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EP1691775A2 - Desorption de l'hydrogene par catalyse dans un materiau de stockage d'hydrogene a base de magnesium et procedes de production correspondants - Google Patents

Desorption de l'hydrogene par catalyse dans un materiau de stockage d'hydrogene a base de magnesium et procedes de production correspondants

Info

Publication number
EP1691775A2
EP1691775A2 EP04812679A EP04812679A EP1691775A2 EP 1691775 A2 EP1691775 A2 EP 1691775A2 EP 04812679 A EP04812679 A EP 04812679A EP 04812679 A EP04812679 A EP 04812679A EP 1691775 A2 EP1691775 A2 EP 1691775A2
Authority
EP
European Patent Office
Prior art keywords
magnesium
hydrogen storage
based hydrogen
storage alloy
desoφtion
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.)
Withdrawn
Application number
EP04812679A
Other languages
German (de)
English (en)
Inventor
Michael A. Fetcenko
Kwo Young
Cheng Tung
Stanford R. Ovshinsky
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.)
Ovonic Hydrogen Systems LLC
Original Assignee
Texaco Ovonic Hydrogen Systems LLC
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 Texaco Ovonic Hydrogen Systems LLC filed Critical Texaco Ovonic Hydrogen Systems LLC
Publication of EP1691775A2 publication Critical patent/EP1691775A2/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/0005—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes
    • C01B3/001—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof
    • C01B3/0026—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof of one single metal or a rare earth metal; Treatment thereof
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/0005—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes
    • C01B3/001—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof
    • C01B3/0031—Intermetallic compounds; Metal alloys; Treatment thereof
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/0005—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes
    • C01B3/001—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof
    • C01B3/0078—Composite solid storage mediums, i.e. coherent or loose mixtures of different solid constituents, chemically or structurally heterogeneous solid masses, coated solids or solids having a chemically modified surface region
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74—Iron group metals
    • B01J23/745—Iron
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/024—Multiple impregnation or coating
    • B01J37/0244—Coatings comprising several layers
    • 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
    • B22F2998/10—Processes characterised by the sequence of their steps
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C2202/00—Physical properties
    • C22C2202/04—Hydrogen absorbing
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/32—Hydrogen storage

