WO2005005945A1 - Verfahren und vorrichtung zum messen abkühlkurve von schmelzen - Google Patents

Verfahren und vorrichtung zum messen abkühlkurve von schmelzen Download PDF

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Publication number
WO2005005945A1
WO2005005945A1 PCT/EP2004/006830 EP2004006830W WO2005005945A1 WO 2005005945 A1 WO2005005945 A1 WO 2005005945A1 EP 2004006830 W EP2004006830 W EP 2004006830W WO 2005005945 A1 WO2005005945 A1 WO 2005005945A1
Authority
WO
WIPO (PCT)
Prior art keywords
optical fiber
melt
receiving space
sample
sample receiving
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.)
Ceased
Application number
PCT/EP2004/006830
Other languages
German (de)
English (en)
French (fr)
Inventor
Francis Dams
Jacques Plessers
Paul Clement Verstreken
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.)
Heraeus Electro Nite International NV
Original Assignee
Heraeus Electro Nite International NV
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 BRPI0412366A priority Critical patent/BRPI0412366B1/pt
Priority to JP2006518031A priority patent/JP4755089B2/ja
Priority to UAA200601220A priority patent/UA81824C2/uk
Priority to EP04763023A priority patent/EP1642101B1/de
Priority to AU2004256175A priority patent/AU2004256175B2/en
Priority to CA2522360A priority patent/CA2522360C/en
Application filed by Heraeus Electro Nite International NV filed Critical Heraeus Electro Nite International NV
Priority to DE502004007155T priority patent/DE502004007155D1/de
Publication of WO2005005945A1 publication Critical patent/WO2005005945A1/de
Priority to US11/326,764 priority patent/US7384192B2/en
Anticipated expiration legal-status Critical
Priority to US11/862,479 priority patent/US7635220B2/en
Ceased legal-status Critical Current

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
    • G01K13/00—Thermometers specially adapted for specific purposes
    • G01K13/12—Thermometers specially adapted for specific purposes combined with sampling devices for measuring temperatures of samples of materials
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J5/00—Radiation pyrometry, e.g. infrared or optical thermometry
    • G01J5/0037—Radiation pyrometry, e.g. infrared or optical thermometry for sensing the heat emitted by liquids
    • G01J5/004—Radiation pyrometry, e.g. infrared or optical thermometry for sensing the heat emitted by liquids by molten metals
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J5/00—Radiation pyrometry, e.g. infrared or optical thermometry
    • G01J5/0044—Furnaces, ovens, kilns
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J5/00—Radiation pyrometry, e.g. infrared or optical thermometry
    • G01J5/02—Constructional details
    • G01J5/0205—Mechanical elements; Supports for optical elements
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J5/00—Radiation pyrometry, e.g. infrared or optical thermometry
    • G01J5/02—Constructional details
    • G01J5/04—Casings
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J5/00—Radiation pyrometry, e.g. infrared or optical thermometry
    • G01J5/02—Constructional details
    • G01J5/04—Casings
    • G01J5/041—Mountings in enclosures or in a particular environment
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J5/00—Radiation pyrometry, e.g. infrared or optical thermometry
    • G01J5/02—Constructional details
    • G01J5/06—Arrangements for eliminating effects of disturbing radiation; Arrangements for compensating changes in sensitivity
    • G01J5/068—Arrangements for eliminating effects of disturbing radiation; Arrangements for compensating changes in sensitivity by controlling parameters other than temperature
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J5/00—Radiation pyrometry, e.g. infrared or optical thermometry
    • G01J5/02—Constructional details
    • G01J5/08—Optical arrangements
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J5/00—Radiation pyrometry, e.g. infrared or optical thermometry
    • G01J5/02—Constructional details
    • G01J5/08—Optical arrangements
    • G01J5/0818—Waveguides
    • G01J5/0821—Optical fibres
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
    • G01K13/00—Thermometers specially adapted for specific purposes
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
    • G01K13/00—Thermometers specially adapted for specific purposes
    • G01K13/12—Thermometers specially adapted for specific purposes combined with sampling devices for measuring temperatures of samples of materials
    • G01K13/125—Thermometers specially adapted for specific purposes combined with sampling devices for measuring temperatures of samples of materials for siderurgical purposes

