Classifications

• • 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
  • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
  • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
  • C21D8/1216—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the working step(s) being of interest
  • C21D8/1222—Hot rolling
• • 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
  • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
  • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
  • C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
  • C21D8/1272—Final recrystallisation annealing
• • 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
  • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
• • 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
  • C22C38/004—Very low carbon steels, i.e. having a carbon content of less than 0,01%
• • 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
  • C22C38/008—Ferrous alloys, e.g. steel alloys containing tin
• • 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
  • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
• • 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
  • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
• • 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
  • C22C38/08—Ferrous alloys, e.g. steel alloys containing nickel
• • 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
  • C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
• • 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
  • C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
• • 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
  • C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
• • 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
• • 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
  • H01F1/16—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 sheets
• • 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
  • C21D2201/00—Treatment for obtaining particular effects
  • C21D2201/05—Grain orientation
• • 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
  • C21D2211/004—Dispersions; Precipitations

Definitions

• the present invention relates to a high-strength non-oriented electrical steel sheet suitable for an iron core material of an electric vehicle motor and an electrical apparatus motor, and a method of manufacturing the same.
• a high-speed rotation motor is also used for a machine tool and an electrical apparatus such as a vacuum cleaner.
• An outer size of a high-speed rotation motor for an electric vehicle is larger than that of a high-speed rotation motor for an electrical apparatus.
• a DC brushless motor is mainly used as the high-speed rotation motor for an electric vehicle.
• magnets are embedded in the vicinity of an outer periphery of a rotor.
• a width of a bridge portion in an outer periphery portion of the rotor (a width between magnets from the most outer periphery of the rotor to a steel sheet) is extremely narrow, which is 1 to 2 mm, depending on a position.
• a high-strength steel sheet has been required for the high-speed rotation motor for an electric vehicle rather than a conventional non-oriented electrical steel sheet.
• Patent Document 1 there is disclosed a non-oriented electrical steel sheet in which Mn and Ni are added to Si to achieve solid solution strengthening.
• Mn and Ni are added to Si to achieve solid solution strengthening.
• due to the addition of Mn and Ni its toughness is likely to be reduced, and sufficient productivity and a sufficient yield cannot be obtained.
• prices of alloys to be added are high. In recent years in particular, the price of Ni has suddenly risen due to a worldwide demand balance.
• Patent Documents 2 and 3 there are disclosed non-oriented electrical steel sheets in which carbonitrides are dispersed in steel to achieve strengthening. However, it is not possible to obtain sufficient strength even by these non-oriented electrical steel sheets.
• Patent Document 4 there is disclosed a non-oriented electrical steel sheet in which a Cu precipitate is used to achieve strengthening.
• a thermal treatment condition is restricted.
• strength and magnetic properties to be required cannot be obtained.
• An object of the present invention is to provide a high-strength non-oriented electrical steel sheet capable of easily obtaining high strength and magnetic properties and a method of manufacturing the same.
• the following is set as the gist in order to solve the above-described problems.
• a high-strength non-oriented electrical steel sheet contains:
• the high-strength non-oriented electrical steel sheet described in (I), further contains by mass%, Ni: not less than 0.5% nor more than 3.0%.
• a method of manufacturing a high-strength non-oriented electrical steel sheet includes:
• the method of manufacturing a high-strength non-oriented electrical steel sheet described in (V), further includes: annealing the hot-rolled sheet between the obtaining the hot-rolled sheet and the pickling the hot-rolled sheet.
• a method of manufacturing a high-strength non-oriented electrical steel sheet includes:
• a method of manufacturing a high-strength non-oriented electrical steel sheet includes:
• the present inventors have investigated the reason why strength and magnetic properties are greatly affected by thermal treatment conditions in a conventional steel strengthening method in which a Cu precipitate is used. As a result, it has been found that a high annealing temperature making Cu once solid-dissolving is needed at finish-annealing after cold rolling in order to strengthen a steel sheet by precipitation of Cu.
• a magnetic property required for a rotor being the main use of a high-strength electrical steel sheet is an eddy current loss (We) at a high frequency of 400 Hz or more, and as for a reduction in the eddy current loss (We) as well, making crystal grains fine by containing C, N, Nb, Zr, Ti, and V is effective.
