US20080302501A1 - Steel for Hot Tooling, and Part Produced From Said Steel, Method for the Production Thereof, and Uses of the Same - Google Patents

Steel for Hot Tooling, and Part Produced From Said Steel, Method for the Production Thereof, and Uses of the Same Download PDF

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US20080302501A1
US20080302501A1 US12/095,174 US9517406A US2008302501A1 US 20080302501 A1 US20080302501 A1 US 20080302501A1 US 9517406 A US9517406 A US 9517406A US 2008302501 A1 US2008302501 A1 US 2008302501A1
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traces
steel
steel according
temperature
hardness
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Nicolas Binot
Andre Grellier
Pierre-Emmanuel Richy
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Aubert and Duval SA
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/46—Ferrous alloys, e.g. steel alloys containing chromium with nickel with vanadium
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/18—Hardening; Quenching with or without subsequent tempering
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/18—Hardening; Quenching with or without subsequent tempering
    • C21D1/19—Hardening; Quenching with or without subsequent tempering by interrupted quenching
    • C21D1/22—Martempering
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D6/00—Heat treatment of ferrous alloys
    • C21D6/004—Heat treatment of ferrous alloys containing Cr and Ni
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/001—Ferrous alloys, e.g. steel alloys containing N
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/52—Ferrous alloys, e.g. steel alloys containing chromium with nickel with cobalt
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D2211/00—Microstructure comprising significant phases
    • C21D2211/008—Martensite

Definitions

  • the invention relates to the field of steels for tooling for hot shaping, which can be used in foundry and moulding, forging, drawing or extrusion.
  • a field of application of the invention which is preferred but not exclusive is the production of moulds of large dimensions for foundry under pressure of light alloys based on aluminium or magnesium or of cuprous alloys.
  • the damage is produced in certain cases by sudden ruptures which instantaneously destroy the tool when the toughness of its material is insufficient. It is generally produced by cracking which starts during the first few hundred cycles of use and develops progressively until the tool is effectively ruined after several tens or hundreds of thousands of cycles. This process is designated by the generic term of “thermal fatigue”.
  • Resistance to damage by thermal fatigue requires a toughness which is sufficient at the temperature corresponding to the coolest point in the thermal cycle. This quality is conventionally measured by the energy of flexion due to shock of standard testpieces, testpieces tested at temperatures between ambient temperature and 150° C. It also requires sufficient properties of hardness and of resistance to softening in use at the hottest temperatures of the cycle.
  • the object of the invention is to propose a novel grade of steel for hot shaping tools producing an excellent compromise between the various properties which have just been mentioned.
  • the invention relates to a steel for hot tooling, having a composition in percentages by weight:
  • traces ⁇ Si ⁇ 040%.
  • traces ⁇ Al ⁇ 0.030%.
  • traces ⁇ O ⁇ 15 ppm Preferably, traces ⁇ O ⁇ 15 ppm.
  • the invention also relates to a method of manufacture of a part made from steel, characterised in that the said steel is prepared from a steel of the preceding type and in that it is subjected to austenisation in the temperature range from 1000 to 1050° C., followed by quenching.
  • the austenisation takes place in the range from 1015 to 1040° C.
  • the part is subjected to at least two temperings in the temperature range from 550 to 650° C., giving the said part a hardness of 42 to 52 HRC.
  • the invention also relates to a part made from steel obtained by the preceding method, characterised in that it is a part for tooling for hot shaping.
  • the said part can have a thickness greater than or equal to 200 mm.
  • It may be a mould or a die for foundry under pressure of light or cuprous alloys.
  • the said part may be a forging tool.
  • the said part may be a forging die.
  • the said part may be a tool for drilling or rolling steel tubes.
  • the said part may be a tool for shaping glass.
  • the said part may be a tool for shaping plastics materials.
  • the said part may be produced from a steel in which 0.335% ⁇ C ⁇ 0.375%, 2.00% ⁇ Ni ⁇ 2.40%, 1.80% ⁇ Mo+0.65W ⁇ 2.90% with 1.80% ⁇ Mo ⁇ 3.40% and W ⁇ 0.90%, 0.66% ⁇ V ⁇ 0.76%, and it is an extrusion die or a mould for founding aluminium alloy.