Definitions

  • the invention relates to a method for measuring the cooling curve of melts and / or the heating curve of melt samples with an optical fiber, an immersion end of the optical fiber, which at least partially has a free surface, being surrounded by a temperature-resistant sample-receiving space so that the optical fiber is immersed immersed in the melt and a sample being formed in the sample receiving space, the sample receiving space with the sample and the optical fiber being then pulled out of the metal melt and the cooling curve of the sample and / or, after the sample had solidified beforehand, the temperature profile during heating using a measured by the optical fiber and transmitted to a measuring device. Furthermore, the invention relates to a corresponding device and its use. Melting is understood to mean the melting of pure metals such as iron, copper or steel or alloys as well as cryolite clay melts, salt salts or glass melts.
  • Temperature measurement methods and devices in which liquid temperatures are measured with the aid of optical fibers are known, inter alia, from EP 646 778 B1. Further devices are known from US 4,355,907.
  • an immersion sensor is described with which a sample is taken from a molten metal. The sample adheres to a cavity. A graphite disc is arranged between the cavity and the optical fiber receiving the measured values.
  • a sample vessel in which molten metal is poured and in which the temperature of the molten metal is then measured by means of an optical fiber is known from DE 36 31 645 A1.
  • Other devices for measuring the temperature in molten metals are known from JP 62-185129 and JP 62-185130.
  • Methods for measuring the melting temperature in a crucible using optical radiation are also known from US 6,106,150, US 6,004,031 or from EP 802401 A1.
  • the object of the present invention is to improve the known methods and devices.
  • both the end face and part of the side wall of the immersion end of the optical fiber have a free surface or are brought into direct contact with the melt, the measurement accuracy and the response time can be improved.
  • Advantageous embodiments result from the subclaims.
  • the length of the part of the side wall of the optical fiber that is in direct contact with the melt is at least 10 times, preferably at least SO times as large as the diameter of the free surface of the end face of the optical fiber that is used in the measurement in direct Is brought into contact with the melt.
  • a negative pressure is preferably generated in the sample receiving space and melt is sucked into the sample receiving space, since this considerably improves the sampling as such. It is also possible to bring the sample into the sample receiving space by means of ferrostatic pressure. Furthermore, it is expedient that after the measurement of the cooling curve, the optical fiber is immersed again in the melt and an excess pressure is generated in the sample receiving space and liquid melt is pressed out of the sample receiving space. The pressing out can of course also take place after the heating curve has been measured. It can also be expedient that after the measurement of the cooling curve and / or heating curve, the immersion end of the fiber and the end of the sample receiving space filled with melt are cut off in order to remove any damaged or used material.
  • the bath temperature of the melt can also be measured.
  • the immersion end of the optical fiber can be vibrated at least temporarily to prevent hypothermia of the sample.
  • the method can preferably be used to measure the liquidus temperature and / or a phase transition temperature of the melt. It is advantageous that the end face of the optical fiber has a free surface in order to improve the signal reception.
  • the optical fiber can be formed in particular from sapphire or from quartz glass in order to be stable in particular in higher temperature ranges.
  • the sample receiving space is expediently designed as a tube, in particular made of quartz glass or of metal or ceramic.
  • a slag cap can be arranged at the immersion end of the sample receiving space in order to prevent material lying on the melt to be analyzed from reaching the sample receiving space.
  • the slag cap is usually made of a material that melts or dissolves as it passes through the layer on top of the melt or in the melt.
  • the sample receiving space is preferably pneumatically connected to a device for generating positive or negative pressure in order to be able to set the necessary pressure and, if necessary, to regulate it precisely.
  • the optical fiber is connected to a vibrator.
  • the vibrator can, for example, be arranged on the carrier for the fiber and, by transmitting a vibration to the fiber and to the sample receiving space, has the effect of preventing the melt to be analyzed from undercooling. For this reason, it is also expedient to ensure that the vibrator is coupled to the sample receiving space.
