WO2016056351A1 - 軟磁性材料粉末及びその製造方法、並びに、磁心及びその製造方法 - Google Patents
軟磁性材料粉末及びその製造方法、並びに、磁心及びその製造方法 Download PDFInfo
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- WO2016056351A1 WO2016056351A1 PCT/JP2015/075945 JP2015075945W WO2016056351A1 WO 2016056351 A1 WO2016056351 A1 WO 2016056351A1 JP 2015075945 W JP2015075945 W JP 2015075945W WO 2016056351 A1 WO2016056351 A1 WO 2016056351A1
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Definitions
- the present invention relates to a soft magnetic material powder used for a magnetic core and a method for producing the same.
- the present invention also relates to a magnetic core using this soft magnetic powder and a method for manufacturing the same.
- magnetic cores used in transformers and coils used are required to have characteristics such as high permeability at high frequencies and low eddy current loss. Yes. For this reason, the magnetic core is required to have a high resistance so as to have a low eddy current loss in a high frequency band.
- a magnetic core for example, there is a powder magnetic core formed by compressing and molding a magnetic material as fine particle powder and covering the surface of each particle with an insulating coating.
- the resistance value can be greatly increased, and the eddy current loss can be remarkably reduced.
- a compacting powder having a metal alkoxide and a mineral containing crystal water on the surface of the soft magnetic metal particles, and compressing the compacting powder to obtain a temporary compact, and then annealing.
- a manufacturing method is known in which a metal alkoxide is hydrolyzed to form an insulating coating on the surface of soft magnetic metal particles to obtain a compacted body (see, for example, Patent Document 2).
- the magnetic material powder described in Patent Document 1 has good insulation and a thin inorganic film is formed on the surface of the metal magnetic powder.
- the flowability during dust molding is poor and the magnetic permeability of the dust core does not increase.
- fine cracks are generated in the inorganic film during dust molding, the resistance value decreases during annealing, and eddy current loss occurs. There is a problem that becomes larger.
- An object of the present invention is to provide a soft magnetic material powder that can obtain a sufficient density, high magnetic permeability, and a magnetic core having high electrical resistance.
- the soft magnetic material powder according to the present invention includes a core made of an Fe-based soft magnetic material, An insulating film covering the surface of the core; Have The insulating film includes soft magnetic material particles containing an inorganic oxide and a water-soluble polymer.
- the soft magnetic material powder according to the present invention when molded into a magnetic core, a sufficient density as a soft magnetic material can be obtained, the magnetic permeability of the magnetic core can be increased, and the soft magnetic material contained in the soft magnetic material powder A magnetic core having high electric resistance can be obtained by the insulating film of the particles and the binder.
- FIG. 3 is an enlarged cross-sectional view showing a fine cross-sectional structure of soft magnetic material particles contained in the soft magnetic material powder according to Embodiment 1.
- FIG. 2 is an enlarged cross-sectional view showing a fine cross-sectional structure of a magnetic core according to Embodiment 1.
- FIG. It is the schematic which shows the analysis location which performed the composition analysis on the line from the core of the soft-magnetic material particle which comprises the cross-section of the magnetic core of FIG. 2, to an insulating film, and a binder. It is a graph which shows the composition analysis result on the line of FIG. It is a graph which shows the relationship between the specific resistance measured with the high resistance measuring device, and the applied voltage.
- the soft magnetic material powder according to the first aspect includes a core made of an Fe-based soft magnetic material, An insulating film covering the surface of the core; Have The insulating film includes soft magnetic material particles containing an inorganic oxide and a water-soluble polymer.
- the soft magnetic material powder according to a second aspect is the above first aspect, wherein the water-soluble polymer is selected from the group consisting of polyvinylpyrrolidone, polyethyleneimine, carboxymethylcellulose, gelatin, polyacrylic acid, polyethylene glycol, and polyvinyl alcohol. It may be at least one selected.
- the water-soluble polymer may be polyvinyl pyrrolidone in the first aspect, and may be included in a range of 0.01 wt% to 1 wt%.
- the soft magnetic material powder according to a fourth aspect is any one of the first to third aspects, wherein the inorganic oxide is at least selected from the group consisting of TiO 2 , SiO 2 , Al 2 O 3 , and ZrO. There may be one.
- the inorganic oxide may be polysiloxane.
- the inorganic oxide is SiO 2 and is contained in a range of 0.01 wt% to 5 wt%. May be.
- the soft magnetic material powder according to the sixth aspect is any one of the first to fifth aspects, and the Fe-based soft magnetic material is selected from the group consisting of Fe, FeNi, FeCo, FeSi, FeSiCr, FeSiAl, and FeSiBCr. It may be at least one selected.
- the method for producing a soft magnetic material powder according to the seventh aspect comprises dispersing Fe-based soft magnetic powder in a solvent, A metal alkoxide and a water-soluble polymer are added to the solvent to hydrolyze the metal alkoxide, and a hydrolyzate of the metal alkoxide is formed on the surface of the soft magnetic material particles constituting the Fe-based soft magnetic powder. An insulating film containing a certain metal oxide and the water-soluble polymer is formed to insulate the soft magnetic material particles.
- a magnetic core according to an eighth aspect includes the soft magnetic material powder according to any one of the first to sixth aspects.
- the magnetic core according to the ninth aspect comprises soft magnetic material particles, A binder that binds the soft magnetic material particles; Including a magnetic core, The soft magnetic material particles are A core containing an Fe-based soft magnetic material; An insulating film covering the surface of the core; Have The insulating film contains an inorganic oxide and a water-soluble polymer.
- a magnetic core according to a tenth aspect includes soft magnetic material particles, A binder that binds the soft magnetic material particles; Including a magnetic core, The soft magnetic material particles are A core made of Fe-based soft magnetic material; An insulating film containing Si covering the surface of the core; Have The Fe-based soft magnetic material includes Fe and Cr, The insulating film contains an inorganic oxide containing more Si than Cr.
- a method of manufacturing a magnetic core according to an eleventh aspect includes mixing the soft magnetic material powder according to any one of the first to sixth aspects and a thermosetting resin as a binder to form a mixture, The mixture is heat-cured to obtain a magnetic core.
