the surface treatment of a component.
  • Operationally stressed components such as turbine blades of gas turbines are subjected to an electrolyte treatment, so that the component can then be worked up again.
  • the operationally stressed MCrAlX layers on the component are removed by immersing them in approximately 50 ° -80 ° C warm 20% hydrochloric acid. After a period of time derived from empirical values, the blades are removed from the acid bath, rinsed with water and then blasted abrasive. The process sequence electrolyte bath and blasting is repeated several times until the entire MCrAlX layer is dissolved or dissolved.
  • the repetition of the individual process steps is usually necessary, since the electrolyte only dissolves near-surface aluminum-containing phases of the MCrAlX layer. Deeper areas of the MCrAlX layer can therefore not be resolved in one step. On the surface remains a porous layer matrix, which is subsequently removed mechanically by means of irradiation, for example.
  • the time that the blades remain in the electrolyte does not reflect the actual time required for the individual blade to stop the dissolution process, but is defaults to a certain time.
  • the residence time in the electrolyte is determined based on general experience.
  • each component is subjected to different individual stresses, so that a fixed time specification leads to different or incomplete dissolution of the claimed surface of the component.
  • the components remain in the acid bath without any further progress of the stripping until the end of the predetermined period of time.
  • EP 1 094 134 A1 and US 2003/0062271 A1 disclose processes for the electrochemical removal of layers.
  • US 4,539,087 discloses a method in which the current of an electrolytic process is measured, so that it can be decided on the basis of the current profile, when the process is to be discontinued.
  • the object is achieved by a method for surface treatment of a component according to claim 1.
  • Another object of the invention is to provide a device that allows an individual determination of the minimum treatment time required per individual component.
  • the object is achieved by a device for surface treatment of a component according to claim 27.
  • FIG. 1 shows an exemplary device 1 according to the invention with which the method according to the invention can be carried out.
  • the device 1 consists of a container 3, for example metallic, ceramic or plastic (Teflon polymer, etc.), in which a treatment agent 6, for example an acid 6 or an electrolyte 6 (with coating material) is arranged, for surface treatment such as stripping or coating at least one component 9 is used.
  • a treatment agent 6 for example an acid 6 or an electrolyte 6 (with coating material) is arranged, for surface treatment such as stripping or coating at least one component 9 is used.
  • an acid or an acid mixture is preferably present in the container 3.
  • the electrolyte 6 has the corresponding chemical elements for the coating.
  • a single component 9 is arranged here, for example, whose surface area is to be dissolved. This happens, for example, due to the acid attack on the surface of the component 9 which is subject to operating conditions, for example.
  • both components 9 each form an electrode (ie anode and cathode), wherein as a treatment agent 6, a nitrogen-containing treatment agent 6 should be used.
  • a first electric circuit can be closed by connecting the connecting means 15 to a further electrical pole, ie the electrode 12, which is arranged in the treatment agent 6 or to the container 3, so that a current I between the component 9 and the pole 3 12, which can also be measured.
  • the current flows through the component 9 through the claimed surface of the component 9 and through the treatment agent 6 to the electrode 12 (or to the container 3).
  • a plurality of components 9 for stripping can also be arranged in a container 3, wherein a current curve I (t) can be determined individually for each component 9, so that the components 9 possibly remain in the treatment agent 6 for different lengths of time.
  • FIG. 2 shows an exemplary voltage profile according to the invention.
  • a pulsed treatment voltage 30 with a pulse duration t 30 is applied, which is, for example, correspondingly large Components 9 (38 cm in length) such as gas turbine blades 120, 130 (Fig. 7, 9) generates currents up to 100 A.
  • the pulse duration t 30 can always be the same or change with time t.
  • the amount of treatment voltage may change with time t.
  • a smaller, for example, pulsed measuring voltage 33 (1 mV to 50 mV) is superimposed on the larger treatment voltage 30 (for stripping) in the circuit 18, 15, 9, 6, 12) or the treatment voltage 30 becomes short (ie at least temporarily) by the height the measuring voltage 33 increases.
  • the pulse duration t 33 of the measurement voltage 33 may be smaller, equal to or greater than the pulse duration t 30 of the treatment voltage 30.
  • the measurement voltage 33 may be applied at the beginning, middle or end of the pulsed treatment voltage 33.
  • the smaller measuring voltage 33 produces much smaller currents that are easier to measure.
  • the separation of the signals of treatment voltage 30 and measurement voltage 33 is effected, for example, by an analysis of the current curve by means of mathematical signal separation methods, such as e.g. the Fourier analysis.
  • three electrodes A further electrode 12 'for a second circuit (FIG. 1) with lines 15' and current / voltage source 18 'for a measuring voltage 33 may also be present according to the invention; the lines 15' are then likewise connected to the component 9 and, for example with the electrode 12 '(indicated by dashed lines) and not connected to the electrode 12), with the stresses superimposed on the large surface area.
