EP1575726B1 - Soft magnetic powder composition comprising insulated particles and a lubricant selected from organo-silanes, -titanates, -aluminates and zirconates and a process for their preparation - Google Patents

Soft magnetic powder composition comprising insulated particles and a lubricant selected from organo-silanes, -titanates, -aluminates and zirconates and a process for their preparation Download PDF

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Publication number
EP1575726B1
EP1575726B1 EP03781264A EP03781264A EP1575726B1 EP 1575726 B1 EP1575726 B1 EP 1575726B1 EP 03781264 A EP03781264 A EP 03781264A EP 03781264 A EP03781264 A EP 03781264A EP 1575726 B1 EP1575726 B1 EP 1575726B1
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European Patent Office
Prior art keywords
composition according
group
iron
powder
particles
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Expired - Lifetime
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EP03781264A
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German (de)
English (en)
French (fr)
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EP1575726A1 (en
Inventor
Mikhail Kejzelman
Björn SKARMAN
Paul Skoglund
Ola Andersson
Per Knutsson
Hilmar Vidarsson
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Hoganas AB
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Hoganas AB
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147—Alloys characterised by their composition
    • H01F1/14708—Fe-Ni based alloys
    • H01F1/14733—Fe-Ni based alloys in the form of particles
    • H01F1/14741—Fe-Ni based alloys in the form of particles pressed, sintered or bonded together
    • H01F1/1475—Fe-Ni based alloys in the form of particles pressed, sintered or bonded together the particles being insulated
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/105—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing inorganic lubricating or binding agents, e.g. metal salts
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/16—Metallic particles coated with a non-metal
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/20—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder
    • H01F1/22—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together
    • H01F1/24—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated
    • H01F1/26—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated by macromolecular organic substances
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0206—Manufacturing of magnetic cores by mechanical means
    • H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder

Definitions

  • the present invention relates to new metal powder compositions. More specifically, the invention concerns a new iron-based powder which is useful for the preparation of soft magnetic materials having improved properties when used both at high and low frequencies. The invention also concerns a method for the manufacturing of soft magnetic composite materials prepared therefrom.
  • Soft magnetic materials are used for applications, such as core materials in inductors, stators and rotors for electrical machines, actuators, sensors and transformer cores.
  • soft magnetic cores such as rotors and stators in electric machines, are made of stacked steel laminates.
  • Soft Magnetic Composite, SMC materials are based on soft magnetic particles, usually iron-based, with an electrically insulating coating on each particle. By compacting the insulated particles optionally together with lubricants and/or binders using the traditionally powder metallurgy process, the SMC parts are obtained.
  • the magnetic permeability of a material is an indication of its ability to become magnetised or its ability to carry a magnetic flux. Permeability is defined as the ratio of the induced magnetic flux to the magnetising force or field intensity.
  • Desired component properties include e.g. a high permeability through an extended frequency range, low core losses, high saturation induction, and high strength. Normally an increased density of the component enhances all of these properties provided that a sufficient electrical resistivity can be maintained.
  • the desired powder properties include suitability for compression moulding techniques, which i.e. means that the powder can be easily moulded to a high density component, which can be easily ejected from the moulding equipment without damages on the component surface.
  • the present invention concerns a new ferromagnetic powder composition, which is suitable of compaction to high density composite components. More specifically the present invention concerns a powder composition comprising soft magnetic iron or iron-based core particles, the surface of which are surrounded by an electrically insulating inorganic coating and which composition also includes a lubricating amount of silanes, titanates, aluminates, or zirconates as defined in claim 1.
  • the present invention also includes a method of preparing high-density green, and optionally heat-treated, compacts from these compositions.
  • This method comprises the steps of providing the composition, optionally mixing said composition with additives, such as conventional lubricants (i.e. particular lubricants) and binders as well as flow-enhancing agents; uniaxially compacting in a die at high pressure and ejecting the green body, which may subsequently be heat-treated.
  • additives such as conventional lubricants (i.e. particular lubricants) and binders as well as flow-enhancing agents
  • the ferromagnetic powders used herein are made up of iron or an alloy containing iron optionally in combination with up to 20 % by weight of one or more of element selected from the group consisting of aluminium, silicon, chromium, niobium, molybdenum, nickel and cobalt.
  • the new powder is based on a base powder that consists of essentially pure iron.
  • This powder could be e.g. commercially available water-atomised or gas-atomised iron powders or reduced iron powders, such as sponge iron powders.
  • the powder particle shape could be round, irregular or flat.
  • Preferred electrically insulating coatings which may be used according to the invention, are thin phosphorous containing coatings of the type described in the US patent 6348265 . Also other, preferably inorganic coatings may be used, for example coatings based on Cr, Mg, Mo, Zn, Ni, or Co.
  • the lubricating agent used according to the invention is a type of organo-silanes, organo-titanates, organo-aluminates or organo-zirconates.
  • This class of substances is often referred to as surface modifying agents, coupling agents, or cross-linking agents depending on the chemical functionality of their linked groups.
  • the specific type of organo-silanes, organo-titanates, organo-aluminates or organo-zirconates which are used according to the present invention and which may be referred to as organo-metallic compounds are distinguished by the presence of at least one hydrolysable group and at least one lubricating organic moiety.
  • This type of compounds can be defined by the following general formula: M ⁇ R 1 n ⁇ R 2 m ,wherein M is a central atom selected from Si, Ti, Al, and Zr; R 1 is a hydrolysable group; R 2 is a group consisting of a lubricating organic moiety; wherein the sum of m+n must equal the coordination number of the central atom and where n is an integer ⁇ 1 and m is an integer ⁇ 1.
  • R 1 is an alkoxy group having less than 12 C atoms. Preferred are those alkoxy groups, which have less than 6, and most preferred are alkoxy groups having 1-3 C atoms.
  • R 1 may also be a chelate group, such as a residue of hydroxyacetic acid (-OC(O))-CH 2 O-) or a residue of ethylene glycol (-OCH 2 CH 2 O-).
  • R 2 is an organic group including between 6-30, preferably 10-24 carbon atoms optionally including one or more hetero atoms selected from the group consisting of N, O, S and P.
  • R 2 is a group consisting of an organic moiety, which is not easily hydrolysed and often lipophilic and can be a chain of an alkyl, ether, ester, phospho-alkyl, phospho-alkyl, phospho-lipid, or phospho-amine.
  • the phosphorous may be present as phosphato, pyrophosphato, or phosphito groups.
  • R 2 may be linear, branched, cyclic, or aromatic.
  • a preferred group of lubricating silanes according to the present invention are alkyl-alkoxy silanes and polyether-alkoxy silanes. Furthermore, promising results have been obtained with hexadecyl-trimethoxy silane, isopropyl-triisostearyl titanate, isopropyl-tri(dioctyl)phosphato titanate, neopentyl(diallyl)oxy-tri(dioctyl)phosphato zirconate, neopentyl(diallyl)oxy-trineodecanoyl zirconate, and diisobutyl-acetoacetyl aluminate.
  • the amount of the compound is present in amounts of 0.05-0.5%, preferably 0.07-0.45%, and most preferably 0.08-0.4% by weight of the composition.
  • a too low amount of lubricating agent gives high density but results in poor ejection behaviour and may thus result in poor surface condition of the tool and/or SMC parts.
  • a too high amount may give excellent ejection behaviour but could render in low component densities.
  • the compound is present as a lubricating layer on the insulated particles. It should, however, be noted that the geometry of the component as well as the material and quality of the tool, have great impact on the surface condition of the SMC parts after ejection.
  • the US patent 6537389 discloses a wide range of silicon-, aluminium-, or boron-containing compounds as molecular precursors for producing electrically insulating ceramics on soft magnetic powders.
  • the precursor compounds are converted by thermal treatments into ceramic, metallic or intermetallic end products to enhance temperature and solvent resistance.
  • the US patent 6537389 distinguishes from the present invention i.a. in that the organo-metallic compounds are used as precursors for producing chemically and thermally resistant coatings, and not as the key component that facilitates production of high density parts.
  • the precursor compounds described in the examples of US patent 6537389 do not include a lubricating moiety.
  • the lubricating compound(s)used according to the present invention can be used in such a way that it is dissolved or dispersed in a suitable solvent, e.g. an organic solvent, such as acetone or ethanol.