- a method for manufacturing a magnetic core according to a twelfth aspect includes mixing the soft magnetic material powder according to any one of the first to sixth aspects and a thermosetting resin as a binder to form a mixture, The mixture is heated to cure the thermosetting resin and then annealed to obtain a magnetic core.
- An electronic component according to a thirteenth aspect includes the magnetic core according to any one of the eighth to tenth aspects.
- FIG. 1 is a cross-sectional view showing a cross-sectional structure of soft magnetic material particles 10 included in the soft magnetic material powder according to the first embodiment.
- the soft magnetic material particle 10 includes a core 1 containing an Fe-based soft magnetic material and an insulating film 2 that covers the surface of the core 1.
- the insulating film 2 contains an inorganic oxide and a water-soluble polymer.
- the raw material of the insulating film 2 contains the water-soluble polymer together with the inorganic oxide, the thin insulating film 2 can be obtained.
- the insulating film 2 since a flexible water-soluble polymer is present in the insulating film 2, stress during compression molding can be relieved, so that molding can be performed at a low pressure. As a result, the insulating film 2 of the soft magnetic material particles contained in the soft magnetic material powder is not cracked even during compression molding when the magnetic core is manufactured. That is, according to this soft magnetic material powder, the compression moldability is good.
- the average particle diameter of the core 1 containing the Fe-based soft magnetic material of the soft magnetic material particles 10 constituting the soft magnetic material powder is, for example, in the range of 0.1 ⁇ m to 100 ⁇ m.
- the thickness of the insulating film 2 of the soft magnetic material particles 10 is, for example, in the range of 5 nm to 100 nm, preferably in the range of 20 nm to 40 nm. The thickness was measured with a transmission electron microscope (TEM). Specifically, the thickness of the insulating film 2 at five locations is measured and averaged with respect to an observation image of five fields of view at 100,000 to 200,000 times with a transmission electron microscope using a sample obtained by processing a thin piece of a magnetic core. Thus, the thickness of the insulating film 2 was obtained.
- TEM transmission electron microscope
- Fe-based soft magnetic material used for the core 1, for example, Fe and an alloy containing Fe can be used.
- the alloy containing Fe is, for example, various Fe-based magnetic metals conventionally used such as FeNi, FeCo, FeSi, FeSiCr, FeSiAl, and FeSiBCr.
- the soft magnetic material may further contain impurities.
- the insulating film 2 contains an inorganic oxide and a water-soluble polymer.
- the metal species M constituting the inorganic oxide at least one kind can be selected from Li, Na, Mg, Al, Si, K, Ca, Ti, Cu, Sr, Y, Zr, Ba, Ce, Ta, and Bi. .
- Si, Ti, Al, and Zr are suitable from the strength of the obtained oxide and the specific resistivity.
- This metal species M is a metal of a metal alkoxide used for forming the insulating film 2.
- Specific inorganic oxides are preferably SiO 2 , TiO 2 , Al 2 O 3 , and ZrO. SiO 2 is particularly preferred. Further, the inorganic oxide is contained in the range of 0.01 wt% to 5 wt% with respect to the soft magnetic material powder.
- the water-soluble polymer is selected from at least one of polyethyleneimine, polyvinyl pyrrolidone, polyethylene glycol, sodium polyacrylate, carboxymethyl cellulose, polyvinyl alcohol, and gelatin, or a combination of two or more thereof.
- the water-soluble polymer is contained in the range of 0.01 wt% to 1 wt% with respect to the soft magnetic material powder.
- Method for producing soft magnetic material powder A method for producing the soft magnetic material powder will be described below.
- An insulating film containing a metal oxide that is a hydrolyzate of metal alkoxide and a water-soluble polymer is formed on the surface of the soft magnetic material particles constituting the Fe-based soft magnetic material powder.
- the soft magnetic material powder containing the insulated soft magnetic material particles can be obtained.
- Fe-based soft magnetic material is the same as described above, and a description thereof is omitted.
- solvent As the solvent, alcohols such as methanol and ethanol may be used.
- the metal species M of the metal alkoxide having the form of M-OR to be added includes Li, Na, Mg, Al, Si, K, Ca, Ti, Cu, Sr, Y, Zr, Ba, Ce, Ta, and Bi. At least one type can be selected. Note that, for example, Si, Ti, Al, and Zr are suitable from the strength of the obtained oxide and the specific resistivity. Further, as the alkoxy group OR of the metal alkoxide, an arbitrary group such as a methoxy group, an ethoxy group, or a propoxy group can be selected. Two or more metal alkoxides may be combined.
- an acidic catalyst for example, hydrochloric acid, acetic acid, phosphoric acid, a basic catalyst, for example, ammonia, sodium hydroxide, piperidine, or a salt catalyst, for example Ammonium carbonate and ammonium acetate may be added.
- the dispersion after stirring may be dried by an appropriate method (oven, spray, vacuum, etc.).
- the drying temperature may be, for example, a temperature range of 50 ° C. or higher and 300 ° C. or lower.
- the drying time can be appropriately set. For example, it may be in the range of 10 minutes to 24 hours.
- FIG. 2 is an enlarged cross-sectional view showing the configuration of the magnetic core (dust core) 20 according to the first embodiment.
- the dust core 20 has a structure in which the insulating film 2 and the binder 12 surround the Fe-based soft magnetic material 1 derived from the core of the soft magnetic material particles 10 constituting the soft magnetic material powder. ing.
- This insulating film 2 has an inorganic oxide and a water-soluble polymer contained in the insulating film 2 of the soft magnetic material particles 10 contained in the soft magnetic material powder.
- the binder 12 consists of a binder added at the time of dust core manufacture.
- the water-soluble polymer may be lost from the insulating film 2, or the water-soluble polymer may be decomposed by thermal decomposition, evaporation or volatilization of the water-soluble polymer. Some or all may be lost.
- the soft magnetic material 1 is separated by the insulating film 2 and the binder 12. ing. A high electrical resistance can be maintained by the insulating film 2 and the binder 12 without causing cracks in the insulating film 2 of soft magnetic material particles. As a result, the effect of low eddy current loss can be achieved. Further, since the insulating film 2 of the soft magnetic material particles 10 included in the soft magnetic material powder is thin, the insulating film 2 can be thinned even in the dust core 20. As a result, the soft magnetic material 1 can have a high density and a high magnetic permeability can be obtained.
