• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    An iron powder for dust cores has an apparent density is 3.8 g/cmor more, a mean particle size (D50) is 80 μm or more, 60 % or more of powder with a powder particle size of 100 gm or more has a mean grain size of 80 μm or more inside the powder particle, an area ratio of inclusions to a matrix phase of the powder is 0.4 % or less, and a micro Vickers hardness (testing force: 0.245 N) of a powder cross-section is 90 Hv or less. It is thus possible to obtain iron powder for dust cores in order to manufacture a dust core that has low hysteresis loss even after the iron powder is formed and subjected to strain relief annealing.
    公开号:SE540046C2
    申请号:SE1551331
    申请日:2014-03-18
    公开日:2018-03-06
    发明作者:Takashita Takuya；Nakamura Naomichi
    申请人:Jfe Steel Corp；
    IPC主号:
    专利说明:

    [2] [0002] Magnetic cores used in motors, transformers, and the like are requiredto have high magnetic flux density and low iron loss. Conventionally,electrical steel sheets have been stacked in such magnetic cores, yet in recentyears, dust cores have attracted attention as magnetic core material formotors.
    [3] [0003] The most notable characteristic of a dust core is that a 3D magneticcircuit can be formed. Since electrical steel sheets are stacked to form amagnetic core, the degree of freedom for the shape is limited. A dust core, onthe other hand, is formed by pressing soft magnetic particles coated withinsulation coating. Therefore, all that is needed is a die in order to obtain agreater degree of freedom for the shape than with electrical steel sheets.[0004] Press forming is also a shorter process than stacking steel sheets and isless expensive. Combined with the low cost of the base powder, dust coresachieve excellent cost performance. Furthermore, since the surfaces of theelectrical steel sheets are insulated, the magnetic properties of the electricalsteel sheet in the direction parallel to the steel sheet surface and the directionperpendicular to the surface differ, causing the magnetic cores consisting ofstacked electrical steel sheets to have the defect of poor magnetic propertiesin the direction perpendicular to the surface. By contrast, in a dust core, eachparticle is coated with insulation coating, yielding uniform magneticproperties in every direction. A dust core is therefore appropriate for use in a3D magnetic circuit.
    [5] [0005] Dust cores are thus indispensable material for designing 3D magneticcircuits, and due to their excellent cost performance, they have also been usedin recent years from the perspectives of reducing the size of motors, reducinguse of rare earth elements, reducing costs, and the like. Research anddevelopment of motors with 3D magnetic circuits has thus flourished.
    [6] [0006] When manufacturing high-performance magnetic components using such powder metallurgy techniques, there is a demand for components to haveexcellent iron loss properties after formation (low hysteresis loss and loweddy current loss).
    [9] [0009] PTL 1: JP 4630251 BPTL 2: WO08/032707PTL 3: JP H08-921 BPTL 4: JP 2005-187918 APTL 5: JP 2007-092162 A
    [10] [0010] While a reduction in iron loss is considered in the techniquesdisclosed in PTL 1 and PTL 2, the value remains high at 40 W/kg for iron lossat 1.5 T and 200 Hz.
    [11] [0011] It could therefore be helpful to provide iron powder for dust cores inorder to manufacture a dust core that has low hysteresis loss even after the iron powder is formed and subjected to strain relief annealing.
    [12] [0012] In the case of an iron core used at a relatively low frequency (3 kHz orless), such as a motor iron core, hysteresis loss accounts for the majority ofiron loss. Nevertheless, the hysteresis loss of a dust core is extremely high ascompared to a stacked steel sheet. In other words, in order to reduce iron lossofa dust core, reduction of hysteresis loss becomes extremely important.[0013] Upon carefully examining hysteresis loss in dust cores, we discoveredthat hysteresis loss in dust cores has a particularly strong correlation with theinverse of the grain size ofthe green compact, and that when the inverse ofthe grain size is small, i.e. in the case of coarse crystal grains, low hysteresisloss is obtained.