  • a suitable solvent e.g. an organic solvent, such as acetone or ethanol.
  • the obtained solution or dispersion is subsequently added to the iron based powder during mixing and optionally heating.
  • the solvent is finally evaporated optionally in vacuum.
  • the powder used has coarse particles i.e. the powder is essentially without fine particles.
  • the term "essentially without fine particles” is intended to mean that less than about 5 % of the iron or iron-based powder particles have size below 45 ⁇ m as measured by the method described in SS-EN 24 497. So far the most interesting results have been achieved with powders essentially consisting of particles above about 106 ⁇ m and particularly above about 212 ⁇ m.
  • the term "essentially consisting” is intended to mean that at least 40 %, preferably at least 60 % of the particles have a particle size above 106 and 212 ⁇ m, respectively. So far the best results have been obtained with powders having an average particle size about 250 ⁇ m and only less than 3 % below 106 ⁇ m.
  • the maximum particle size may be about 5 mm.
  • the particle size distribution for iron-based powders used at PM manufacturing is normally distributed with a Gaussian distribution with an average particle diameter in the region of 30 to 100 ⁇ m and about 10-30% less than 45 ⁇ m.
  • Iron based powders essentially free from fine particles may be obtained by removing the finer fractions of the powder or by manufacturing a powder having the desired particle size distribution.
  • the iron or iron-based powder must not be mixed with a separate (particular) lubricant before it is transferred to the die.
  • external lubrication die wall lubrication
  • the invention does not exclude the possibility of, when it is of interest, to utilise conventional internal lubrication (in an amount up to 0.5% by weight), external lubrication or a combination of both.
  • soft magnetic composite materials having a density of at least 7.45 g/cm 3 can be prepared by uniaxially compacting the new powder compositions in a die at high compaction pressures and without die wall lubrication.
  • the green body When the green body has been ejected from the compaction tool it can be heat treated up to temperatures of about 700°C.
  • the term "at high compaction pressure” is intended to mean at pressures of about at least 800 MPa. More interesting results are obtained with higher pressures such as pressures above 900, more preferably above 1000, and most preferably above 1100 MPa.
  • Conventional compaction at high pressures, i.e. pressures above about 800 MPa, with conventionally used powders including finer particles are generally considered unsuitable due to the high forces required in order to eject the compacts from the die, the accompanying high wear of the die, and the fact that the surfaces of the components tend to be less shiny or deteriorated. High electrical resistance can be obtained even though high compaction pressures are used to achieve the high density.
  • the powders according to the present invention it has unexpectedly been found that the ejection force is reduced at high pressures of about 1000 MPa, and that components having acceptable or even perfect surfaces may be obtained.
  • the compaction may be performed with standard equipment, which means that the new method may be performed without expensive investments.
  • the compaction is performed uniaxially and preferably in a single step at ambient or elevated temperature.
  • the compaction may be performed with the aid of a percussion machine (Model HYP 35-4 from Hydropulsor) as described in patent publication WO 02/38315 .
  • the heat treatment may be performed at the temperatures normally used, e.g. up to temperatures of about 700°C in different types of atmospheres or at reduced pressure and optionally in the presence of steam. Prior to the heat treatment the pressed components may optionally be green machined and/or cleaned.
  • a main object of the present invention is to achieve high density products and to this end it is preferred to use coarse powders as described above. It has, however, also been found that these lubricating effects can also be obtained in combination with powders including higher amounts of fine particles i.e. the type of powders which are conventionally used in the PM industry today.
  • Example 3 and 5 below illustrates the lubricating effect of the organo-metallic compounds according to the present invention on both conventional powders and coarse powders. As can be observed high densities are obtained also with a conventional powder including higher amounts of fine particles.
  • Compositions including iron or iron-based powders with the particle size distributions which are normally used today and the lubricating agents according to the present invention may be of special interest for certain applications and are therefore also within the scope of the invention.
  • high density is intended to mean compacts having a density of about at least 7.45 g/cm 3 .
  • “High density” is not an absolute value.
  • a typical achievable density according to the state of the art for single heat-treated, single pressed components is about 7.2 g/cm 3 .
  • warm compaction an increase of about 0.2 g/cm 3 may be reached.
  • high density is intended to mean compacts having a density of about 7.45-7.65 g/cm 3 and above, depending on type and amount of additives used, and type of iron-based powder used. Components having lower densities can of course also be produced but are believed to be of less interest.
  • the advantage obtained by using the powder and method according to the present invention is that high-density SMC parts can be cost-efficiently produced. SMC parts with remarkably high magnetic induction levels together with low core losses can be obtained. Other advantages are that the mechanical strength after heat treatment is increased and that, in spite of very high densities, compacted parts with high electrical resistance can be successfully ejected from the dies without negatively influence the finish of the die walls and/or on the surfaces of the compacted SMC parts. It is thus possible to obtain parts having excellent surface finish. These results can be obtained with a single compaction step. Examples of products of special interest for the new powder compacts are inductors, stators and rotors for electrical machines, actuators, sensors and transformer cores.
  • Table 1 Sample Compaction Pressure MPa Density g/cm 3 ⁇ max B 1500 (T) B 6900 (T) Core loss/cycle at 1T and 50 Hz (J/kg) Core loss/cycle at 1T and 400 Hz (J/kg) According to the invention 800 7.45 720 1.08 1.53 0.134 0.178 1000 7.59 790 1.15 1.59 0.126 0.163 1200 7.64 820 1.18 1.62 0.124 0.165 Comparative example 800 7.39 620 0.95 1.46 0.142 0.200 1000 7.47 590 0.95 1.49 0.140 0.198 1200 7.49 550 0.92 1.48 0.140 0.193
  • the green density is significantly higher for the powder according to the invention and magnetic properties are, hence, improved compared with the materials used in the comparative examples.
  • the comparative example also demonstrates that no or only minor improvements of the magnetic properties can be obtained by increasing the compaction pressure to 1000 MPa and 1200 MPa.
  • a very high purity water atomised iron-based powder the particles of which were provided with a thin insulating coating and which had a mean particle size above 212 ⁇ m was treated with 0.1% and 0.2% of hexadecyltrimethoxysilane, respectively, according to the procedure in Example 1.
  • the same iron-based powder without any lubricating agent was used as a reference.
  • Cylindrical samples with a diameter of 25 mm and a height of 4 mm were compacted in an uniaxially press movement at a compaction pressure of 1000 MPa.