- This magnetic core may be used for electronic parts such as coil parts and inductors.
- the magnetic core may be a member around which a coiled conductor is wound in a coil component.
- the magnetic core may be a member in which a coiled conductor is disposed inside the coil component.
- the coiled conductor may be a coiled winding, or a patterned conductor formed in a coiled shape.
- the soft magnetic material 1 is substantially the same as the Fe-based soft magnetic material, description thereof is omitted.
- the insulating film 2 is derived from the insulating film 2 of the soft magnetic material particles 10 contained in the soft magnetic material powder. That is, the insulating film 2 contains an inorganic oxide and a water-soluble polymer. However, the insulating film 2 of the magnetic core (hereinafter also referred to as “annealing type magnetic core”) formed by heat annealing may not contain a water-soluble polymer, and the insulating film 2 of the annealing type magnetic core contains inorganic oxide.
- the object may contain an oxide of Fe in addition to the oxide of the metal species M described above.
- the inorganic oxide included in the insulating film 2 of the annealed magnetic core using an alloy containing Fe and Cr or Al as a soft magnetic material is an oxide of the metal species M and oxidation of Fe. In addition to the above materials, it may further contain Cr oxide or Al oxide.
- the binder 12 is a binder added at the time of manufacturing the dust core.
- the binder 12 is not particularly limited as long as it is a thermosetting resin.
- an epoxy resin, an imide resin, a silicon resin, a fluorine resin, or the like can be used. These may be selected singly or in combination of two or more thereof.
- the insulating film 2 and the binder 12 separate the soft magnetic materials 1 from each other.
- thermosetting resin used as the binder is not particularly limited, and examples thereof include an epoxy resin, an imide resin, a silicon resin, and a fluorine resin. These are selected from one or a combination of two or more thereof.
- the curing agent for curing the thermosetting resin is not particularly limited, and phenol resin, polyamine, imidazole and the like can be used.
- the binder may be added in a range of 1 wt% to 6 wt% with respect to 100 wt% of the dust core.
- glass frit or a silane coupling agent can also be used.
- a mold may be used during compression molding.
- the density of the soft magnetic material can be increased by performing compression molding. Note that compression molding is not essential, and may be performed as necessary.
- a magnetic core obtained by compression molding is called a dust core.
- a magnetic core not subjected to compression molding is also simply called a magnetic core.
- the term “magnetic core” widely includes the entire magnetic core regardless of compression molding.
- the powder magnetic core is annealed at a temperature of 400 ° C. or higher. Specifically, for example, the annealing treatment may be performed by heat treatment in an atmosphere of N 2 or N 2 + H 2 in the temperature range of 400 ° C. to 900 ° C., and further in the temperature range of 600 ° C. to 900 ° C.
- a silicon resin is preferable as the binder for the heat annealing treatment.
- a magnetic core can be obtained.
- a magnetic core that has been annealed at 400 ° C. or higher is called, for example, an annealed magnetic core.
- a magnetic core that is not annealed is called, for example, a heat-hardening type magnetic core.
- the core 1 including the Fe-based soft magnetic material as described above, the insulating film 2 covering the surface of the core 1 and including the inorganic oxide and the water-soluble polymer,
- the soft magnetic material powder containing the soft magnetic material particles 10 having the above is used. Since a soft water-soluble polymer is present in the insulating film 2 of the soft magnetic material particles 10, stress during compression molding can be relieved, so that molding can be performed with low pressure. As a result, the insulating film 2 of the soft magnetic material particles 10 contained in the soft magnetic material powder is not cracked and the insulating film 2 and the binder 12 are not broken even during the dust molding during the production of the dust core. As a result, in this dust core, high resistance can be realized, and the effect of low eddy current loss can be achieved.
- Example 1-19 and Comparative Example 1-3 will be described with reference to Tables 1 and 2.
- Table 1 shows the manufacturing conditions of the soft magnetic material powder and the dust core
- Table 2 shows the measured values and evaluation results.
- Example 1 ⁇ Insulation treatment of soft magnetic material powder> A method for producing the soft magnetic material powder according to Example 1 will be described.
- polyvinyl pyrrolidone is weighed so as to be 0.1 wt% with respect to 100 wt% of the Fe-based soft magnetic material, dissolved in 3.2 g of pure water, and added in ethanol to which FeSiCr powder is added. It was dripped. Stir and mix for 60 minutes. In this way, an insulating-treated soft magnetic material powder (with an insulating film formed) was obtained.
- FIG. 3 is a schematic view showing an analysis location where a composition analysis is performed on the line from the core of the soft magnetic material particles constituting the cross-sectional structure of the magnetic core of FIG. 2 to the insulating film and the binder.
- FIG. 4 is a graph showing the composition analysis results on the line of FIG.
- the composition analysis of the cross-sectional structure of the magnetic core was performed as follows. First, about the test piece which performed the heat annealing process, about the surface perpendicular
- FIG. 5 is a graph showing the relationship between the specific resistance measured by the high resistance measuring instrument and the applied voltage.
- IR insulation resistance
- Comparative Example 1 IR (insulation resistance) dropped when 900 V was applied. From this test, it was found that Examples 1 and 2 according to the present invention can provide a magnetic core with high voltage resistance that can withstand 900 V application.
- the soft magnetic material powder according to Example 1 was able to create a dust core with a low molding pressure (4 t / cm 2 ).
- the obtained dust core had a high relative magnetic permeability (39) and a high specific resistance (6.0 ⁇ 10 11 ⁇ ⁇ cm) even after heat annealing.
- the soft magnetic material powder according to Example 1 contained more Si than Cr in the obtained insulating film 2.
- the soft magnetic material powder according to the first embodiment is made of an Fe-based soft magnetic material, and includes a core 1 containing Cr and an insulating film 2 containing Si covering the surface of the core 1.
- the insulating film 2 contains an inorganic oxide containing more Si than Cr. From this analysis result, it is considered that a magnetic core having a high withstand voltage can be obtained when the insulating film 2 contains more Si than Cr in comparison with Example 1 and Comparative Example 1.
- Example 2 As shown in Table 1, the soft magnetic material was the same as in Example 1 except that the addition amount of tetraethylorthosilicate, which is a metal alkoxide (Example 2: 0.01 wt%, Example 3: 5 wt%) was changed. Powders and dust cores were prepared and measured and evaluated. ⁇ Action and effect> As shown in Table 2, a dust core could be produced at a low molding pressure (4 t / cm 2 ) as in Example 1.