  • the device according to the invention can be used both for measuring the bath temperature of the melt and for measuring the liquidus temperature and / or a phase transition temperature of the melt.
  • FIG. 1 shows a measuring device with a support tube
  • Figure 2 shows another embodiment of the measuring device.
  • the embodiment shown in FIG. 1 has a replaceable carrier tube 1 through which the optical fiber 2 is guided.
  • the carrier tube 1 can be replaced in the molten metal 3 after consumption. For this purpose, it is removed from the connecting pipe 4 of the housing 5 and a new carrier pipe 1 is plugged onto the connecting pipe 4 with a tight connection 6.
  • a system of transport rollers 7 is arranged in the housing 5, with the aid of which the optical fiber 2 is unwound from a coil 8 and fed to the molten metal 3.
  • the immersion end of the fiber 3 has a free surface both on the end face and on the part of the side wall adjoining it.
  • the remaining part of the fiber can have a coating, for example made of plastic, which can be removed, for example, by burning.
  • the other end of the optical fiber is connected to a measuring device 9, which is used for signal recording and evaluation.
  • the housing 5 also contains a gas connection stub 10 to which the overpressure / underpressure unit 11 is connected.
  • the embodiment shown in FIG. 2 has a cable box 12 as its core.
  • the optical fiber 2 is wound on a roll 13.
  • the optical fiber 2 is surrounded by a cladding tube 14 which is unwound together with the fiber 2 and is fed to the molten metal 3 by means of transport rollers 7.
  • the end of the optical fiber 2 facing away from the molten metal 3 is connected to the measuring device 9.
  • the cable box 12 is hermetically sealed and has a gas connection stub 10.
  • the overpressure / underpressure unit 11 is connected to this gas connection stub 10.
  • the optical fiber 2 has at its end facing the molten metal 3 a free surface, both on the front side and on the side wall, the length of the free surface of the optical fiber 2, measured from the front side in the longitudinal direction, being more than 50 times as large is like the diameter of the end face of the optical fiber 2 intended for immersion in the molten metal 3.
  • the optical fiber 2 with its Immersed immersed in the melt 3. In this case, a negative pressure is generated in the carrier tube 1 or the cladding tube 14 and a portion 15 of the melt is sucked into the tube. This lower part of the carrier tube 1 or the cladding tube 14 forms the sample receiving space.
  • the device with the sample receiving space and the sample located therein (part 15 of the metal melt 3 sucked into the sample receiving space) is pulled out of the metal melt 3. Outside the molten metal 3, the temperature is significantly lower than in the molten metal 3, so that the sample is cooled and the cooling curve is recorded on the basis of the radiation signal picked up by the optical fiber 2 and passed on to the measuring device 9.
  • the well-known effect of a black radiator is used.
  • the sample can be heated / melted after solidification / cooling, for example by immersing the sample receiving space of the sampler in the melt.
  • the heating curve is also recorded and evaluated as a temperature-time diagram.
  • the cooling curve / heating curve provides information about the liquidus temperature and / or the solidus temperature, since at this temperature a temperature plateau is recorded for a short time in a temperature-time diagram. Phase changes within the cooling metal melt can also be recognized by temperature plateaus in the temperature-time diagram. As long as the immersion end of the optical fiber 2 is in the molten metal 3 itself, its current bath temperature can be measured.
  • the optical fiber 2 After measuring the cooling curve, the optical fiber 2 can be immersed again in the molten metal 3. The sample melts in the process. After melting, the heating curve can be determined. An overpressure is then generated in the measuring device, in particular within the carrier tube 1 or the cladding tube 14, via the gas connecting piece 10, so that the liquid melt sample is pressed out of the sample receiving space. The device can then be used for a new sampling.
  • the carrier tube 1 may have to be replaced and the optical fiber 2 may have to be fed into the new carrier tube 1.
  • the immersion end of the cladding tube 14 with the optical fiber 2 and any melt residues contained in the cladding tube 14 are cut off as soon as this immersion end has become unusable is.
  • the optical fiber 2 is then unwound from the coil 13 together with the cladding tube 14.
  • the optical fiber is connected to a vibrator, not shown in the drawing.
  • the vibrator can, for example, be arranged on the carrier 1 for the fiber 2 and, by transmitting a vibration to the fiber 2 and to the sample receiving space, has the effect of preventing the melt to be analyzed from undercooling. For this reason, the rigid coupling of the vibrator to the sample receiving space is also expedient.