    [14] [0014] Furthermore, in order to obtain a dust core with coarse crystal grains, we discovered that the following factors are important: (I) a coarse particle size and grain size in the original powder, (II) no unnecessary strain in the powder, (III) strain not accumulating easily upon formation, and (IV) nothing to impede growth of crystal grains in the powder at the time ofstrain relief annealing.
    [15] [0015] We thus provide: 1. An iron powder for dust cores comprising iron as a principal component,wherein the iron powder has an apparent density of 3.8 g/cm3 or more and amean particle size (D50) of 80 um or more, 60 % or more of powder with apowder particle size of 100 um or more has a mean grain size of 80 um ormore inside the powder particle, an area ratio of an inclusion within an area ofa matrix phase ofthe powder is 0.4 % or less, and a micro Vickers hardness(testing force: 0.245 N) of a powder cross-section is 90 Hv or less.
    [16] [0016] 2. The iron powder for dust cores of 1., wherein 70 % or more ofthepowder with the powder particle size of 100 um or more has the mean grainsize of 80 um or more inside the powder particle.
    [17] [0017] It is thus possible to obtain iron powder for dust cores in order tomanufacture a dust core that has a coarse grain size and low hysteresis loss even after the iron powder is formed and subjected to strain relief annealing.
    [20] [0020] (Mean particle size: D50) The upper limit on the grain size ofthe green compact is the particlesize of the base power. The reason is that in the case of a dust core, theparticle surface is covered by an insulating layer, and the crystal grain cannotgrow coarser beyond the insulating layer. Therefore, the mean particle size ofthe powder should be as large as possible, such as 80 um or more andpreferably 90 um or more. No upper limit is placed on the mean particle sizeofthe powder, yet the upper limit may be approximately 425 um.
    [21] [0021] (Grain size within particles having a particle size of 100 um or more) At the time of plastic deformation, high strain easily accumulates atcrystal grain boundaries, which easily become nuclei-generating sites ofrecrystallized grains. In particular, powder with a large powder particle sizeeasily undergoes plastic deformation at the time of formation, and straineasily accumulates. Therefore, in powder with a powder particle size of 100um or more, there should be few crystal grain boundaries in the powder state.Specifically, 60 % or more of powder with a powder particle size of 100 um ormore needs to have a mean grain size of 80 um or more inside the powderparticle when the mean grain size measured by powder cross-sectionobservation. The ratio of powder for which the mean grain size is 80 um ormore is preferably 70 % or more.
    [22] [0022] The grain size of our powder may be calculated with the followingmethod.
    [24] [0024] (Area ratio of inclusions) When present in the powder, inclusions become a pinning site at thetime of recrystallization and thus are not preferable for suppressing graingrowth. Furthermore, inclusions themselves become nuclei-generating sites ofrecrystallized grains and refine the crystal grain after formation and strainrelief annealing. Inclusions themselves also cause an increase in hysteresisloss. Therefore, there are preferably few inclusions, and when observing apowder cross-section, the area ratio of inclusions should be 0.4 % or less ofthe area of the matrix phase ofthe powder, preferably 0.2 % or less. The lowerlimit is not restricted and may be 0 %. The area of the matrix phase of thepowder refers to the phase occupying 50 % or more of the powdercross-sectional area when observing a cross-section of a certain powder. For example, in the case of pure iron powder, the matrix phase refers to the ferrite phase in the powder cross-section. In the case of pure iron powder, the matrixphase is the result of subtracting the area of voids within the grain boundaryofthe powder from the area surrounded by the grain boundary ofthe powder.[0025] Oxides including one or more of Mg, Al, Si, Ca, Mn, Cr, Ti, Fe, andthe like are possible inclusions. The area ratio of inclusions may be calculatedwith the following method.