  • the invention also relates to use of a part for hot tooling, characterised in that the said part is made from a steel in which 0335% ⁇ C ⁇ 0375%, 2.00% ⁇ Ni ⁇ 2.40%, 1.80% ⁇ Mo+0.65W ⁇ 2.90% with 1.80% ⁇ Mo ⁇ 3.40% and W ⁇ 0.90%, 0.66% ⁇ V ⁇ 0.76% and its working temperature at the surface remains lower than 680° C.
  • the invention also relates to use of a part for hot tooling, characterised in that the said part is made from a steel in which 0.335% ⁇ C ⁇ 0.375%, 0.90% ⁇ Ni ⁇ 1.50%, 1.50% ⁇ Mo+0.6 W ⁇ 1.90% with W ⁇ 0.40%, 0.55% ⁇ V ⁇ 0.63% and its surface temperature in use remains lower than 770° C.
  • the invention is based in particular on a simultaneous adaptation of the softening and stabilising elements which are Mo and V, and Ni which neutralises their weakening effects.
  • the joining of the whole produces an improvement in the quenchability and therefore improves the capacity for reproducing on large parts the properties which until then had only been available on smaller tools.
  • the optimisation according to the invention of the composition of the steel has been possible because the inventors initially devoted themselves to effective measurement of the instantaneous heat flows which pass through the surface of the hot shaping tools while they are in use. They are then deduced therefrom by calculation of the transitory mechanical stresses induced by the thermal shocks which cause the cracks. This has made possible a better understanding of the mechanical behaviour of the material in operation. They were able to establish, by virtue of the experimental measurements which reconstitute the industrial quenching speeds on test samples, and by virtue of the thermodynamic simulations, the links which exist between the composition of the steel, the parameters of the heat treatment prior to its implementation and the microstructure thus obtained. In particular they demonstrated the crucial importance of the interdependence between the composition and the quenching temperature for obtaining the compromise sought between the various mechanical properties which are important in steels for hot tooling.
  • FIG. 1 which shows the evolution of the fraction of undissolved carbides according to the permitted temperature for the reference compositions ( FIGS. 1 a ) to 1 e )) to produce a composition according to the invention ( FIG. 1 f )),
  • FIG. 2 which shows the QCC curves of a reference steel ( FIG. 2 a )) and of a steel according to the invention ( FIG. 2 b )).
  • FIG. 3 which shows the comparison, for various reference samples and samples according to the invention, between the breaking energies after quenching carried out under laboratory conditions and quenching carried out under industrial conditions.
  • the invention is based essentially on the study of the actions and interactions of the elements carbon, chromium, molybdenum, vanadium and nickel and of the influence of the austenisation temperature before quenching on the mechanical properties of the steels studied.
  • the austenisation temperature decides the partitioning of the alloy elements between the undissolved carbides and the matrix.
  • the dissolution of the carbides is all the more advanced as the temperature rises.
  • the undissolved carbides must remain in an adequate quantity on the final product in order to control the grain size.
  • a fine grain is necessary in order to guarantee the properties of toughness and of resistance to fatigue.
  • the alloy elements dissolved in the matrix govern the quenchability, the resistance to annealing and in general all of the mechanical properties.
  • Table 2 illustrates, for one of the compositions studied (reference melt 10), the effect of the quenching temperature on the microstructure and the properties.
  • the increase in the austenisation temperature causes, in this case, both an improvement in the resistance to softening when hot and a loss of toughness.
  • thermodynamic simulation by the description of the phase equilibriums with the calculation code THERMOCALC® currently utilised by metallurgists, provides concrete elements of information on the amount of undissolved carbides for each of the types VC, M 23 C 6 and, possibly, M 6 C, Fe 3 C, M 2 C . . . . FIG. 1 was produced with the aid of such a simulation. It shows the evolution of the fraction of undissolved carbides according to the austenisation temperature for five reference compositions ( FIGS. 1 a ) to 1 e )) and a composition according to the invention ( FIG. 1 f )).
  • the experimental microstructural observations on the crude quenching state confirm the tendencies predicted by the simulation.
  • the austenisation temperatures are optimised according to the following principles:
  • an essential object of the invention consists of defining an equilibrium between:
  • the steels in the field of the invention must exhibit a hardness when hot which is sufficient in order to avoid recessing and to resist fatigue, and that in a first approximation they exhibit the same relation between hardness at 20° C. and hardness when hot, they have been compared in quenched and tempered thermal states which give them the same hardness at 20° C.