Landscapes

  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Investigating Or Analyzing Materials Using Thermal Means (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)
  • Radiation Pyrometers (AREA)
  • Investigating And Analyzing Materials By Characteristic Methods (AREA)
  • Sampling And Sample Adjustment (AREA)
PCT/EP2004/006830 2003-07-09 2004-06-24 Verfahren und vorrichtung zum messen abkühlkurve von schmelzen Ceased WO2005005945A1 (de)

Priority Applications (9)

Application Number Priority Date Filing Date Title
JP2006518031A JP4755089B2 (ja) 2003-07-09 2004-06-24 溶融した塊の冷却曲線を測定するための方法及び装置
UAA200601220A UA81824C2 (uk) 2003-07-09 2004-06-24 Спосіб і пристрій для вимірювання кривої охолодження розплавів
EP04763023A EP1642101B1 (de) 2003-07-09 2004-06-24 Verfahren und vorrichtung zum messen abkühlkurve von schmelz en
AU2004256175A AU2004256175B2 (en) 2003-07-09 2004-06-24 Method and device for measuring a melt cooling curve
CA2522360A CA2522360C (en) 2003-07-09 2004-06-24 Method and device for measuring the cooling curve of molten masses
BRPI0412366A BRPI0412366B1 (pt) 2003-07-09 2004-06-24 processo e dispositivo para a medição da curva de resfriamento de massas fundidas
DE502004007155T DE502004007155D1 (de) 2003-07-09 2004-06-24 Verfahren und vorrichtung zum messen abkühlkurve von schmelz en
US11/326,764 US7384192B2 (en) 2003-07-09 2006-01-06 Method for measuring cooling/heating curves of molten masses
US11/862,479 US7635220B2 (en) 2003-07-09 2007-09-27 Device for measuring cooling/heating curves of molten masses

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10331124.6 2003-07-09
DE10331124A DE10331124B3 (de) 2003-07-09 2003-07-09 Verfahren und Vorrichtung zum Messen der Abkühlkurve von Schmelzenproben und/oder der Aufheizkurve von Schmelzenproben sowie deren Verwendung

Related Child Applications (2)

Application Number Title Priority Date Filing Date
US11/326,764 Continuation US7384192B2 (en) 2003-07-09 2006-01-06 Method for measuring cooling/heating curves of molten masses
US11/862,479 Continuation US7635220B2 (en) 2003-07-09 2007-09-27 Device for measuring cooling/heating curves of molten masses

Publications (1)

Publication Number Publication Date
WO2005005945A1 true WO2005005945A1 (de) 2005-01-20

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2004/006830 Ceased WO2005005945A1 (de) 2003-07-09 2004-06-24 Verfahren und vorrichtung zum messen abkühlkurve von schmelzen

Country Status (14)

Country Link
US (2) US7384192B2 (https=)
EP (1) EP1642101B1 (https=)
JP (1) JP4755089B2 (https=)
KR (1) KR101044301B1 (https=)
CN (1) CN100427909C (https=)
AT (1) ATE395581T1 (https=)
AU (1) AU2004256175B2 (https=)
BR (1) BRPI0412366B1 (https=)
CA (1) CA2522360C (https=)
DE (2) DE10331124B3 (https=)
ES (1) ES2303949T3 (https=)
RU (1) RU2336504C2 (https=)
UA (1) UA81824C2 (https=)
WO (1) WO2005005945A1 (https=)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2492655A1 (de) * 2011-02-23 2012-08-29 Heraeus Electro-Nite International N.V. Messgerät zur Messung von Parametern in Schmelzen
CN105388179A (zh) * 2015-12-15 2016-03-09 冶金自动化研究设计院 一种炉前钢种液固相线温度快速检测装置及方法
DE102017004222A1 (de) * 2017-05-03 2018-11-08 Vdeh-Betriebsforschungsinstitut Gmbh Bestimmung der Zusammensetzung einer Metallschmelze