• the recrystallization area ratio at finish-annealing at 900°C was low. This is inferred that Nb, which was a little contained, precipitated immediately before recrystallization during finish-annealing to delay recrystallization. Further, it is inferred that at finish-annealing at 1000°C, Nb solid-dissolved to coarsen crystal grains, and thus a result similar to that of Material F was exhibited.
• Finish-annealing at 800°C has been so far performed as a process of making crystal grains fine. That is, finish-annealing at 800°C has been performed under a purpose in which by finish-annealing as above, Cu once solid-dissolves to achieve high-strengthening, and a steel sheet is recrystallized, and then crystal grains are not allowed to be coarsened.
• finish-annealing at 800°C has been performed under a purpose in which by finish-annealing as above, Cu once solid-dissolves to achieve high-strengthening, and a steel sheet is recrystallized, and then crystal grains are not allowed to be coarsened.
• the present invention as will be described below makes it possible to achieve both mechanical properties and magnetic properties.
• % means mass%.
• C is an element necessary for making crystal grains fine. Fine carbide increases nucleation sites at the time of recrystallization and further has an effect of suppressing crystal grain growth. In order to enjoy the effect, a C content is 0.002% or more.
• N is less than 0.005% in particular, the preferable C content is 0.01% or more, and more preferably 0.02% or more.
• an upper limit of the C content is set to 0.05%.
• Si is effective for reducing the eddy current loss, and is an element effective for solid solution strengthening as well.
• an upper limit of a Si content is set to 4.0%.
• a lower limit is set to 2.0%.
• Mn similarly to Si, reduces the eddy current loss, and is an element effective for increasing strength.
• an upper limit of the Mn content is set to 1.0%.
• a lower limit is set to 0.05%.
• Al similarly to Si, is an element effective for increasing resistivity.
• an Al content exceeds 3.0%, castability is reduced, and thus considering productivity, an upper limit of the Al content is set to 3.0%.
• a lower limit is not set in particular.
• the Al content in the case of Al deoxidation is 0.02% or more, and the Al content in the case of Si deoxidation is 0.01% or more.
• N is an element necessary for making crystal grains fine. Fine nitride increases nucleation sites at the time of recrystallization, and further has an effect of suppressing crystal grain growth. In order to enjoy the effect, an N content is set to 0.002% or more. When N of 0.005% or more is contained greatly over a normal level, the effect of suppressing crystal grain growth becomes further remarkable. The higher the N content is, the larger the above effect is, so that the N content is preferably further increased to 0.01% or more, and more preferably to 0.02% or more. In the case when the C content is less than 0.005% in particular, the effect to be obtained by the N addition as above appears more strongly. On the other hand, when N is added over 0.05%, the fracture elongation is remarkably reduced. Thus, an upper limit of the N content is set to 0.05%.
• Cu is an important element of bringing precipitation strengthening.
• a Cu content is less than 0.5%, Cu completely solid-dissolves in the steel and an effect of the precipitation strengthening cannot be obtained, so that a lower limit of the Cu content is set to 0.5%.
• An upper limit is set to 3.0% in consideration of the fact that strength is to be saturated.
• Ni is an effective element that hardly embrittles the steel sheet to enable the steel sheet to be high-strengthened.
• Ni may be added depending on strength to be required because it is expensive. In the case when Ni is added, 0.5% or more is preferably contained in order to sufficiently obtain an effect of Ni. Further, an upper limit is set to 3.0% in consideration of its cost. Further, from the viewpoint of suppressing a scab to occur by the Cu addition, Ni of 1/2 or more of a Cu addition amount is preferably added.
• Sn improves texture and further has an effect of suppressing nitriding and oxidation at the time of annealing. Particularly, an effect of improving a magnetic flux density to be reduced by the Cu addition is large.
• an Sn content is less than 0.01%, the desired effects cannot be obtained, and on the other hand, when Sn is added over 0.10%, there is sometimes a case that an increase in a scab is caused.
• an Sn addition amount is preferably not less than 0.01% nor more than 0.10%.
• B segregates in grain boundaries and has an effect of increasing toughnesses of a hot-rolled sheet and a hot-rolled-annealed sheet.
• a B content is less than 0.0010%, the desired effect cannot be obtained, and on the other hand, when B is added over 0.0050%, there is sometimes a case that a slab crack at the time of casting occurs.