  • the preselected levels are 47, 45, 42 HRC.
  • the measurements were carried out systematically and simultaneously on laboratory test bars capable of being quenched at a high speed and on testpieces quenched in an experimental device reproducing a quenching speed representative of the treatment of industrial parts and chosen to be equal to 22° C. per minute on average within the range 900/400° C.
  • the measurements include:
  • Nickel Molybdenum Vanadium Point Ac1 Casting (%) (%) (%) (° C.) 1 0.06 1.21 0.47 825 7 0.08 2.29 0.57 820 8 0.15 1.62 0.64 805 12 1.42 1.21 0.46 770 13 2.93 1.23 0.47 680 20 0.59 2.14 0.77 800 22 (inv.) 1.63 1.82 0.71 755 23 (inv.) 1.05 1.78 0.70 785 26 (inv.) 2.19 2.28 0.70 710
  • Table 5 illustrates the effect of the alloy elements on the resistance to reduction in hardness whilst being kept at high temperature.
  • the hardnesses of 47 and 42 HRC are obtained after two temperings each of two hours, the first at 550° C., the second at the characteristic temperature appearing in the table.
  • Table 5A shows the results obtained on a reference sample 1 and on two samples 12, 13 having a nickel content higher than the reference sample.
  • Table 5B shows the results obtained on the sample 1 and on samples 3, 5, 6, 8 which show contents of Mo and possibly V which are higher than those of the sample 1.
  • Table 5C shows the results obtained on samples 8 and 22 on the one hand and 6 and 26 on the other hand which show contents of Ni, Mo and V which are higher than the sample 1.
  • ⁇ HRC 5 - A Effect of an addition of nickel on the reference composition 1 0.06 1.21 0.47 603 625 7.0 605 619 8.0 12 1.42 1.21 0.46 593 618 7.5 597 623 8.0 13 2.93 1.23 0.47 588 611 8.5 592 613 9.0 5 - B: Effect of additions of molybdenum and vanadium on the reference composition 1 0.06 1.21 0.47 603 625 7.0 605 619 8.0 3 0.16 1.74 0.49 605 630 5.0 608 624 6.0 5 0.17 2.74 0.48 622 648 5.0 620 637 6.5 6 0.11 2.24 0.54 617 640 5.0 617 638 6.0 8 0.15 1.62 0.64 610 638 4.5 612 631 6.5 5 - C: Effect of combined additions of nickel, molybdenum and vanadium, samples outside the invention (castings 6, 8) and samples according to the invention (castings 22, 26) 6 0.11 2.24 0.54 617 640 5.0 6
  • Table 5-A demonstrates the detrimental effect of a simple addition of nickel which lowers the tempering temperature too markedly for a recording of hardness and increases the loss of hardness when kept hot for a prolonged period.
  • a lowering of the tempering temperature is damaging in that the steel must offer the highest possible operating temperature, situated at least between 600 and 630° C., for fear of softening it excessively.
  • Table 5-B shows the beneficial effect of the simple additions of molybdenum and vanadium in order to increase the resistance to tempering and to softening in operation.
  • the reduction of the quenching speed between the laboratory conditions and the industrial conditions is detrimental for these characteristics, which is due to insufficient quenchability of the material.
  • composition pairs (8, 22) and (6, 26) in Table 5-C illustrates that in laboratory conditions the castings with nickel offer a lesser resistance to the lowering of the hardness than the corresponding castings with a low nickel content, but that with industrial quenching their properties become very close.
  • FIG. 2 compares the QCC continuous cooling diagrams of the reference composition 1 ( FIG. 2 a ) which have been subjected to an austenisation at 990° C. for 30 minutes and of the composition 22 according to the invention ( FIG. 2 b ) which has been subjected to an austenisation at 1030° C. for 30 minutes.
  • the composition according to the invention has pearlitic zones and bainitic zones which are clearly offset towards the low cooling speeds relative to the reference composition. Consequently, knowing that the usual industrial quenchings (of which the paths are shown in bold in FIGS. 2 a and 2 b ) make it possible to reach, on the tools to be treated, a temperature of 400° C. in 1000 to 5000 seconds according to the sizes of the parts and the situation in the part, the composition according to the invention enables an exclusive martensitic transformation. On the contrary, the reference composition necessitates the formation of a significant proportion of bainite, which is less favourable to obtaining the envisaged properties.