  • the metrological separation of the current signals for example, by two partially decoupled circuits (15 + 18 + 9 + 6 + 12, 15 '+ 18' + 9 + 6 + 12 or +12 ').
  • a DC measurement voltage 33 (indicated by dashed lines) can be used.
  • FIG. 3 shows a further exemplary voltage curve according to the invention of the method according to the invention.
  • a high pulsed treatment voltage 30 is used for stripping, which generates very high currents.
  • the measuring voltage 33 is also pulsed here, for example, and is applied during the pulse pauses 36 (t 36 ) of the treatment voltage pulses 30 (t 36 > t 33 ). This is done by the synchronization of the voltage pulses 30, 33.
  • FIG. 4 shows further exemplary voltage profiles.
  • the treatment voltage 30 (corresponding to a pulse-like increase) can be increased by the height of the measuring voltage 33, wherein only one circuit is necessary, or the measuring voltage 33 '(indicated by dashed lines) is superimposed on the treatment voltage, for example by a second circuit.
  • a smaller DC measurement voltage 33 can be used, in particular in a second circuit 18 ', 15', 9, 6, 12 or 12 '.
  • a time profile of the current I (t) caused by the measuring voltage during the electrolysis for stripping is shown in FIG.
  • the current I (t) increases at the beginning with the time t and is initially substantially constant after a certain time.
  • the stripping has not yet been completed, ie the stripping rate is still high.
  • the current I decreases.
  • the decrease (range or point 27 in the curve I (t)) of the current I indicates that only a small amount of layer material is dissolved.
  • the dissolution process can therefore be stopped if, for example, a predetermined comparison value for the current intensity is reached or the current intensity decreases by a certain value (see difference measuring points 27, 22) or a trend line results in a decreasing profile for the current intensity.
  • the method can also be carried out in substeps.
  • an abrasive stripping is carried out, which removes residues of acid products and / or accelerates stripping, since after a certain period of residence of the component 9 in the treatment agent 6, for example, a brittle layer has formed which is better abrasive can be removed.
  • a washing (rinsing) of the component 9 can be carried out in a process intermediate step. Thereafter, the component 9 is again placed in the treatment agent 6.
  • the process steps treatment of the component 9 in the treatment agent 6, abrasive irradiation can be repeated as desired.
  • the delamination of the component or components 9 also runs without the presence of a treatment voltage, ie there is then no electrolytic stripping process.
  • FIG. 6 shows an experimentally mediated progression of the measured or used currents and voltages.
  • a constant treatment voltage 30 of 1.2V being used as the electrolyte, for example, 5% HCl (hydrochloric acid) with 2% triethanolamine.
  • the treatment voltage 30 is represented by the rhombus and generates a current I of 10 to 11 A (not shown).
  • the pulsed measuring voltage 33 for determining the end point here is for example 50 mV and is applied by pulses with a pulse length of, for example, 0.5 s.
  • the ratio measuring voltage 33 to the treatment voltage 30 is therefore 1:24 and is, for example, 1:10 (or 1:20, 1:30 or more than 1:50, 1: 100).
  • the measuring voltage 33 is represented by squares in FIG.
  • the current I which is measured on the basis of the measuring voltage 33, is represented by the triangles in FIG.
  • a dividing line (indicated by dashed lines) shows the intrapolated and expected time course of the current. This curve corresponds to that in FIG. 2.
  • the time course 24 of the current I (t) can also be determined from individual measuring points 21, which are determined at regular or irregular intervals.
  • FIG. 7 shows a perspective view of a blade 120, 130 which extends along a longitudinal axis 121.
  • the blade as an example of the component 9 may be a blade 120 or guide blade 130 of a turbomachine.
  • the turbomachine may be a gas turbine of an aircraft or a power plant for power generation, a steam turbine or a compressor.
  • the blade 120, 130 has along the longitudinal axis 121 consecutively a fastening region 400, a blade platform 403 adjoining thereto and an airfoil 406.
  • the blade at its blade tip 415 may have another platform (not shown).
  • a blade root 183 is formed, which serves for attachment of the blades 120, 130 to a shaft or a disc (not shown).
  • the blade root 183 is designed, for example, as a hammer head. Other designs as Christmas tree or Schwalbenschwanzfuß are possible.
  • the blade 120, 130 has a leading edge 409 and a trailing edge 412 for a medium flowing past the airfoil 406.
  • the blade 120, 130 can be made by a casting process, also by directional solidification, by a forging process, by a milling process or combinations thereof.
  • directionally solidified microstructures which means both single crystals that have no grain boundaries or at most small angle grain boundaries, and stem crystal structures that have probably longitudinal grain boundaries but no transverse grain boundaries. These second-mentioned crystalline structures are also known as directionally solidified structures.