• a B addition amount is preferably not less than 0.0010% nor more than 0.0050%.
• Nb represents a Nb content (mass%)
• Zr represents a Zr content (mass%)
• Ti represents a Ti content (mass%)
• V represents a V content (mass%)
• a precipitation amount becomes insufficient, and the sufficient effect of suppressing crystal grains cannot be obtained.
• a lower limit of the value on the right side is set to 2.0 ⁇ 10 -4 .
• excess contents of these elements solid-dissolve in the steel and do not affect properties of the steel, so that an upper limit of the value on the right side is not defined in particular.
• the value on the right side is preferably 1.0 ⁇ 10 -2 or less.
• Formula (2) where a relationship of the six elements of C, N, Nb, Zr, Ti, and V is defined, is an important parameter for making crystal grains fine in alliance with Formula (1).
• [C] represents the C content (mass%) and [N] represents the N content (mass%) .
• Formula (1) is merely such that a maximum amount capable of forming carbide or nitride is defined, and it is not possible to sufficiently suppress crystal grain growth during final annealing only by the above condition.
• the second term in Formula (2) is such that the right side in Formula (1) is subtracted from the sum of a value obtained after mass% of C is divided by an atomic weight and a value obtained after mass% of N is divided by an atomic weight, and is a parameter representing the excess C amount and/or N amount that do/does not form carbonitride.
• carbide, nitride, and carbonitride have extremely important roles, and among them, nitride and carbonitride are effective, and particularly, nitride has a remarkable effect. That is, when carbide and nitride are compared, nitride is more effective for the effect of the present invention, and nitride rather exhibits the effect contributing to the effect of the present invention by a reduced amount. Further, when carbide and nitride in the same amount are compared, nitride rather can obtain a large favorable effect, and can suppress an unfavorable side effect.
• the "favorable effect” to be described here means making crystal grains fine, high-strengthening, and stability at a high temperature
• the "unfavorable side effect” means an increase in a core loss and a crack originating from a precipitate (embittlement in particular).
• a composition thereof varies depending on forming processes, so that properties and effects of carbonitride do not become the same, but it is said that carbonitride exhibits a more favorable effect than the precipitate composed of at least only carbide.
• a ratio of the N content to the C content is preferably high, and [N]/[C] is preferably three or more, and more preferably five or more.
• a composition of carbonitride is considered to change by effects such that, for example, carbide is set as initial formation, nitride is set as initial formation, structure similar to that of carbide is held in a growth process, structure similar to that of nitride is held in a growth process and the like.
• thermal stability of carbonitride weakens.
• carbonitride precipitates immediately before recrystallization during finish-annealing to delay recrystallization, and further an annealing temperature is increased, the precipitate solid-dissolves again and crystal grains are coarsened, resulting that it becomes difficult to form fine grains stably.
• C and/or N become/becomes excessive to a level where the parameter value exceeds 3.0 ⁇ 10 -3 , hardening occurs during cooling, and elongation and toughness of the steel sheet deteriorate.
• a lower limit of the parameter value in Formula (2) is set to 1.0 ⁇ 10 -3
• an upper limit is set to 3.0 ⁇ 10 -3 .
• the above recrystallization area ratio is set to 50% or more.
• the yield stress at a tensile test is set to 700 MPa or more in consideration of strength to be required for a rotor to rotate at a high speed. Note that the yield stress to be defined here is a lower yield point.
• the fracture elongation is set to 10% or more from the viewpoint of suppressing a crack in a punched-out end surface of a motor core.
• the eddy current loss is a loss to occur after current flows through a steel sheet at excitation, and in the case when the above loss is large, the motor core easily generates heat to cause demagnetization of magnets.
• An eddy current loss We 100/400 has large dependence on a sheet thickness of the steel sheet, and thus a sheet thickness t (mm) is set as a parameter to set the eddy current loss We 100/400 to 70 ⁇ t 2 or less as shown in Formula (3) as a tolerance range of the rotor heat generation. W ⁇ e 10 / 400 ⁇ 70 ⁇ t 2
• a dual frequency method is used as a method of calculating the above eddy current loss.