  • Table 6 illustrates the representative trends over a selection of results; the combined addition of Ni, Mo, V effected on the casting 21 according to the invention is favourable at the same time for obtaining the highest resilience values after treatment under the industrial conditions and the slightest reduction caused by the slowing down of the quenching speed.
  • FIG. 3 compares, for all of the castings, the values obtained with a quenching according to the industrial speed and those resulting from a rapid quenching for one and the same composition of the metal, wherein the pairs of batches of testpieces then undergo annealings in order to record hardnesses of 42, 45 and 47 HRC and the testpieces are broken at 20° C. and at 100° C. Each point is representative of a hardness and of a temperature of breaking of the testpiece. The results demonstrate that the loss of hardness due to the reduction in the quenching speed is very generally more limited for the compositions according to the invention.
  • the average values of the energies of flexion due to shock set out in Table 7 confirm that the steel 22 according to the invention has superior properties, in particular in the core block position, a position which represents even larger part sizes.
  • it has a detrimental effect on the toughness.
  • Their level should be within the range situated between a value of at least 0.30% necessary for obtaining a sufficient hardness and of 0.39% at most in order to avoid an irremediable fragility. The optimum range is from 0.33 to 0.38%.
  • Chromium has a favourable effect for the quenchability. It plays a part in the hardening by tempering, and for the preferred applications envisaged by the invention, namely large parts which necessitate a high hardness (42 to 52 HRC), this characteristic is advantageous.
  • the carbides which it generates evolve quickly to more stable forms and do not prove very effective for the resistance to the reduction in hardness at high temperature. It is therefore essential to complement the addition of Cr by other carbide-forming elements such as Mo and V.
  • the content of this element must remain limited between a minimum of 4.0% necessary for the quenchability and a maximum of 6.0% above which its action partially inhibits that of vanadium and of molybdenum.
  • a Cr content of 4.6 to 6% is set.
  • Molybdenum improves the quenchability. It combines with chromium in the same chromium-based carbides, which contributes to an increase in the number thereof. At high contents it forms specific species M 2 C, M 6 C. With regard to the macroscopic properties it increases the hardness and the resistance to tempering and decreases the toughness. Its content is between 1.50 and 2.60%. It is also necessary to take into account the possible presence of tungsten as will be described below. Preferably, the Mo content is between 1.60 and 2.00% with Mo+0.65W between 1.60 and 2.20%.
  • Vanadium forms specific carbides of the VC type which, in the area covered by the experimental castings, are predominant among the precipitates which are not dissolved at the austenisation temperature and thus ensure that the grain does not enlarge.
  • new generations of micro- and nanometric carbides are precipitated and by their interaction with crystal defects of the martensite participate actively in the secondary softening and in the resistance to softening in operation under the effect of the temperature and of the cyclical forces.
  • an excess of these carbides formed during tempering causes a marked weakening.
  • the vanadium content must of necessity be between 0.55% and 0.75%.
  • Nickel has a negative effect on the hardness in the treated state; it decreases the tempering temperature to be applied in order to obtain an envisaged hardness, and the resistance to softening while maintained at operating temperatures. Moreover an excessive content of the order of 3% lowers the re-austenisation point too markedly within the range of the temperatures used, which must be absolutely avoided. On the other hand, nickel increases the quenchability, in particular for contents of 1 to 3% and significantly improves the toughness. It is considered that within the context of the invention the Ni content is between 0.80 and 2.80%. The negative effects on the hardness of a substantial addition of Ni can be compensated for by additions of Cr, Mo, V and W within the prescribed limits.
  • Tungsten may constitute an optional additional element within the limit of 1.45% maximum and under conditions such that the content of Mo+0.65W is between 1.50 and 3.20% with the Mo content between 1.50 and 2.60%, preferably between 1.60 and 2.20% with the Mo content between 1.60 and 2.00%.
  • the tungsten complements the action of the molybdenum with an equivalence ratio of 1% for 0.65% of Mo.
  • This addition of tungsten causes limited negative effects on the toughness and the quenchability and positive effects on the resistance to softening when hot, in particular for test temperatures higher than 560° C., for example 600° C.