Definitions

  • the instant invention relates generally to hydrogen storage materials and more specifically magnesium-based hydrogen storage materials in which hydrogen desorption is catalyzed by materials which are insoluble in said magnesium-based hydrogen storage material.
  • the insoluble catalytic material may be in the form of: 1) discrete dispersed regions of catalytic material in a hydrogen storage material bulk; 2) discrete dispersed regions on the surface of particles of the hydrogen storage material; 3) a continuous or semi-continuous layer of catalytic material on the surface of bulk or particulate hydrogen storage material; or 4) combinations thereof.
  • Hydrogen may be used, for example, as fuel for internal-combustion engines in place of hydrocarbons. In this case it has the advantage of eliminating atmospheric pollution through the formation of oxides of carbon, nitrogen and sulfur upon combustion of the hydrocarbons. Hydrogen may also be used to fuel hydrogen-air fuel cells for production of the electricity needed for electric motors.
  • One of the problems posed by the use of hydrogen is its storage and transportation.
  • Hydrogen may be stored under high pressure in steel cylinders, but this approach has the drawback of requiring hazardous and heavy containers which are difficult to handle (in addition to having a low storage capacity of about 1% by weight). Hydrogen may also be stored in cryogenic containers, but this entails the disadvantages associated with the use of cryogenic liquids; such as, for example, the high cost of the containers, which also require careful handling. There are also "boil off" losses of about 2-5% per day. Another method of storing hydrogen is to store it in the form of a hydride, which then is decomposed at the proper time to furnish hydrogen.
  • the MgH 2 ⁇ Mg system is the most appropriate of all known metal-hydride and metal systems that can be used as reversible hydrogen-storage systems because it has the highest percentage by weight (7.65 % by weight) of theoretical capacity for hydrogen storage and hence the highest theoretical energy density
  • this alloy can be titanium/iron hydride (a typical low-temperature hydride store) which can be operated at temperatures down to below 0 °C.
  • These low-temperature hydride alloys have the disadvantage of having a low hydrogen storage capacity. Storage materials have been developed in the past, which have a relatively high storage capacity but from which hydrogen is nevertheless expelled at temperatures of up to about 250 °C.
  • these alloys also have the disadvantage that the price of the alloy is very high when metallic vanadium is used.
  • U.S. Pat. No. 4,111,689 has disclosed a storage alloy which comprises 31 to 46% by weight of titanium, 5 to 33% by weight of vanadium and 36 to 53% by weight of iron and/or manganese.
  • alloys of this type have a greater storage capacity for hydrogen than the alloy according to U.S. Pat. No. 4,160,014, hereby incorporated by reference, they have the disadvantage that temperatures of at least 250 °C. are necessary in order to completely expel the hydrogen. At temperatures of up to about 100 °C, about 80% of the hydrogen content can be discharged in the best case. However, a high discharge capacity, particularly at low temperatures, is frequently necessary in industry because the heat required for liberating the hydrogen from the hydride stores is often available only at a low temperature level.
  • magnesium is preferred for the storage of hydrogen not only because of its lower material costs, but above all, because of its lower specific weight as a storage material.
  • the hydriding Mg+H 2 ⁇ MgH 2 is, in general, more difficult to achieve with magnesium, inasmuch as the surface of the magnesium will rapidly oxidize in air so as to form stable MgO and/or Mg(OH) 2 surface layers. These layers inhibit the dissociation of hydrogen molecules, as well as the absorption of produced hydrogen atoms and their diffusion from the surface of the granulate particles into the magnesium storage mass.
  • Amo ⁇ hicity is a generic term referring to lack of X-ray diffraction evidence of long- range periodicity and is not a sufficient description of a material.
  • amo ⁇ hous materials there are several important factors to be considered: the type of chemical bonding, the number of bonds generated by the local order, that is its coordination, and the influence of the entire local environment, both chemical and geometrical, upon the resulting varied configurations.
  • Amo ⁇ hicity is not determined by random packing of atoms viewed as hard spheres nor is the amorphous solid merely a host with atoms imbedded at random.
  • Amo ⁇ hous materials should be viewed as being composed of an interactive matrix whose electronic configurations are generated by free energy forces and they can be specifically defined by the chemical nature and coordination of the constituent atoms. Utilizing multi-orbital elements and various preparation techniques, one can outwit the normal relaxations that reflect equilibrium conditions and, due to the three-dimensional freedom of the amo ⁇ hous state, make entirely new types of amo ⁇ hous materials-chemically modified materials . . .
  • amo ⁇ hicity was understood as a means of introducing surface sites in a film, it was possible to produce "disorder" that takes into account the entire spectrum of effects such as porosity, topology, crystallites, characteristics of sites, and distances between sites.
  • Ovshinsky and his team at ECD began constructing "disordered" materials where the desired irregularities were tailor made. See, U.S. Pat. No.4,623,597, the disclosure of which is inco ⁇ orated by reference.
  • disordered corresponds to the meaning of the term as used in the literature, such as the following:
  • a disordered semiconductor can exist in several structural states. This structural factor constitutes a new variable with which the physical properties of the [material] . . . can be controlled.
  • structural disorder opens up the possibility to prepare in a metastable state new compositions and mixtures that far exceed the limits of thermodynamic equilibrium.
  • disordered [materials] . . . it is possible to control the short-range order parameter and thereby achieve drastic changes in the physical properties of these materials, including forcing new coordination numbers for elements . . . S. R.
  • Venkatesan, Fetcenko, Jeffries, Stahl, and Bennet the disclosure of which is inco ⁇ orated by reference. Since all of the constituent elements, as well as many alloys and phases thereof, are present throughout the metal, they are also represented at the surfaces and at cracks which form in the metal/electrolyte interface. Thus, the characteristic surface roughness is descriptive of the interaction of the physical and chemical properties of the host metals as well as of the alloys and crystallographic phases of the alloys, in an alkaline environment. The microscopic chemical, physical, and crystallographic parameters of the individual phases within the hydrogen storage alloy material are important in determining its macroscopic electrochemical characteristics.