- the obtained powder magnetic core has a high relative permeability (Example 2: 39, Example 3: 39), and the specific resistance (Example 2: 1.0 ⁇ 10 11 ⁇ ⁇ cm, Example 3: 3.5 ⁇ 10 11 ⁇ ⁇ cm) was high.
- Example 4 soft magnetism was the same as in Example 1 except that the addition amount of the water-soluble polymer polyvinylpyrrolidone (Example 4: 0.01 wt%, Example 5: 1 wt%) was changed.
- Material powders and dust cores were prepared and measured and evaluated. ⁇ Action and effect> As shown in Table 2, a dust core could be produced at a low molding pressure (4 t / cm 2 ) as in Example 1. Further, the obtained dust core has a high relative permeability (Example 4: 37, Example 5: 33), and the specific resistance (Example 4: 1.8 ⁇ 10 11 ⁇ ⁇ cm, Example 5: 4.3 ⁇ 10 11 ⁇ ⁇ cm) was high.
- Example 6 As shown in Table 1, the type of water-soluble polymer used (Example 6: Polyethyleneimine, Example 7: Carboxymethylcellulose, Example 8: Gelatin, Example 9: Polyacrylic acid, Example 10: Polyethylene glycol
- Example 11 A soft magnetic material powder and a dust core were prepared, and measured and evaluated in the same manner as in Example 1 except that polyvinyl alcohol) was changed. ⁇ Action and effect> As shown in Table 2, a dust core could be produced at a low molding pressure (4 t / cm 2 ) as in Example 1. The obtained dust core has a relative permeability (Example 6: 35, Example 7: 36, Example 8: 38, Example 9: 36, Example 10: 35, Example 11: 37).
- Example 6 High and specific resistance even after heat annealing (Example 6: 3.9 ⁇ 10 11 ⁇ ⁇ cm, Example 7: 4.5 ⁇ 10 11 ⁇ ⁇ cm, Example 8: 3.4 ⁇ 10 11 ⁇ ⁇ cm, Example 9: 5.4 ⁇ 10 11 ⁇ ⁇ cm, Example 10: 3.0 ⁇ 10 11 ⁇ ⁇ cm, Example 11: 3.4 ⁇ 10 11 ⁇ ⁇ cm) there were.
- Example 12 As shown in Table 1, except that the type of metal alkoxide used (Example 12: Aluminum isopropoxide, Example 13: Titanium tetraisopropoxide, Example 14: Zirconium-n-butoxide)
- a soft magnetic material powder and a dust core were prepared in the same manner as in Example 1 and measured and evaluated.
- a dust core could be produced at a low molding pressure (4 t / cm 2 ) as in Example 1. Further, the obtained dust core has a high relative magnetic permeability (Example 12:37, Example 13:38, Example 14:36), and has a specific resistance (Example 12: 6. 4 ⁇ 10 11 ⁇ ⁇ cm, Example 13: 4.2 ⁇ 10 11 ⁇ ⁇ cm, and Example 14: 7.4 ⁇ 10 11 ⁇ ⁇ cm) were high.
- Example 15 As shown in Table 1, a soft magnetic material powder and a dust core were prepared, measured and evaluated in the same manner as in Example 1 except that the heat annealing treatment was not performed. ⁇ Action and effect> As shown in Table 2, according to the dust core according to Example 15, it can be produced at a low molding pressure, and a high specific permeability (30) and a high specific resistance (6. 0 ⁇ 10 13 ⁇ ⁇ cm) was obtained.
- Example 16 to 17 As shown in Table 1, the soft magnetic material was the same as in Example 15 except that the amount of addition of tetraethylorthosilicate as a metal alkoxide (Example 16: 0.01 wt%, Example 17: 5 wt%) was changed. Powders and dust cores were prepared and measured and evaluated. ⁇ Action and effect> As shown in Table 2, similar to Example 15, it can be produced at a low molding pressure, and has a high relative magnetic permeability (Examples 16:31 and 17:30) and high without performing a heat annealing treatment. Specific resistance (Example 16: 5.0 ⁇ 10 13 ⁇ ⁇ cm, Example 17: 4.8 ⁇ 10 13 ⁇ ⁇ cm) was obtained.
- Example 18 As shown in Table 1, soft magnetism was the same as in Example 15 except that the addition amount of the water-soluble polymer polyvinylpyrrolidone (Example 18: 0.01 wt%, Example 19: 1 wt%) was changed. Material powders and dust cores were prepared and measured and evaluated. ⁇ Action and effect> As shown in Table 2, like Example 15, it can be produced at a low molding pressure, and has a high relative magnetic permeability (Examples 18:31, Example 19:30) and high without performing a heat annealing treatment. Specific resistance (Example 18: 1.9 ⁇ 10 13 ⁇ ⁇ cm, Example 19: 3.8 ⁇ 10 13 ⁇ ⁇ cm) was obtained.
- Comparative Examples 1 and 2 As shown in Table 1, in Comparative Example 1, the magnetic powder that was not subjected to insulation treatment was granulated in the same manner as in Example 1, and then heated at 150 ° C. and compacted at a molding pressure of 8 t / cm 2. Created a magnetic core. In Comparative Example 2, a soft magnetic material powder and a powder magnetic core were prepared in the same manner as in Example 1 except that polyvinylpyrrolidone as a water-soluble polymer was not added.
- FeSiCr is used as the magnetic material.
- the present invention is not limited to this, and other Fe-based magnetic materials may be used.
- the temperature of the heat annealing treatment is not limited to 720 ° C., and the heat annealing treatment may be performed as long as the temperature range is 400 ° C. or more and 900 ° C. or less, and the temperature range is 600 ° C. or more and 900 ° C. or less.
- the present disclosure includes appropriately combining any of the various embodiments described above, and can provide the effects of the respective embodiments.
- the soft magnetic material powder according to the present invention a sufficient density as a soft magnetic material can be obtained, high magnetic permeability can be obtained, and the soft magnetic material powder contains a high insulating film and a binder. Since a magnetic core having an electric resistance and a high withstand voltage can be obtained, it is useful as a soft magnetic material powder for a magnetic core.