  • Refurbishment means that, after use, components 120, 130 may have to be freed from protective layers by the method according to the invention (for example by sandblasting). This is followed by removal of the corrosion and / or oxidation layers or products. Optionally, even cracks in the component 120, 130 are repaired. Thereafter, a re-coating of the component 120, 130 takes place, for example, by the method according to the invention and a renewed use of the component 120, 130.
  • the blade 120, 130 may be hollow or solid. When the blade 120, 130 is to be cooled, it is hollow and may still have film cooling holes (not shown). As protection against corrosion, the blade 120, 130, for example, corresponding mostly metallic coatings and as protection against heat usually still a ceramic coating.
  • FIG. 8 shows a combustion chamber 110 of a gas turbine.
  • the combustion chamber 110 is configured, for example, as a so-called annular combustion chamber, in which a plurality of burners 102 arranged around the turbine shaft 103 in the circumferential direction open into a common combustion chamber space.
  • the combustion chamber 110 is configured in its entirety as an annular structure, which is positioned around the turbine shaft 103 around.
  • the combustion chamber 110 is designed for a comparatively high temperature of the working medium M of about 1000 ° C to 1600 ° C.
  • the combustion chamber wall 153 is provided on its side facing the working medium M with an inner lining formed of heat shield elements 155 (further example for component 9).
  • Each heat shield element 155 is equipped on the working medium side with a particularly heat-resistant protective layer or made of high-temperature-resistant material. Due to the high temperatures in the interior of the combustion chamber 110, a cooling system is additionally provided for the heat shield elements 155 or for their holding elements.
  • the materials of the combustion chamber wall and its coatings may be similar to the turbine blades.
  • FIG. 9 shows by way of example a gas turbine 100 in a longitudinal partial section.
  • the gas turbine 100 has inside a rotatably mounted about a rotation axis 102 rotor 103, which is also referred to as a turbine runner.
  • a compressor 105 for example, a toroidal combustion chamber 110, in particular annular combustion chamber 106, with a plurality of coaxially arranged burners 107, a turbine 108, and the exhaust case 109.
  • the annular combustion chamber 106 communicates with an annular annular hot gas channel 111, for example.
  • Each turbine stage 112 is formed, for example, from two blade rings.
  • a series 125 formed of rotor blades 120 follows.
  • the guide vanes 130 are fastened to an inner housing 138 of a stator 143, whereas the moving blades 120 of a row 125 are attached to the rotor 103 by means of a turbine disk 133, for example. Coupled to the rotor 103 is a generator or work machine (not shown).
  • air 105 is sucked in and compressed by the compressor 105 through the intake housing 104.
  • the compressed air provided at the turbine-side end of the compressor 105 is supplied to the burners 107 where it is mixed with a fuel.
  • the mixture is then burned to form the working fluid 113 in the combustion chamber 110.
  • the working medium 113 flows along the hot gas channel 111 past the guide vanes 130 and the rotor blades 120.
  • the working medium 113 expands in a pulse-transmitting manner, so that the rotor blades 120 drive the rotor 103 and drive the machine coupled to it.
  • the components exposed to the hot working medium 113 are subject to thermal loads during operation of the gas turbine 100.
  • the guide vanes 130 and blades 120 of the first turbine stage 112 seen in the flow direction of the working medium 113 are in addition to the Ring combustion chamber 106 lining heat shield bricks most thermally stressed. To withstand the prevailing temperatures, they can be cooled by means of a coolant.
  • substrates of the components can have a directional structure, ie they are monocrystalline (SX structure) or have only longitudinal grains (DS structure).
  • SX structure monocrystalline
  • DS structure only longitudinal grains
  • iron-, nickel- or cobalt-based superalloys are used as the material for the components, in particular for the turbine blade 120, 130 and components of the combustion chamber 110. Such superalloys are known, for example, from EP 1204776, EP 1306454, EP 1319729, WO 99/67435 or WO 00/44949; these writings are part of the revelation.
  • blades 120, 130 may be anti-corrosion coatings (MCrA1X; M is at least one element of the group iron (Fe), cobalt (Co), nickel (Ni), X is an active element and is yttrium (Y) and / or silicon and / or at least one element of the rare earths) and heat through a thermal barrier coating.
  • the thermal barrier coating consists for example of ZrO 2 , Y 2 O 4 -ZrO 2 , ie it is not, partially or completely stabilized by yttrium oxide and / or calcium oxide and / or magnesium oxide.
  • suitable coating processes such as electron beam evaporation (EB-PVD), stalk-shaped grains are produced in the thermal barrier coating.
  • EB-PVD electron beam evaporation
  • the vane 130 has a guide vane foot (not shown here) facing the inner housing 138 of the turbine 108 and a vane head opposite the vane foot.
  • the vane head faces the rotor 103 and fixed to a mounting ring 140 of the stator 143.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Automation & Control Theory (AREA)
  • Turbine Rotor Nozzle Sealing (AREA)
  • Electrical Discharge Machining, Electrochemical Machining, And Combined Machining (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
EP04015424A 2004-06-30 2004-06-30 Procédé et appareil pour traitement de surface de matériaux de construction Not-in-force EP1612299B1 (fr)