  • Cobalt may be added up to an upper limit of 2.75%. It has a favourable effect for the resistance to softening, in particular for residence temperatures of the order of 600° C., but its action is detrimental to the quenchability. Taking account of the high price of this additional element, it does not appear that its use must be particularly recommended.
  • K between ⁇ 0.65 and +0.65, preferably between ⁇ 0.35 and +0.35, optimally as close to zero as possible, with:
  • Table 1 sets out the values of the coefficients K1, K2, K for all of the castings.
  • Silicon due to its detrimental effect on the toughness, must be kept at a low level compatible with economic industrial production conditions; a limit of 0.50% and preferably of 0.40% must not be exceeded.
  • Manganese which is favourable to the quenchability, but detrimental to the toughness, must not be present in a content higher than 0.80%, preferably 0.60%.
  • the aluminium content must be between traces and 0.080%, preferably between traces and 0.030%. Its function is to deoxidise the steel, thus limiting the quantity of inclusions of oxides capable in particular of decreasing the resistance to fatigue of the steel. From this point of view and simultaneously the oxygen content must not exceed 30 ppm, preferably 15 ppm.
  • a high Al content reduces the O content dissolved in the liquid steel, but it also renders the liquid steel more sensitive to atmospheric reoxidations during casting and therefore increases the risk of forming detrimental oxidised inclusions.
  • the steels according to the invention can fall within two quality levels.
  • a “standard” level of quality is attained when the composition does not absolutely have to be situated within the optimal ranges which are defined above for all the elements.
  • the improvement relative to the prior art then resides above all in the properties of quenchability. These allow the manufacture of large products which have a high hardness and are homogeneous in the entire section of the products.
  • a “superior” level of quality is attained when all the elements are situated within the optimal ranges of contents defined above. Under these conditions, in addition to the improved quenchability, a high toughness is obtained which provides, in conjunction with the high hardness, a great resistance to thermal fatigue and to sudden rupture.
  • VAR vacuum arc refusion
  • ESR electroconductive slag refusion
  • the invention has a preferred application in the manufacture of such parts having a thickness of 200 mm and more.

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US12/095,174 2005-11-29 2006-11-28 Steel for Hot Tooling, and Part Produced From Said Steel, Method for the Production Thereof, and Uses of the Same Abandoned US20080302501A1 (en)

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FR0512091 2005-11-29
FR0512091A FR2893954B1 (fr) 2005-11-29 2005-11-29 Acier pour outillage a chaud, et piece realisee en cet acier et son procede de fabrication
PCT/FR2006/002607 WO2007063210A1 (fr) 2005-11-29 2006-11-28 Acier pour outillage a chaud, et piece realisee en cet acier, son procede de fabrication et ses utilisations.

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US20100276038A1 (en) * 2007-09-10 2010-11-04 Aubert & Duval Martensitic stainless steel, method for making parts from said steel and parts thus made
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US9464336B2 (en) 2010-09-14 2016-10-11 Snecma Martensitic stainless steel machineability optimization
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US11319621B2 (en) 2018-04-02 2022-05-03 Daido Steel Co., Ltd. Steel for mold, and mold
EP3862458A4 (en) * 2018-10-05 2022-09-28 Hitachi Metals, Ltd. HOT WORK STEEL AND HOT WORK TOOL
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JP6032881B2 (ja) * 2011-10-18 2016-11-30 山陽特殊製鋼株式会社 熱間金型用鋼
CN103725859B (zh) * 2013-11-30 2015-09-16 常熟市东鑫钢管有限公司 无缝钢管的制造方法
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CN105886942A (zh) * 2016-06-21 2016-08-24 安庆市灵宝机械有限责任公司 一种高钨耐磨合金钢
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BRPI0620491A2 (pt) 2011-11-16
EP1954846A1 (fr) 2008-08-13
CN101316943B (zh) 2012-07-04
JP2009517546A (ja) 2009-04-30
FR2893954B1 (fr) 2008-02-29
WO2007063210A1 (fr) 2007-06-07
CN102851608A (zh) 2013-01-02
AR057195A1 (es) 2007-11-21
TW200734471A (en) 2007-09-16
HK1122072A1 (en) 2009-05-08

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