- Soft magnetic material 1
- Insulating film 10
- Soft magnetic material particles 12
- Binder 20 Powder magnetic core
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Abstract
Description
前記コアの表面を被覆する絶縁膜と、
を有し、
前記絶縁膜には無機酸化物と水溶性高分子とを含有する、軟磁性材料粒子を含む。
前記コアの表面を被覆する絶縁膜と、
を有し、
前記絶縁膜には無機酸化物と水溶性高分子とを含有する、軟磁性材料粒子を含む。
前記溶媒中に金属アルコキシド及び水溶性高分子を添加して、前記金属アルコキシドを加水分解させ、前記Fe系の軟磁性粉末を構成する軟磁性材料粒子の表面に、前記金属アルコキシドの加水分解物である金属酸化物と前記水溶性高分子とを含む絶縁膜を形成して軟磁性材料粒子を絶縁処理する。
前記各軟磁性材料粒子を結合する結合剤と、
を含む磁心であって、
前記軟磁性材料粒子は、
Fe系の軟磁性材料を含むコアと、
前記コアの表面を被覆する絶縁膜と、
を有し、
前記絶縁膜には無機酸化物と水溶性高分子とを含有する。
前記各軟磁性材料粒子を結合する結合剤と、
を含む磁心であって、
前記軟磁性材料粒子は、
Fe系の軟磁性材料からなるコアと、
前記コアの表面を被覆するSiを含む絶縁膜と、
を有し、
前記Fe系の軟磁性材料は、Fe及びCrを含み、
前記絶縁膜にはCrよりSiを多く含む無機酸化物を含有する。
前記混合物を加熱硬化して磁心を得る。
前記混合物を加熱して前記熱硬化性樹脂を硬化させたのち、焼鈍処理して磁心を得る。
<軟磁性材料粉末>
図1は、実施の形態1に係る軟磁性材料粉末に含まれる軟磁性材料粒子10の断面構造を示す断面図である。この軟磁性材料粒子10は、Fe系の軟磁性材料を含むコア1と、コア1の表面を被覆する絶縁膜2とを有する。絶縁膜2は、無機酸化物と水溶性高分子とを含む。
この軟磁性材料粉末では、絶縁膜2の原料が無機酸化物と共に水溶性高分子を含むので、薄い絶縁膜2を得ることができる。さらに、絶縁膜2中に柔軟な水溶性高分子が存在することによって、圧縮成型時の応力を緩和できるので、低い圧力で成型できる。その結果、磁心の製造時の圧縮成型時にも軟磁性材料粉末に含まれる軟磁性材料粒子の絶縁膜2のひび割れを生じない。つまり、この軟磁性材料粉末によれば、圧縮成型性がよい。
コア1に用いるFe系の軟磁性材料としては、例えば、Fe、及び、Feを含む合金を用いることができる。Feを含む合金とは、たとえば、FeNi、FeCo、FeSi、FeSiCr、FeSiAl、FeSiBCr等の従来から用いられているFe系の各種磁性金属である。軟磁性材料は、さらに不純物を含んでいてもよい。
絶縁膜2は、無機酸化物と水溶性高分子とを含む。
<無機酸化物>
無機酸化物を構成する金属種Mとしては、Li、Na、Mg、Al、Si、K、Ca、Ti、Cu、Sr、Y、Zr、Ba、Ce、Ta、Biから少なくとも一種類を選択できる。なお、例えば、得られる酸化物の強度と固有の比抵抗から、Si、Ti、Al、Zrが好適である。この金属種Mは、絶縁膜2を形成するのに用いられる金属アルコキシドの金属である。具体的な無機酸化物としては、SiO2、TiO2、Al2O3、ZrOが好ましい。SiO2が特に好ましい。
また、無機酸化物は、軟磁性材料粉末に対し0.01wt%以上5wt%以下の範囲で含まれている。
水溶性高分子としては、ポリエチレンイミン、ポリビニルピロリドン、ポリエチレングリコール、ポリアクリル酸ナトリウム、カルボキシメチルセルロース、ポリビニルアルコール、ゼラチンから少なくとも一種類、またはその二種類以上の組み合わせから選択される。
水溶性高分子は、軟磁性材料粉末に対し0.01wt%以上1wt%以下の範囲で含まれている。
この軟磁性材料粉末の製造方法について以下に説明する。
(1)溶媒中にFe系の軟磁性材料粉末を分散させる。
(2)溶媒中に金属アルコキシド及び水溶性高分子を添加して撹拌する。
このとき、金属アルコキシドが加水分解される。Fe系の軟磁性材料粉末を構成する軟磁性材料粒子の表面に、金属アルコキシドの加水分解物である金属酸化物と水溶性高分子とを含む絶縁膜を形成する。
以上によって、絶縁処理した軟磁性材料粒子を含む軟磁性材料粉末を得ることができる。
Fe系の軟磁性材料としては、上記と同様であり、説明を省略する。
溶媒としては、メタノール、エタノール等のアルコール類を用いてもよい。
添加するM-ORの形態をもつ金属アルコキシドの金属種Mとしては、Li、Na、Mg、Al、Si、K、Ca、Ti、Cu、Sr、Y、Zr、Ba、Ce、Ta、Biから少なくとも一種類を選択できる。なお、例えば、得られる酸化物の強度と固有の比抵抗から、Si、Ti、Al、Zrが好適である。
また、金属アルコキシドのアルコキシ基ORとしては、メトキシ基、エトキシ基、プロポキシ基など、任意のものを選択できる。
また、金属アルコキシドは二種類以上を組み合わせてもよい。
撹拌した後の分散液を適宜の方法(オーブン、スプレー、真空中など)で乾燥させてもよい。乾燥温度は、例えば50℃以上300℃以下の温度範囲であってよい。乾燥時間は、適宜設定できる。例えば、10分以上24時間以下の範囲であってよい。
図2は、実施の形態1に係る磁心(圧粉磁心)20の構成を示す拡大断面図である。この圧粉磁心20は、軟磁性材料粉末を構成する軟磁性材料粒子10のコアに由来するFe系の軟磁性材料1の周囲を絶縁膜2と結合剤12とが取り囲むような構造で構成されている。この絶縁膜2には、軟磁性材料粉末に含まれる軟磁性材料粒子10の絶縁膜2に含まれていた無機酸化物及び水溶性高分子を有する。結合剤12は、圧粉磁心製造時に添加される結合剤からなる。
なお、加熱焼鈍処理の温度によっては、絶縁膜2から水溶性高分子の官能基等の一部が失われる場合や、あるいは、水溶性高分子の熱分解、蒸発又は揮発によって水溶性高分子の一部又は全体が失われる場合もある。