    [26] [0026] First, the iron powder to be measured is mixed into thermoplastic resinpowder. The resulting mixed powder is then injected into an appropriate moldand heated to melt the resin. The result is cooled and hardened to yield a resinsolid that contains iron powder. An appropriate cross-section of this resinsolid that contains iron powder is cut, and the resulting face is polished andtreated by corrosion. Using a scanning electron microscope (1000x to 5000xmagnification), the cross-sectional microstructure ofthe iron powder particlesis then observed and imaged as a backscattered electron image. In thecaptured image, inclusions appear with dark contrast. Therefore, the area ratioof inclusions can be calculated by applying image processing. We performedthis process in any five or more fields chosen from the entire amount of ironpowder that is being measured and then used the mean area ratio of inclusionsin each field.
    [27] [0027] (Micro Vickers hardness of powder cross-section) If strain accumulates inside the powder from before formation, then even if the above-described powder adjustment is performed, the crystalgrains end up being refined, after formation and strain relief annealing, to theextent of the accumulated strain. Accordingly, the strain in the powder shouldbe reduced insofar as possible.For manufacturing reasons, however, atomized iron powder issubjected to reduction annealing in order to reduce the oxygen content, afterwhich the iron powder needs to be mechanically crushed. Therefore, strainaccumulates in the powder.
    [28] [0028] The micro Vickers hardness can be measured with the followingmethod.
    [29] [0029] Next, a representative method of manufacturing to obtain our productis described. Of course, a method other than the one described below may beused to obtain our product.
    [30] [0030] The atomizing method may be of any type, such as gas, water, gas andwater, centrifugation, or the like. In practical terms, however, it is preferableto use an inexpensive water atomizing method or a gas atomizing method,which is more expensive than a water atomizing method yet which allows forrelative mass production. As a representative example, the followingdescribes a method of manufacturing when using a water atomizing method.
    [31] [0031] It suffices for the chemical composition of molten steel beingatomized to have iron as the principal component. However, since a largequantity of oxide-based inclusions might be generated at the time of atomizing,the content of oxidizable metal elements (Al, Si, Mn, Cr, and the like) ispreferably low. The following contents are preferable: Al S 0.01 mass%, Si S0.03 mass%, Mn S 0.1 mass%, and Cr S 0.05 mass%. Of course, the content of oxidizable metal elements other than those listed above is also preferably reduced insofar as possible.
    [32] [0032] The atomized powder is then subjected to decarburization andreduction annealing. The annealing is preferably high-load treatmentperformed in a reductive atmosphere including hydrogen. For example, one ormultiple stages of heat treatment is preferably performed in a reductiveatmosphere including hydrogen, at a temperature of 700 °C or more to lessthan 1200 °C, preferably 900 °C or more to less than ll00 °C, with a holdingtime of l h to 7 h, preferably 2 h to 5 h. The grain size in the powder is thuscoarsened. The dew point in the atmosphere is not limited and may be set inaccordance with the C content included in the atomized powder.
    [33] [0033] After reduction annealing, the powder is subject to the first crushing.The apparent density is thus set to 3.8 g/cm3 or more. After the first crushing,annealing is performed in hydrogen at 600 °C to 850 °C to remove strain inthe iron powder. The reason for performing the annealing at 600 °C to 850 °Cis in order to set the micro Vickers hardness ofthe powder cross-section to 90Hv or less. After strain removal, the powder is crushed, avoiding theapplication of strain insofar as possible. After crushing, the particle sizedistribution is adjusted by sieve classification using sieves prescribed in JIS Z880l-l so that the apparent density and mean particle size fall within theranges of our powder.
    [34] [0034] Furthermore, an insulation coating is applied to the above-describediron powder, which is then formed into a dust core.
    [35] [0035] After applying an insulation coating to the particle surface with such amethod, the resulting iron-based powder is injected in a die and pressureformed to a shape with desired dimensions (dust core shape) to yield a dustcore. The pressure formation method may be any regular formation method,such as cold molding, die lubrication molding, or the like. The compactingpressure may be determined in accordance with use. If the compactingpressure is increased, however, the green density increases. Hence, a compacting pressure of 10 t/cmz (981 MN/mz) or more is preferable, with l5 _10- t/cmz (1471 MN/mz) or more being more preferable.