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Dispersion Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Electromagnetism (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Soft Magnetic Materials (AREA)
  • Powder Metallurgy (AREA)
  • Lubricants (AREA)
  • Silicon Polymers (AREA)
EP03781264A 2002-12-23 2003-12-22 Soft magnetic powder composition comprising insulated particles and a lubricant selected from organo-silanes, -titanates, -aluminates and zirconates and a process for their preparation Expired - Lifetime EP1575726B1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
SE0203851A SE0203851D0 (sv) 2002-12-23 2002-12-23 Iron-Based Powder
SE0203851 2002-12-23
PCT/SE2003/002067 WO2004056508A1 (en) 2002-12-23 2003-12-22 Soft magnetic powder composition comprising insulated particles and a lubricant selected from organo-silanes, -titanates, -aluminates and zirconates and a process for their preparation

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EP1575726A1 EP1575726A1 (en) 2005-09-21
EP1575726B1 true EP1575726B1 (en) 2010-07-07

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EP03781264A Expired - Lifetime EP1575726B1 (en) 2002-12-23 2003-12-22 Soft magnetic powder composition comprising insulated particles and a lubricant selected from organo-silanes, -titanates, -aluminates and zirconates and a process for their preparation

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EP (1) EP1575726B1 (ja)
JP (2) JP4886987B2 (ja)
KR (1) KR101035757B1 (ja)
CN (1) CN100548541C (ja)
AT (1) ATE473064T1 (ja)
AU (1) AU2003288880B8 (ja)
BR (1) BR0317661A (ja)
CA (1) CA2505381C (ja)
DE (1) DE60333309D1 (ja)
ES (1) ES2348212T3 (ja)
MX (1) MXPA05006847A (ja)
PL (1) PL209529B1 (ja)
RU (1) RU2335817C2 (ja)
SE (1) SE0203851D0 (ja)
TW (1) TWI229018B (ja)
WO (1) WO2004056508A1 (ja)
ZA (1) ZA200503597B (ja)