軟磁性材料1は、上記Fe系の軟磁性材料と実質的に同じであるので説明を省略する。
絶縁膜2は、軟磁性材料粉末に含まれる軟磁性材料粒子10の絶縁膜2に由来する。つまり、絶縁膜2は、無機酸化物及び水溶性高分子を含む。但し、加熱焼鈍を行って形成された磁心(以下、焼鈍型磁心とも言う)の絶縁膜2は、水溶性高分子を含まないことがある、また、焼鈍型磁心の絶縁膜2が含む無機酸化物は、上述の金属種Mの酸化物に加え、Feの酸化物を含むことがある。また、軟磁性材料としてFeとCrまたはAlを含む合金(たとえば、FeSiCr、FeSiBCr、FeSiAl)を用いた焼鈍型磁心の絶縁膜2が含む無機酸化物は、金属種Mの酸化物及びFeの酸化物に加え、さらに、Crの酸化物又はAlの酸化物を含むことがある。
結合剤12は、圧粉磁心製造時に添加される結合剤である。結合剤12は、熱硬化性樹脂であればよく、特に限定されないが、例えば、エポキシ樹脂、イミド樹脂、シリコン樹脂、フッ素樹脂などを用いることができる。これらは単独、またはその二種類以上の組み合わせから選択されしてもよい。この絶縁膜2と結合剤12とによって軟磁性材料1同士が隔てられている。
次に、圧粉磁心の製造方法について以下に説明する。
(1)得られた絶縁被膜処理された軟磁性材料粉末は、エタノールで洗浄した後、結合剤となる熱硬化性樹脂と混合し、圧縮成型し、その後、熱硬化性樹脂を加熱硬化させる。加熱硬化の温度は、10℃以上400℃未満であってよい。なお、軟磁性材料粉末と結合剤とを混合した後、造粒を行ってもよい。結合剤となる熱硬化性樹脂は、特に限定されないが、例えば、エポキシ樹脂、イミド樹脂、シリコン樹脂、フッ素樹脂などがあげられる。これらは単独、またはその二種類以上の組み合わせから選択される。熱硬化性樹脂を硬化させる硬化剤は特に限定されるものではなく、フェノール樹脂、ポリアミン、イミダゾール等を使用できる。結合剤は、圧粉磁心100wt%に対して、1wt%以上6wt%以下の範囲で添加してもよい。また、圧粉磁心の強度を上げるために、ガラスフリットやシランカップリング剤を用いることもできる。さらに、圧縮成型時には金型を用いてもよい。圧縮成形を行うことによって軟磁性材料の密度を高くすることができる。なお、圧縮成形は必須ではなく、必要により行えばよい。圧縮成形を行って得られた磁心を圧粉磁心という。一方、圧縮成形を行わなかった磁心も単に磁心と呼ばれる。ここでは、「磁心」という場合には圧縮成形の有無を問わず、広く磁心全体を含むものとする。
(2)圧粉磁心について、磁心損失を低減させるために加熱硬化させた圧粉磁心について加熱焼鈍処理を行ってもよい。磁心損失は周波数に依存するため、使用する圧粉磁心の周波数帯域によっては焼鈍処理を省略することもできる。必要に応じて圧粉磁心を400℃以上の温度で焼鈍処理を行う。焼鈍処理は、具体的には、例えば、400℃以上900℃以下の温度範囲、さらに600℃以上900℃以下の温度範囲の大気中、N2あるいはN2+H2雰囲気で熱処理してもよい。加熱焼鈍処理する場合の結合剤はシリコン樹脂が好ましい。
以上によって、磁心を得ることができる。400℃以上の焼鈍処理を行った磁心は、例えば、焼鈍型磁心と呼ばれる。一方、焼鈍処理を行わない磁心は、例えば、加熱硬化型磁心と呼ばれる。
表1に軟磁性材料粉末及び圧粉磁心の製造条件を示し、表2に各測定値及び評価結果を示した。
<軟磁性材料粉末の絶縁処理>
実施例1に係る軟磁性材料粉末の製造方法について説明する。
(a)37.2gのエタノール中に軟磁性材料として平均粒径30μmのFeSiCr粉を20g添加する。
(b)次に、テトラエチルオルソシリケートをSiO2換算でFe系の軟磁性材料100wt%に対して1wt%になるように秤量し、FeSiCr粉が添加されたエタノール中に添加して撹拌した。
(c)さらに、Fe系の軟磁性材料100wt%に対して0.1wt%になるようにポリビニルピロリドンを秤量し、3.2gの純水に溶解させて、FeSiCr粉が添加されたエタノール中に滴下した。60分間にわたって撹拌混合した。
以上によって、絶縁処理された(絶縁膜が形成された)軟磁性材料粉末を得た。
次に、得られた絶縁処理された軟磁性材料粉末を用いた圧粉磁心の作成について説明する。
(1)得られた絶縁処理された軟磁性材料粉末500gと、結合剤としてのシリコン樹脂20.9gと、を混合し、4t/cm2の圧力で内径4mm、外径9mm、厚さ1mmのトロイダルリングを作成した。また同様に4t/cm2の圧力で3mm×3mm×1mmの試験片を作成した。
(2)次いで、トロイダルリングと試験片を200℃、1時間加熱した(硬化処理)。
(3)さらに、一部のトロイダルリングと試験片を大気中雰囲気下で720℃、50分間加熱した(加熱焼鈍処理)。
(4)その後、RFインピーダンスアナライザー(Agilent E4991A)で1MHzの際のトロイダルリングの透磁率を測定した。また、高抵抗測定器(Advantest R8340A ULTRA HIGH RESISTANCE METER)により900Vの電圧を試験片の3mm間に5秒間かけて比抵抗を測定した。
測定した透磁率から求めた比透磁率が30以上、かつ比抵抗が108Ω・cm以上を満たす場合を○(適合)とし、いずれか一方でも上記基準を満たさない場合は×(不適合)として評価した。
<耐電圧試験>
図5は、上記高抵抗測定器によって測定した比抵抗と印加電圧との関係を示すグラフである。実施例1、2では、900VをかけてもIR(絶縁抵抗)が落ちなかった。一方、比較例1では、900Vをかけると、IR(絶縁抵抗)が落ちた。
この試験より、本発明に係る実施例1、2では、900V印加時にも耐えられる耐電圧性の高い磁心を提供できることがわかった。