• a core loss at a frequency f 1 is set to W 1 and a core loss at a frequency f 2 is set to W 2
• the eddy current loss We 10/400 of W 10/400 can be calculated by "(W 2 /f 2 -W 1 /f 1 )/(f 2 -f 1 ) ⁇ 400 ⁇ 400".
• the calculation is possible to be performed, and thus a measurement frequency is not defined in particular. However, if possible, the calculation is preferably performed at a frequency close to 400 Hz, or in a frequency range of, for example, 100 to 800 Hz or so.
• the maximum magnetic flux density Bmax is a maximum magnetic flux density to be excited when measuring a core loss.
• a soaking temperature T (°C) of finish-annealing has to be a solid solution temperature of Cu or more.
• the solid solution temperature depends on the Cu content.
• a temperature (°C) is 200 ⁇ a + 500 or more, Cu completely solid-dissolves, so that the soaking temperature T (°C) of finish-annealing is set to 200 ⁇ a + 500 or more as shown in Formula (4).
• a coiling temperature at the time of hot rolling exceeds 550°C, carbonitride and a Cu precipitate, depending on a hot-rolled sheet, remarkably reduce its toughness.
• the coiling temperature at the time of hot rolling is set to 550°C or less.
• a ductile/brittle fracture transition temperature at a Charpy impact test is set to 70°C or less from the viewpoint of fracture suppression at the time of cold rolling.
• the cooling rate in the above temperature range is set to 50°C/sec or more.
• the toughness of the steel sheet after annealing is set to 70°C or less from the viewpoint of fracture suppression at the time of cold rolling.
• an annealing temperature of the hot-rolled sheet is not defined in particular, but the purpose of annealing of the hot-rolled sheet is recrystallization and grain growth promotion of the hot-rolled sheet, and thus the annealing temperature is preferably 900°C or more, and on the other hand, from the viewpoint of brittleness, it is preferably 1100°C or less.
• the transition temperature defined here is a temperature such that as defined in Japan Industrial Standard (JIS), in a transition curve showing a relationship between a test temperature and a ductile fracture rate, the ductile fracture rate is 50%.
• JIS Japan Industrial Standard
• a temperature corresponding an average value of absorbed energy at the ductile fracture rate of 0% and absorbed energy at the ductile fracture rate of 100% may also be employed.
• a length and height of a test piece to be used for the Charpy impact test are set to sizes defined in JIS.
• a width of the test piece is set to a thickness of the hot-rolled sheet.
• the size, in a rolling direction is 55 mm in length and 10 mm in height, and the width is 1.5 mm to 3.0 mm or so depending on the thickness of the hot-rolled sheet.
• the plural test pieces are stacked to approximate a thickness of 10 mm that is a regular test condition.
• Non-existence Invention example c8 1.3 0.8 720 12 9.2 Non-existence Invention example c9 1.7 0.6 740 21 4.2 Non-existence Invention example c10 2.5 0.4 760 11 4.1 Existence Invention example c11 3.5 0.4 2.5 650 17 3.4 Non-existence Comparative example c12 0.6 1.7 710 14 3.3 Non-existence Invention example c13 1.1 0.9 730 13 3.2 Non-existence Invention example c14 2.1 0.5 790 13 3.3 Non-existence Invention example c15 2.5 0.4 810 12 3.2 Existence Invention example c16 3.9 0.4 2.5 690 15 2.9 Non-existence Comparative example c17 0.6 1.7 720 11 2.8 Non-existence Invention example c18 1.1 0.9 770 11 2.9 Non-existence Invention example c19 1.9 0 .5 880 11 3.0 Non-existence Invention example c20 2.6 0.4 900 10 2.8 Existence Invention example c21 4.1 0.4 2.5 820 1
• these hot-rolled sheets were annealed (intermediate annealed) at 1050°C for 60 seconds and further are pickled, and by cold rolling once, cold-rolled sheets having sheet thicknesses of 0.35 mm were obtained. Finish-annealing at 950°C for 60 seconds was applied to these cold-rolled sheets.
• Table 8 the B amount, the Sn amount, the transition temperature after intermediate annealing, and the magnetic flux density after finish-annealing are shown.
• a non-oriented electrical steel sheet excellent in strength can be provided at a low cost.

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• 2009
  • 2009-04-13 WO PCT/JP2009/057453 patent/WO2009128428A1/fr active Application Filing
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