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SE0203851D0 (sv) * 2002-12-23 2002-12-23 Hoeganaes Ab Iron-Based Powder
CA2679363C (en) * 2007-03-21 2015-06-02 Hoeganaes Ab (Publ) Powder metal polymer composites
JP5697589B2 (ja) * 2008-03-20 2015-04-08 ホガナス アクチボラグ （パブル） 強磁性粉末組成物及びその生産方法
JP5482097B2 (ja) * 2009-10-26 2014-04-23 Ｔｄｋ株式会社 軟磁性材料、並びに、圧粉磁芯及びその製造方法
CN102844824B (zh) * 2010-02-18 2017-08-15 霍加纳斯股份有限公司 铁磁粉末组合物及其制造方法
AT12021U1 (de) * 2010-04-14 2011-09-15 Plansee Se Beschichtungsquelle und verfahren zu deren herstellung
CN101982856B (zh) * 2010-09-21 2012-02-15 李延军 笔杆式汽车点火线圈内用软磁铁芯及其制作方法
CN102136330A (zh) * 2011-04-01 2011-07-27 钢铁研究总院 一种复合软磁材料及其制备方法
EP2509081A1 (en) * 2011-04-07 2012-10-10 Höganäs AB New composition and method
CN102909373A (zh) * 2012-09-15 2013-02-06 安徽省怀远县尚冠模具科技有限公司 一种模具冲压顶杆的制备方法
CN102896315B (zh) * 2012-09-15 2015-04-01 安徽省怀远县尚冠模具科技有限公司 一种模具上压板的制备方法
JP2014196554A (ja) * 2013-03-08 2014-10-16 Ntn株式会社 磁心用粉末および圧粉磁心、並びに磁心用粉末および圧粉磁心の製造方法
CN104217834B (zh) * 2013-06-03 2018-01-23 株式会社田村制作所 软磁性粉末组合物、芯、电抗器
CN105108166B (zh) * 2015-09-29 2017-06-06 四川有色金源粉冶材料有限公司 一种注射成型用铁基合金粉末的制备方法
CN105149601A (zh) * 2015-09-29 2015-12-16 四川有色金源粉冶材料有限公司 一种高比重合金喂料的制备方法
JP7322846B2 (ja) * 2019-12-12 2023-08-08 株式会社村田製作所 軟磁性材料および圧粉成形体
US11948714B2 (en) 2019-12-12 2024-04-02 Murata Manufacturing Co., Ltd. Soft magnetic material and green compact

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BR0317661A (pt) 2005-12-06
CA2505381A1 (en) 2004-07-08
CN100548541C (zh) 2009-10-14
KR101035757B1 (ko) 2011-05-20
ZA200503597B (en) 2006-08-30
TW200422122A (en) 2004-11-01
WO2004056508A1 (en) 2004-07-08
JP2010251779A (ja) 2010-11-04
AU2003288880B8 (en) 2006-11-16
CA2505381C (en) 2011-12-13
RU2335817C2 (ru) 2008-10-10
ATE473064T1 (de) 2010-07-15
PL376102A1 (en) 2005-12-12
TWI229018B (en) 2005-03-11
CN1732059A (zh) 2006-02-08
KR20050085871A (ko) 2005-08-29
AU2003288880A1 (en) 2004-07-14
JP4886987B2 (ja) 2012-02-29
MXPA05006847A (es) 2005-08-16
PL209529B1 (pl) 2011-09-30
DE60333309D1 (de) 2010-08-19
AU2003288880B2 (en) 2006-10-12
RU2005123385A (ru) 2006-03-27
JP2006511711A (ja) 2006-04-06
ES2348212T3 (es) 2010-12-01
SE0203851D0 (sv) 2002-12-23
EP1575726A1 (en) 2005-09-21

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