表2に示すように、実施例1に係る軟磁性材料粉末は、低い成型圧力(4t/cm2)で圧粉磁心を作成できた。また得られた圧粉磁心は、比透磁率(39)が高く、また加熱焼鈍処理しても比抵抗(6.0×1011Ω・cm)が高いものであった。また、図4で得られたライン分析の結果から、実施例1に係る軟磁性材料粉末は、得られた絶縁膜2中にはCr以上にSiが多く含まれていた。実施例1に係る軟磁性材料粉末は、Fe系の軟磁性材料からなり、Crを含むコア1と、コア1の表面を被覆するSiを含む絶縁膜2と、を有する。さらに、絶縁膜2にはCrよりSiを多く含む無機酸化物を含有する。
この分析結果から、実施例1と比較例1との対比から、絶縁膜2にCrよりSiを多く含むことにより耐電圧性が高い磁心が得られると考えられる。
表1の示すように、金属アルコキシドであるテトラエチルオルソシリケートの添加量(実施例2:0.01wt%、実施例3:5wt%)を変えたこと以外は、実施例1と同様に軟磁性材料粉末及び圧粉磁心を作成し、測定及び評価を行った。
<作用・効果>
表2に示すように、実施例1と同様に低い成型圧力(4t/cm2)で圧粉磁心を作成できた。また得られた圧粉磁心は、比透磁率(実施例2:39、実施例3:39)が高く、また加熱焼鈍処理しても比抵抗(実施例2:1.0×1011Ω・cm、実施例3:3.5×1011Ω・cm)が高いものであった。
表1に示すように、水溶性高分子であるポリビニルピロリドンの添加量(実施例4:0.01wt%、実施例5:1wt%)を変えたこと以外は、実施例1と同様に軟磁性材料粉末及び圧粉磁心を作成し、測定及び評価を行った。
<作用・効果>
表2に示すように、実施例1と同様に低い成型圧力(4t/cm2)で圧粉磁心を作成できた。また得られた圧粉磁心は、比透磁率(実施例4:37、実施例5:33)が高く、また加熱焼鈍処理しても比抵抗(実施例4:1.8×1011Ω・cm、実施例5:4.3×1011Ω・cm)が高いものであった。
表1に示すように、使用する水溶性高分子の種類(実施例6:ポリエチレンイミン、実施例7:カルボキシメチルセルロース、実施例8:ゼラチン、実施例9:ポリアクリル酸、実施例10:ポリエチレングリコール、実施例11:ポリビニルアルコール)を変えたこと以外は、実施例1と同様に軟磁性材料粉末及び圧粉磁心を作成し、測定及び評価を行った。
<作用・効果>
表2に示すように、実施例1と同様に低い成型圧力(4t/cm2)で圧粉磁心を作成できた。また得られた圧粉磁心は、比透磁率(実施例6:35、実施例7:36、実施例8:38、実施例9:36、実施例10:35、実施例11:37)が高く、また加熱焼鈍処理しても比抵抗(実施例6:3.9×1011Ω・cm、実施例7:4.5×1011Ω・cm、実施例8:3.4×1011Ω・cm、実施例9:5.4×1011Ω・cm、実施例10:3.0×1011Ω・cm、実施例11:3.4×1011Ω・cm)が高いものであった。
表1に示すように、使用する金属アルコキシドの種類(実施例12:アルミニウムイソプロポキシド、実施例13:チタンテトライソプロポキシド、実施例14:ジルコニウム-n-ブトキシド)を変えたこと以外は、実施例1と同様に軟磁性材料粉末及び圧粉磁心を作成し、測定及び評価を行った。
<作用・効果>
表2に示すように、実施例1と同様に低い成型圧力(4t/cm2)で圧粉磁心を作成できた。また得られた圧粉磁心は、比透磁率(実施例12:37、実施例13:38、実施例14:36)が高く、また加熱焼鈍処理しても比抵抗(実施例12:6.4×1011Ω・cm、実施例13:4.2×1011Ω・cm、実施例14:7.4×1011Ω・cm)が高いものであった。
表1に示すように、加熱焼鈍処理を行わなかったこと以外は、実施例1と同様に軟磁性材料粉末及び圧粉磁心を作成し、測定及び評価を行った。
<作用・効果>
表2に示すように、実施例15に係る圧粉磁心によれば、低い成型圧力で作成可能であり、加熱焼鈍処理を行わなくても高い比透磁率(30)および高い比抵抗(6.0×1013Ω・cm)が得られた。
表1に示すように、金属アルコキシドであるテトラエチルオルソシリケートの添加量(実施例16:0.01wt%、実施例17:5wt%)を変えたこと以外は、実施例15と同様に軟磁性材料粉末及び圧粉磁心を作成し、測定及び評価を行った。
<作用・効果>
表2に示すように、実施例15と同様に、低い成型圧力で作成可能であり、加熱焼鈍処理を行わなくても高い比透磁率(実施例16:31、実施例17:30)および高い比抵抗(実施例16:5.0×1013Ω・cm、実施例17:4.8×1013Ω・cm)が得られた。
表1に示すように、水溶性高分子であるポリビニルピロリドンの添加量(実施例18:0.01wt%、実施例19:1wt%)を変えたこと以外は、実施例15と同様に軟磁性材料粉末及び圧粉磁心を作成し、測定及び評価を行った。
<作用・効果>
表2に示すように、実施例15と同様に、低い成型圧力で作成可能であり、加熱焼鈍処理を行わなくても高い比透磁率(実施例18:31、実施例19:30)および高い比抵抗(実施例18:1.9×1013Ω・cm、実施例19:3.8×1013Ω・cm)が得られた。
表1に示すように、比較例1では、絶縁処理を行わなかった磁性粉末を用い、実施例1と同様に造粒した後、150℃に加熱しながら8t/cm2の成型圧力で圧粉磁心を作成した。
比較例2では、水溶性高分子としてのポリビニルピロリドンを添加しなかったこと以外は、実施例1と同様に軟磁性材料粉末及び圧粉磁心を作成した。
表1及び表2に示すように、比較例1によれば、高い比透磁率(39)の圧粉磁心が得られるが、高い成型圧力(8t/cm2)と温間成型が必要であり、また軟磁性材料粉末の絶縁処理をしていないので加熱焼鈍処理後の比抵抗(1.5×105Ω・cm)が低くなった。
比較例2では、相対的に低い比透磁率(20)の圧粉磁心しか得られなかった。また加圧成型時に、絶縁膜に微細なクラックが入り、比抵抗(4.2×107Ω・cm)が低下した。
2 絶縁膜
10 軟磁性材料粒子
12 結合剤
20 圧粉磁心
Claims (13)
- Fe系の軟磁性材料を含むコアと、
前記コアの表面を被覆する絶縁膜と、