    [36] [0036] At the time of the above-described pressure formation, as necessary, alubricant may be applied to the die walls or added to the powder. At the timeofpressure formation, the friction between the die and the powder can thus bereduced, thereby suppressing a reduction in the green density. Furthermore,the friction upon removal from the die can also be reduced, effectivelypreventing cracks in the green compact (dust core) at the time of removal.Preferable lubricants in this case include metallic soaps such as lithiumstearate, zinc stearate, and calcium stearate, and waxes such as fatty acidamide.
    [37] [0037] The dust core thus formed is subjected, after pressure formation, toheat treatment in order to reduce hysteresis loss via strain relief and toincrease the green compact strength. The heat treatment time of this heattreatment is preferably approximately 5 min to 120 min. Any ofthe followingmay be used without any problem as the heating atmosphere: the regularatmosphere, an inert atmosphere, a reductive atmosphere, or a vacuum. Theatmospheric dew point may be determined appropriately in accordance withuse. Furthermore, when raising or lowering the temperature during heattreatment, a stage at which the temperature is maintained constant may be provided.
    [39] [0039] [Tabie 1] Table 1Ratio of powder witha gram size of 80 um MicroNo. of Appafent or more among . .. d . D50 . Inclus1ons Vickers1ron GUSIW powder with a 0 Notes3 (um) _ _ ( A5) hardnesspowder (g/Cm ) part1c1e size of 100 (HV)um or more(%) 1 4.3 98.6 100 0.38 85 Example 2 4.2 102.4 86.2 0.24 80 Example 3 4. 3 98. 6 62. 0 0.26 82 Examplc 4 4.2 102.2 65.0 0.21 83 Examplc 5 4. 4 104.5 70. 8 0.18 78 Examplc 6 4.4 106.4 95.0 0.39 100 CompamtweExample 7 4.1 39.0 45.0 0.37 37 CompamtweExample 3 3.2 95.0 62.0 0.26 76 CompamnveExample 9 3.3 75.5 60.1 0.37 35 CompamtweExample 10 3.9 160.0 100 0.57 34 CompamnveExample
    [40] [0040] An insulation coating was applied to these powders using siliconeresin. The silicone resin was dissolved in toluene to produce a resin dilutesolution such that the resin component is 0.9 mass%. The powder and the resindilute solution were then mixed so that the rate of addition of the resin withrespect to the powder became 0.15 mass%. The result was then dried in theatmosphere. After drying, a resin baking process was performed in theatmosphere at 200 °C for 120 min to yield coated iron-based soft magneticpowders. These powders were then formed using die lubrication at acompacting pressure of 15 t/cmz (1471 MN/mz) to produce ring-shaped testpieces with an outer diameter of 38 mm, an inner diameter of 25 mm, and aheight of 6 mm.
    [41] [0041] The samples after iron loss measurement Were dissected, and the grainsize Was measured. Since dissected samples maintain the grain size in a greencompact cross-section, the grain size in a green compact cross-section Wasmeasured With the following method.
    [42] [0042] [Table 2] Table 2No. of green No. of iron Green compact. . Notescompact sample powder used gram size (pm)1 1 27.0 Example2 2 29.7 Example3 3 28.7 Example4 4 27.9 Example5 5 33.6 Example6 6 19. 9 ComparativeExample7 7 21. 2 ComparativeExample8 8 12. 1 ComparativeExample9 9 17. 7 ComparativeExampleComparative10 10 19.0Example
    [43] [0043] Table 2 shows that the largest grain size in the Comparative ExamplesWas 21.2 pm, Whereas in the Examples, the smallest grain size Was 27.0 pm,and the largest Was 33.6 pm.