Priority Applications (8)

Application Number Priority Date Filing Date Title
DE502004006578T DE502004006578D1 (de) 2004-06-30 2004-06-30 Verfahren und Vorrichtung zur Oberflächenbehandlung eines Bauteils
EP04015424A EP1612299B1 (fr) 2004-06-30 2004-06-30 Procédé et appareil pour traitement de surface de matériaux de construction
AT04015424T ATE389739T1 (de) 2004-06-30 2004-06-30 Verfahren und vorrichtung zur oberflächenbehandlung eines bauteils
US11/630,137 US20080277288A1 (en) 2004-06-30 2005-06-13 Method For Removing A Coating From A Component
PCT/DE2005/001090 WO2006002610A1 (fr) 2004-06-30 2005-06-13 Procede pour enlever un revetement applique sur une piece
EP05770315A EP1761660A1 (fr) 2004-06-30 2005-06-13 Procede pour enlever un revetement applique sur une piece
CNA2005100813633A CN1721580A (zh) 2004-06-30 2005-06-28 用于处理构件表面的方法和设备
US11/170,662 US7794581B2 (en) 2004-06-30 2005-06-29 Process for the surface treatment of a component, and apparatus for the surface treatment of a component

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP04015424A EP1612299B1 (fr) 2004-06-30 2004-06-30 Procédé et appareil pour traitement de surface de matériaux de construction

Publications (2)

Publication Number Publication Date
EP1612299A1 true EP1612299A1 (fr) 2006-01-04
EP1612299B1 EP1612299B1 (fr) 2008-03-19

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EP04015424A Not-in-force EP1612299B1 (fr) 2004-06-30 2004-06-30 Procédé et appareil pour traitement de surface de matériaux de construction

Country Status (5)

Country Link
US (1) US7794581B2 (fr)
EP (1) EP1612299B1 (fr)
CN (1) CN1721580A (fr)
AT (1) ATE389739T1 (fr)
DE (1) DE502004006578D1 (fr)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1473387A1 (fr) * 2003-05-02 2004-11-03 Siemens Aktiengesellschaft Procédé de décapage d'une couche d'une pièce
DE102010046372A1 (de) * 2010-09-24 2012-03-29 Oerlikon Trading Ag, Trübbach Verfahren zum Entschichten von Werkstücken
CN103088398B (zh) * 2011-10-31 2016-05-11 通用电气公司 多通道电化学去金属涂层系统及其控制电路
US9163322B2 (en) * 2013-07-01 2015-10-20 General Electric Company Method and apparatus for refurbishing turbine components
CN104593830A (zh) * 2013-11-01 2015-05-06 无锡华臻新能源科技有限公司 带测量反馈的电化学增材制造方法及装置
CN105033372B (zh) * 2015-09-01 2017-09-01 太原科技大学 回转类刀具电解钝化装置
CN111715605B (zh) * 2019-03-22 2022-02-08 潍坊华光光电子有限公司 一种光学镀膜夹具的清洗装置及清洗方法