を有し、
前記絶縁膜には無機酸化物と水溶性高分子とを含有する、軟磁性材料粒子を含む、軟磁性材料粉末。 - 前記水溶性高分子は、ポリビニルピロリドン、ポリエチレンイミン、カルボキシメチルセルロース、ゼラチン、ポリアクリル酸、ポリエチレングリコール、ポリビニルアルコールからなる群から選ばれる少なくとも一つである、請求項1に記載の軟磁性材料粉末。
- 前記水溶性高分子は、ポリビニルピロリドンであり、Fe系の軟磁性材料100wt%に対して0.01wt%以上1wt%以下の範囲で含まれている、請求項1に記載の軟磁性材料粉末。
- 前記無機酸化物は、TiO2、SiO2、Al2O3、ZrOからなる群から選ばれる少なくとも一つである、請求項1から3のいずれか一項に記載の軟磁性材料粉末。
- 前記無機酸化物は、SiO2であり、Fe系の軟磁性材料100wt%に対して0.01wt%以上5wt%以下の範囲で含まれている、請求項1から3のいずれか一項に記載の軟磁性材料粉末。
- 前記Fe系の軟磁性材料は、Fe、FeNi、FeCo、FeSi、FeSiCr、FeSiAl、FeSiBCrの群から選ばれる少なくとも一つである、請求項1から5のいずれか一項に記載の軟磁性材料粉末。
- 溶媒中にFe系の軟磁性粉末を分散させ、
前記溶媒中に金属アルコキシド及び水溶性高分子、水を添加して撹拌し、前記Fe系の軟磁性粉末を構成する軟磁性材料粒子の表面に、前記金属アルコキシドの加水分解物である金属酸化物と前記水溶性高分子とを含む絶縁膜を形成して軟磁性材料粒子を絶縁処理する、
軟磁性材料粉末の製造方法。 - 請求項1から6のいずれか一項に記載の前記軟磁性材料粉末を含む磁心。
- 軟磁性材料粒子と、
前記各軟磁性材料粒子を結合する結合剤と、
を含む磁心であって、
前記軟磁性材料粒子は、
Fe系の軟磁性材料を含むコアと、
前記コアの表面を被覆する絶縁膜と、
を有し、
前記絶縁膜には無機酸化物と水溶性高分子とを含有する、磁心。 - 軟磁性材料粒子と、
前記各軟磁性材料粒子を結合する結合剤と、
を含む磁心であって、
前記軟磁性材料粒子は、
Fe系の軟磁性材料からなるコアと、
前記コアの表面を被覆するSiを含む絶縁膜と、
を有し、
前記Fe系の軟磁性材料は、Fe及びCrを含み、
前記絶縁膜にはCrよりSiを多く含む無機酸化物を含有する、磁心。 - 請求項1から6のいずれか一項に記載の前記軟磁性材料粉末と結合剤である熱硬化性樹脂とを混合して混合物を形成し、
前記混合物の熱硬化性樹脂を加熱硬化して磁心を得る、
磁心の製造方法。 - 請求項1から6のいずれか一項に記載の前記軟磁性材料粉末と結合剤である熱硬化性樹脂とを混合して混合物を形成し、
前記混合物を加熱して前記熱硬化性樹脂を硬化させたのち、焼鈍処理して磁心を得る、
磁心の製造方法。 - 請求項8から10のいずれか一項に記載の前記磁心を含む電子部品。
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WO2017150610A1 (ja) * | 2016-03-03 | 2017-09-08 | Ntn株式会社 | 圧粉磁心用造粒粉及びその製造方法 |
JP2018011043A (ja) * | 2016-06-30 | 2018-01-18 | 太陽誘電株式会社 | 磁性材料及び電子部品 |
WO2020171178A1 (ja) * | 2019-02-22 | 2020-08-27 | アルプスアルパイン株式会社 | 圧粉磁心およびその製造方法 |
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JPWO2021020402A1 (ja) * | 2019-07-29 | 2021-02-04 | ||
JP7475352B2 (ja) | 2019-07-29 | 2024-04-26 | 株式会社村田製作所 | 軟磁性粉末およびその製造方法、軟磁性粉末を用いたコイル部品ならびに軟磁性粉末を用いた磁性体材料の製造方法 |
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US11965229B2 (en) | 2020-03-27 | 2024-04-23 | Murata Manufacturing Co., Ltd. | Metal magnetic particle, inductor, method for manufacturing metal magnetic particle, and method for manufacturing metal magnetic core |
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CN106233401B (zh) | 2019-08-13 |
JPWO2016056351A1 (ja) | 2017-04-27 |
KR20170009928A (ko) | 2017-01-25 |
CN106233401A (zh) | 2016-12-14 |
US10825590B2 (en) | 2020-11-03 |
US10685768B2 (en) | 2020-06-16 |
TW201618133A (zh) | 2016-05-16 |
US20200258664A1 (en) | 2020-08-13 |
TWI605478B (zh) | 2017-11-11 |
US20170162307A1 (en) | 2017-06-08 |
KR101881246B1 (ko) | 2018-07-23 |
US11965117B2 (en) | 2024-04-23 |
US20210054218A1 (en) | 2021-02-25 |
JP6436172B2 (ja) | 2018-12-12 |
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