  • FIGURES Figure 1 is a scanning electron micrograph (SEM) taken in back-scattering mode of a hydrogen storage material of the instant invention made from pure metal powders pressed and sintered at a temperature above 500° C for 22 hours under vacuum;
  • Figure 2 is an X-ray diffraction pattern of the material of figure 1 ;
  • Figure 3 is a plot of the pressure-concentration-isotherm (PCT) curve for the material of figure 1 measured at 240° C;
  • Figure 4 plots the percent hydrogen abso ⁇ tion versus time (i.e. abso ⁇ tion rates) of the material of figure 1 at various temperatures;
  • Figure 5 plots the percent of hydrogen desorbed versus time (i.e.
  • Figure 6 plots the PCT curves of samples having the same composition as that of figure 1, but sintered/annealed at 570 and 600 °C respectively;
  • Figure 7 is an SEM back-scattering micrograph of another material according to the instant invention having the same composition as the material of figure 1 but formed by mechanical alloying;
  • Figure 8 is the XRD plot of the material of figure 7;
  • Figure 9 is a plot of the PCT curve of the material of figure 7, measured at 240 °C;
  • Figure 10 plots the PCT absorption curves of the material of figure 7 at 240 °C, 210 °C, 180 °C, and 150 °C;
  • Figure 11 is an SEM backscattered photomicrograph of a cross-section of a melt spun ribbon of a very uniform Mg-Al alloy used to produce a material according to the instant invention;
  • Figure 12 shows a PCT plot of a hydrogen storage material according to the instant invention at 150 °C, the material was produced using the
  • the insoluble catalytic material may be in the form of: 1) discrete dispersed regions of catalytic material in a hydrogen storage material bulk; 2) discrete dispersed regions on the surface of particles of the hydrogen storage material; 3) a continuous or semi-continuous layer of catalytic material on the surface of bulk or particulate hydrogen storage material; or 4) combinations thereof.
  • the catalytic material can be added during the alloying process by special rapid quenching methods; or by mechanical alloying methods.
  • the catalytic material can also be applied to the surface of the magnesium-based alloy by processes such as thermal evaporation, magnetic sputtering, or by electrolytic or electroless plating methods. Elements which have almost no solid solubility in Mg may be used as grain grow inhibitors/deso ⁇ tion catalysts.
  • Example 2 Another MM-1 material was produced by the process described in Example 1 with a change in sintering/annealing temperature.
  • Figure 6 plots the PCT curves of samples sintered/annealed at 570 °C and
  • Example 3 The mechanically alloyed (MA) powders of MM- 1 were prepared from mixtures of pure elemental magnesium (99.8%, -325 mesh), aluminum (99.5%, -325 mesh), and iron (99.9+%, 10 micron). The milling was carried out in an attritor loaded with Cr-steel grinding balls.
  • Figure 9 is a plot of the PCT curve measured at 240 ° C for the MA-MM- 1.
  • the pressure plateau is higher than that of the sintered MM-1 due to the varied distance between Mg-storage phase and Fe-catalytic phase and shows a spectrum of varying kinetics.
  • the maximum hydrogen storage capacity was increased from 5.0 to 5.7% and the hydrogen is fully desorbed at 240 °C.
  • Figure 10 plots the PCT abso ⁇ tion curves of the MA-MM-1 sample at 240 °C, 210 °C, 180 °C, and 150 °C.
  • the plateau pressure increases with the temperature. This phenomenon is to be expected from thermo-equilibrium considerations. However, the maximum storage capacity decreases with decreasing in temperature.
  • Example 4 Raw material with the designed composition of MM- 1 was put in an air-operated induction furnace with additional flux to isolate surface from the atmosphere and prevent excessive magnesium evaporation from the metal liquid. Extra argon gas was supplied to the crucible as an isolation blanket to prevent oxidation of the molten metal. After melting all ingredients in the crucible, the melt was tilted pour into a mold and slowly cooled to room temperature. The composition of the resulting ingot was examined by induction coupled plasma (ICP) analysis and no trace of iron was detected. From this comparative example, it can be seen that conventional induction melting techniques cannot inco ⁇ orated iron in the Mg bulk. The Mg- Al Ingot from above was placed in a bottom-poured melt-spinning machine.
  • ICP induction coupled plasma
  • FIG. 11 is an SEM backscattered photomicrograph of the ribbon cross-section which shows a very uniform Mg-Al alloy.
  • the ribbon was then chopped into small pieces and was placed into attritor for the same MA process as described in Example 3.
  • the ground powder was then pressed onto a Ni expanded metal substrate and coated on both faces with 100 angstroms of Fe.
  • the MS+MA-MM- 1 shows very good hydrogen deso ⁇ tion kinetics at relatively low temperatures.
  • Figure 12 shows a PCT plot of this sample measured at 150 ° C.
  • the abso ⁇ tion/deso ⁇ tion pressure hysteresis observed is due to the low measuring temperature. Nevertheless, a deso ⁇ tion plateau at 250 ton- is very exciting.
  • Figure 13 compares the maximum reversible hydrogen storage capacities at various temperatures for the three different processes (i.e. sintering, MA-only, MS + MA).
  • the MS + MA process gives the lowest deso ⁇ tion onset temperature (90° C) but also the lowest maximum reversible capacity due to the non-uniform distribution of the Fe phase.
  • the MA-only sample shows the highest deso ⁇ tion temperature onset (150° C) but with the highest reversible storage capacity.
  • Example 5 Raw materials with the nominal composition of MM-1 were put in an air-operated induction furnace with additional flux to isolate the molten surface from the atmosphere and prevent excessive magnesium evaporation from the liquid metal. Extra argon gas was supplied to the crucible as an isolation blanket to prevent oxidation of the metal. The molten alloy was stirred manually to uniformly suspend immiscible FeAl and Fe phases in the liquid. The liquid was tilt-poured through an argon protected ladle into a water-cooled quenching mold to inco ⁇ orate the Fe and FeAl phases into the final product.
  • Figure 1 Raw materials with the nominal composition of MM-1 were put in an air-operated induction furnace with additional flux to isolate the molten surface from the atmosphere and prevent excessive magnesium evaporation from the liquid metal. Extra argon gas was supplied to the crucible as an isolation blanket to prevent oxidation of the metal. The molten alloy was stirred manually to uniformly suspend immiscible FeAl and Fe phases in the liquid. The liquid was tilt-