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US4539087A (en) * 1982-10-29 1985-09-03 Latszereszeti Eszkozok Gyara Method for electrolytic removal of galvanic nickel, chromium or gold layers from the surface of a copper or copper alloy base and apparatus for carrying out the method
US4713153A (en) * 1985-07-12 1987-12-15 N. V. Bekaert S. A. Process and apparatus for cleaning by electrochemical pickling with alternating current of specified frequency
EP1094134A1 (fr) * 1999-10-18 2001-04-25 General Electric Company Système et procédé électrochimique pour l'enlèvement de revêtements métalliques
DE10259365A1 (de) * 2002-04-08 2003-10-30 Siemens Ag Vorrichtung und Verfahren zur Entfernung von Oberflächenbereichen eines Bauteils
EP1473387A1 (fr) * 2003-05-02 2004-11-03 Siemens Aktiengesellschaft Procédé de décapage d'une couche d'une pièce

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EP0861927A1 (fr) 1997-02-24 1998-09-02 Sulzer Innotec Ag Procédé de fabrication de structures monocristallines
EP0892090B1 (fr) 1997-02-24 2008-04-23 Sulzer Innotec Ag Procédé de fabrication de structure monocristallines
EP1306454B1 (fr) 2001-10-24 2004-10-06 Siemens Aktiengesellschaft Revêtement protecteur contenant du rhénium pour la protection d'un élément contre l'oxydation et la corrosion aux températures élevées
WO1999067435A1 (fr) 1998-06-23 1999-12-29 Siemens Aktiengesellschaft Alliage a solidification directionnelle a resistance transversale a la rupture amelioree
US6231692B1 (en) 1999-01-28 2001-05-15 Howmet Research Corporation Nickel base superalloy with improved machinability and method of making thereof
WO2001009403A1 (fr) 1999-07-29 2001-02-08 Siemens Aktiengesellschaft Piece resistant a des temperatures elevees et son procede de production
JP4513145B2 (ja) * 1999-09-07 2010-07-28 ソニー株式会社 半導体装置の製造方法および研磨方法
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US6599416B2 (en) 2001-09-28 2003-07-29 General Electric Company Method and apparatus for selectively removing coatings from substrates
JP3807295B2 (ja) * 2001-11-30 2006-08-09 ソニー株式会社 研磨方法
EP1319729B1 (fr) 2001-12-13 2007-04-11 Siemens Aktiengesellschaft Pièce résistante à des températures élevées réalisé en superalliage polycristallin ou monocristallin à base de nickel
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Patent Citations (5)

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Publication number Priority date Publication date Assignee Title
US4539087A (en) * 1982-10-29 1985-09-03 Latszereszeti Eszkozok Gyara Method for electrolytic removal of galvanic nickel, chromium or gold layers from the surface of a copper or copper alloy base and apparatus for carrying out the method
US4713153A (en) * 1985-07-12 1987-12-15 N. V. Bekaert S. A. Process and apparatus for cleaning by electrochemical pickling with alternating current of specified frequency
EP1094134A1 (fr) * 1999-10-18 2001-04-25 General Electric Company Système et procédé électrochimique pour l'enlèvement de revêtements métalliques
DE10259365A1 (de) * 2002-04-08 2003-10-30 Siemens Ag Vorrichtung und Verfahren zur Entfernung von Oberflächenbereichen eines Bauteils
EP1473387A1 (fr) * 2003-05-02 2004-11-03 Siemens Aktiengesellschaft Procédé de décapage d'une couche d'une pièce

Also Published As

Publication number Publication date
US7794581B2 (en) 2010-09-14
CN1721580A (zh) 2006-01-18
DE502004006578D1 (de) 2008-04-30
US20060084190A1 (en) 2006-04-20
EP1612299B1 (fr) 2008-03-19
ATE389739T1 (de) 2008-04-15

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