    [44] [0044] [Tabie 3] Table 3Sample NO' Oíllron Hysteresis Eddy current Iron loss NotesN6. POW d” 1655 (W/kg) 1655 (W/kg) (w/kg)use 1 1 23.1 3.7 26. 8 Example 2 2 20.6 3.8 24.4 Example 3 3 21.1 3.8 24.9 Example 4 4 20.2 3.9 24. 1 Example 5 5 19.6 4.2 23.8 Example 6 6 27.1 4.9 32.0 CompamtweExample 7 7 27.1 3.1 30.2 ComparatweExample 8 8 31.2 unmeasurable unmeasurable ComparatweExample 9 9 23.4 2.6 31.0 CompamtweExample 10 10 32.3 7.0 39.3 ComparatweExample
    [45] [0045] Table 3 shows that as compared to the Comparative Examples, thehysteresis loss was kept lower in all ofthe Examples, thereby keeping the ironloss low and satisfying the acceptance criterion for iron loss in all of theabove Examples.
    [46] [0046] It is also clear that for both the Examples and the ComparativeExamples, every sample with an apparent density of 3.8 g/cm3 or more had aneddy current loss of less than 10 W/kg. This shows that by only covering withsilicone resin, the insulation between particles was maintained even afterstrain relief annealing at 650 °C, and that the increase in apparent density was effective for reducing both hysteresis loss and eddy current loss.
    权利要求:
    Claims (2)
    [1] 1. l. An iron powder for dust cores comprising iron as a principalcomponent, wherein the iron powder is an atomized powder, and has anapparent density of 3.8 g/cm3 or more and a mean particle size (D50) of 80 timor more, 60 % or more of powder with a powder particle size of 100 tim ormore has a mean grain size of 80 tim or more inside the powder particle, anarea ratio of an inclusion to a matrix phase of the powder is 0.4 % or less, anda micro Vickers hardness (testing force: 0.245 N) of a powder cross-section is90 HV or less.
    [2] 2. The iron powder for dust cores of claim l, wherein 70 % ormore ofthe powder with the powder particle size of 100 tim or more has the mean grain size of 80 tim or more inside the powder particle.
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    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    JPH08921B2|1992-06-19|1996-01-10|株式会社神戸製鋼所|Pure iron powder for powder metallurgy with excellent compressibility and magnetic properties|
    JP2005187918A|2003-12-26|2005-07-14|Jfe Steel Kk|Insulating coated iron powder for powder compact magnetic core|
    JP4457682B2|2004-01-30|2010-04-28|住友電気工業株式会社|Powder magnetic core and manufacturing method thereof|
    JP4305222B2|2004-03-05|2009-07-29|住友電気工業株式会社|Method for producing a green compact|
    SE0401042D0|2004-04-21|2004-04-21|Hoeganaes Ab|Lubricants for metallurgical powder compositions|
    JP2006024869A|2004-07-09|2006-01-26|Toyota Central Res & Dev Lab Inc|Dust core and manufacturing method thereof|
    JP2007092162A|2005-02-03|2007-04-12|Jfe Steel Kk|Highly compressive iron powder, iron powder for dust core using the same and dust core|
    JP4701797B2|2005-04-04|2011-06-15|Ｊｆｅスチール株式会社|Coated iron-based powder for dust core and dust core|
    JP4630251B2|2006-09-11|2011-02-09|株式会社神戸製鋼所|Powder cores and iron-based powders for dust cores|
    WO2008093430A1|2007-01-30|2008-08-07|Jfe Steel Corporation|High-compressibility iron powder, iron powder comprising the same for dust core, and dust core|
    JP5263653B2|2007-04-04|2013-08-14|日立金属株式会社|Powder magnetic core and manufacturing method thereof|
    JP5206648B2|2009-11-16|2013-06-12|Ｊｆｅスチール株式会社|Soft magnetic metal powder for dust core and dust core|
    JP4957859B2|2010-08-31|2012-06-20|Ｊｆｅスチール株式会社|Iron powder for seed coating and seed|
    JP5438669B2|2010-12-28|2014-03-12|株式会社神戸製鋼所|Iron-based soft magnetic powder for dust core and dust core|
    JP5565453B2|2012-12-19|2014-08-06|Ｊｆｅスチール株式会社|Iron powder for dust core|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    JP2013088720A|JP5929819B2|2013-04-19|2013-04-19|Iron powder for dust core|
    PCT/JP2014/001559|WO2014171065A1|2013-04-19|2014-03-18|Iron powder for dust core|
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