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DE102005061675B3 (de) * 2005-12-21 2007-07-26 Betriebsforschungsinstitut VDEh - Institut für angewandte Forschung GmbH Konverter mit einem Behälter zur Aufnahme geschmolzenen Metalls und einer Messvorrichtung zur optischen Temperaturbestimmung des geschmolzenen Metalls
GB2438214A (en) * 2006-05-19 2007-11-21 Heraeus Electro Nite Int Measuring a parameter of a molten bath
DE102006047765B3 (de) * 2006-10-06 2007-12-20 Heraeus Electro-Nite International N.V. Eintauchlanze für die Analyse von Schmelzen und Flüssigkeiten
US20090110026A1 (en) * 2007-10-24 2009-04-30 Heraeus Electro-Nite Co. Expendable immersion device
CN101907587A (zh) * 2009-06-05 2010-12-08 贺利氏电子耐特国际股份公司 插入式探针
DE102010020715A1 (de) 2010-05-17 2011-11-17 Heraeus Electro-Nite International N.V. Sensoranordnung zur Temperaturmessung sowie Verfahren zum Messen
DE102011012175A1 (de) 2011-02-23 2012-08-23 Heraeus Electro-Nite International N.V. Sensoranordnung zur Messung von Parametern in Schmelzen
DE102012201501B4 (de) 2012-02-02 2015-11-12 Ignatios Giannelis Vorrichtung zur Bestimmung der Temperatur einer Schmelze
EP2799824B1 (en) * 2013-04-30 2019-10-23 Heraeus Electro-Nite International N.V. Method and apparatus for measuring the temperature of a molten metal
KR101450651B1 (ko) * 2013-11-27 2014-10-15 우진 일렉트로나이트(주) 연속 측온 장치 및 이를 포함하는 ｒｈ장치
EP2940441B1 (en) * 2014-04-30 2020-01-01 Heraeus Electro-Nite International N.V. Device for measuring the temperature of a molten metal
CN104048780B (zh) * 2014-06-06 2016-12-07 上海大学 测量脉冲电流液面扰动凝固细晶工艺中熔体热历史曲线的装置
DE102014012698B8 (de) * 2014-09-01 2016-07-14 Minkon GmbH Messvorrichtung zur optischen Temperaturbestimmung eines geschmolzenen Metalls
EP3051264B1 (en) * 2015-01-28 2017-11-15 Heraeus Electro-Nite International N.V. Immersion device for an optical fiber for measuring the temperature of a melt
EP3051263A1 (en) * 2015-01-28 2016-08-03 Heraeus Electro-Nite International N.V. Immersion device for an optical fiber for measuring the temperature of a melt
RU2651931C2 (ru) * 2016-06-08 2018-04-24 Общество с ограниченной ответственностью "Объединенная Компания РУСАЛ Инженерно-технологический центр" Способ и устройство для определения состава электролита
EP3290881B1 (en) * 2016-09-01 2019-08-07 Heraeus Electro-Nite International N.V. Method for feeding an optical cored wire and immersion system to carry out the method
EP3929548A1 (en) * 2020-06-22 2021-12-29 Heraeus Electro-Nite International N.V. Device and method for measuring a temperature of a molten metal
CN111999341B (zh) * 2020-08-19 2023-04-07 之江实验室 一种基于微纳光纤的柔性热导检测装置和方法
DE102021109431A1 (de) 2021-04-15 2022-10-20 Vaillant Gmbh Sensor für einen Verbrennungsraum und Verfahren zu seinem Einbau
PL4141396T3 (pl) * 2021-08-26 2024-12-16 Heraeus Electro-Nite International N.V. Urządzenie pomiarowe i sposób pomiaru temperatury kąpieli stopionego metalu za pomocą urządzenia optycznego
CN116559221A (zh) * 2023-04-11 2023-08-08 承德天大钒业有限责任公司 一种炉外测量中间合金锭冷却曲线的装置及方法

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RU2006103787A (ru) 2006-06-27
EP1642101B1 (de) 2008-05-14
ATE395581T1 (de) 2008-05-15
DE10331124B3 (de) 2005-02-17
AU2004256175B2 (en) 2007-06-28
DE502004007155D1 (de) 2008-06-26
CA2522360C (en) 2014-06-17
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US7384192B2 (en) 2008-06-10
AU2004256175A1 (en) 2005-01-20
CN1820189A (zh) 2006-08-16
JP4755089B2 (ja) 2011-08-24
RU2336504C2 (ru) 2008-10-20
ES2303949T3 (es) 2008-09-01
UA81824C2 (uk) 2008-02-11
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BRPI0412366B1 (pt) 2017-02-07
CN100427909C (zh) 2008-10-22
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KR20060026014A (ko) 2006-03-22
CA2522360A1 (en) 2005-01-20

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