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Combustion & Propulsion (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Hydrogen, Water And Hydrids (AREA)
  • Powder Metallurgy (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

La présente invention concerne un matériau de stockage d'hydrogène à base de magnésium comprenant du magnésium ou un alliage de stockage d'hydrogène à base de magnésium et un catalyseur de désorption de l'hydrogène qui est insoluble dans ledit alliage et qui se présente sous la forme: 1) de zones dispersées discrètes de matériau catalytique dans le magnésium ou dans l'alliage de stockage de l'hydrogène à base de magnésium ; 2) de zones dispersées discrètes sur la surface de particules dudit magnésium ou dudit alliage de stockage de l'hydrogène à base de magnésium; 3) d'une couche continue ou semi-continue de matériau catalytique sur la surface du magnésium ou de l'alliage de stockage de l'hydrogène à base de magnésium, lequel se trouve en masse ou sous forme de particules ; 4) ou de combinaisons de ces éléments. Cette invention concerne également des procédés permettant de produire le matériau.
EP04812679A 2003-12-11 2004-12-02 Desorption de l'hydrogene par catalyse dans un materiau de stockage d'hydrogene a base de magnesium et procedes de production correspondants Withdrawn EP1691775A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US10/735,240 US20050126663A1 (en) 2003-12-11 2003-12-11 Catalyzed hydrogen desorption in Mg-based hydrogen storage material and methods for production thereof
PCT/US2004/040227 WO2005060547A2 (fr) 2003-12-11 2004-12-02 Desorption de l'hydrogene par catalyse dans un materiau de stockage d'hydrogene a base de magnesium et procedes de production correspondants

Publications (1)

Publication Number Publication Date
EP1691775A2 true EP1691775A2 (fr) 2006-08-23

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EP04812679A Withdrawn EP1691775A2 (fr) 2003-12-11 2004-12-02 Desorption de l'hydrogene par catalyse dans un materiau de stockage d'hydrogene a base de magnesium et procedes de production correspondants

Country Status (9)

Country Link
US (1) US20050126663A1 (fr)
EP (1) EP1691775A2 (fr)
JP (1) JP2007522917A (fr)
KR (1) KR20060123300A (fr)
CN (1) CN101072889A (fr)
CA (1) CA2548093A1 (fr)
MX (1) MXPA06006678A (fr)
NO (1) NO20063136L (fr)
WO (1) WO2005060547A2 (fr)

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CN114229797B (zh) * 2022-01-17 2024-01-12 重庆大学 一种基于含LPSO第二相的Mg-Ni-Y合金水解制氢的方法
CN114411028B (zh) * 2022-01-21 2022-09-20 徐州工程学院 一种微量镍复合层状镁复合材料及其制备方法和应用
CN115417373B (zh) * 2022-08-02 2023-09-15 华南理工大学 一种非晶/晶态复合镁基储氢材料的制备方法
CN115367700B (zh) * 2022-08-31 2024-04-05 理工清科(重庆)先进材料研究院有限公司 锌铜双金属MOF催化的MgH2储氢材料、其制备方法和应用
CN116426803B (zh) * 2023-03-07 2025-07-08 上海镁源动力科技有限公司 一种用于循环储放氢的镁基合金及其制备方法
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WO2005060547A2 (fr) 2005-07-07
NO20063136L (no) 2006-09-07
MXPA06006678A (es) 2007-02-02
CA2548093A1 (fr) 2005-07-07
CN101072889A (zh) 2007-11-14
US20050126663A1 (en) 2005-06-16
JP2007522917A (ja) 2007-08-16
KR20060123300A (ko) 2006-12-01

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