JP5682741B2 - SOFT MAGNETIC PARTICLE POWDER AND PROCESS FOR PRODUCING THE SAME, - Google Patents
SOFT MAGNETIC PARTICLE POWDER AND PROCESS FOR PRODUCING THE SAME, Download PDFInfo
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- JP5682741B2 JP5682741B2 JP2008223884A JP2008223884A JP5682741B2 JP 5682741 B2 JP5682741 B2 JP 5682741B2 JP 2008223884 A JP2008223884 A JP 2008223884A JP 2008223884 A JP2008223884 A JP 2008223884A JP 5682741 B2 JP5682741 B2 JP 5682741B2
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- 239000006249 magnetic particle Substances 0.000 title claims description 78
- 238000000034 method Methods 0.000 title description 5
- 239000000843 powder Substances 0.000 claims description 185
- 239000003607 modifier Substances 0.000 claims description 91
- 150000002484 inorganic compounds Chemical class 0.000 claims description 78
- 229910010272 inorganic material Inorganic materials 0.000 claims description 78
- 239000002923 metal particle Substances 0.000 claims description 55
- 239000002245 particle Substances 0.000 claims description 51
- 238000010438 heat treatment Methods 0.000 claims description 19
- 239000011248 coating agent Substances 0.000 claims description 18
- 238000000576 coating method Methods 0.000 claims description 18
- 238000004519 manufacturing process Methods 0.000 claims description 16
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 229910052782 aluminium Inorganic materials 0.000 claims description 10
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- 239000011246 composite particle Substances 0.000 claims description 8
- 239000000696 magnetic material Substances 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 229910052726 zirconium Inorganic materials 0.000 claims description 8
- 238000000748 compression moulding Methods 0.000 claims description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- 229940125898 compound 5 Drugs 0.000 claims description 4
- 230000005389 magnetism Effects 0.000 claims description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 3
- 229910052684 Cerium Inorganic materials 0.000 claims description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- 239000011575 calcium Substances 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 239000011162 core material Substances 0.000 description 47
- 239000010410 layer Substances 0.000 description 32
- 230000007797 corrosion Effects 0.000 description 29
- 238000005260 corrosion Methods 0.000 description 29
- 239000000428 dust Substances 0.000 description 23
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 22
- 229910052751 metal Inorganic materials 0.000 description 18
- 239000002184 metal Substances 0.000 description 18
- -1 polysiloxane Polymers 0.000 description 15
- 229920001296 polysiloxane Polymers 0.000 description 13
- 239000006247 magnetic powder Substances 0.000 description 12
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- 230000000052 comparative effect Effects 0.000 description 6
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- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 229910052742 iron Inorganic materials 0.000 description 6
- 239000007822 coupling agent Substances 0.000 description 5
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
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- 238000003756 stirring Methods 0.000 description 4
- 230000000007 visual effect Effects 0.000 description 4
- 239000006087 Silane Coupling Agent Substances 0.000 description 3
- UMHKOAYRTRADAT-UHFFFAOYSA-N [hydroxy(octoxy)phosphoryl] octyl hydrogen phosphate Chemical compound CCCCCCCCOP(O)(=O)OP(O)(=O)OCCCCCCCC UMHKOAYRTRADAT-UHFFFAOYSA-N 0.000 description 3
- 150000004645 aluminates Chemical class 0.000 description 3
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
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- 229910017060 Fe Cr Inorganic materials 0.000 description 2
- 229910002544 Fe-Cr Inorganic materials 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
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- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- UPHIPHFJVNKLMR-UHFFFAOYSA-N chromium iron Chemical compound [Cr].[Fe] UPHIPHFJVNKLMR-UHFFFAOYSA-N 0.000 description 2
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- XEJNLUBEFCNORG-UHFFFAOYSA-N ditridecyl hydrogen phosphate Chemical compound CCCCCCCCCCCCCOP(O)(=O)OCCCCCCCCCCCCC XEJNLUBEFCNORG-UHFFFAOYSA-N 0.000 description 2
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- 239000000314 lubricant Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 150000003961 organosilicon compounds Chemical class 0.000 description 2
- 229910000889 permalloy Inorganic materials 0.000 description 2
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- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 229910000702 sendust Inorganic materials 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 238000004876 x-ray fluorescence Methods 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- KKYDYRWEUFJLER-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,5,5,6,6,7,7,10,10,10-heptadecafluorodecyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)CCC(F)(F)F KKYDYRWEUFJLER-UHFFFAOYSA-N 0.000 description 1
- 125000000022 2-aminoethyl group Chemical group [H]C([*])([H])C([H])([H])N([H])[H] 0.000 description 1
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 description 1
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
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- 229910000676 Si alloy Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 239000007983 Tris buffer Substances 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- FVQVTTMDOISRDX-UHFFFAOYSA-J [Zr+4].CCC(C([O-])=O)C(=O)C(CC)(CC)CC.CCC(C([O-])=O)C(=O)C(CC)(CC)CC.CCC(C([O-])=O)C(=O)C(CC)(CC)CC.CCC(C([O-])=O)C(=O)C(CC)(CC)CC Chemical compound [Zr+4].CCC(C([O-])=O)C(=O)C(CC)(CC)CC.CCC(C([O-])=O)C(=O)C(CC)(CC)CC.CCC(C([O-])=O)C(=O)C(CC)(CC)CC.CCC(C([O-])=O)C(=O)C(CC)(CC)CC FVQVTTMDOISRDX-UHFFFAOYSA-J 0.000 description 1
- WDJHALXBUFZDSR-UHFFFAOYSA-M acetoacetate Chemical compound CC(=O)CC([O-])=O WDJHALXBUFZDSR-UHFFFAOYSA-M 0.000 description 1
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- VSSMJHUOAAZQMT-UHFFFAOYSA-N butanedioic acid;1-octylsulfonyloctane Chemical compound OC(=O)CCC(O)=O.CCCCCCCCS(=O)(=O)CCCCCCCC VSSMJHUOAAZQMT-UHFFFAOYSA-N 0.000 description 1
- XGZGKDQVCBHSGI-UHFFFAOYSA-N butyl(triethoxy)silane Chemical compound CCCC[Si](OCC)(OCC)OCC XGZGKDQVCBHSGI-UHFFFAOYSA-N 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
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- BAAAEEDPKUHLID-UHFFFAOYSA-N decyl(triethoxy)silane Chemical compound CCCCCCCCCC[Si](OCC)(OCC)OCC BAAAEEDPKUHLID-UHFFFAOYSA-N 0.000 description 1
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- ZZNQQQWFKKTOSD-UHFFFAOYSA-N diethoxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](OCC)(OCC)C1=CC=CC=C1 ZZNQQQWFKKTOSD-UHFFFAOYSA-N 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
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- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 description 1
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- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 1
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 description 1
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- PYGSKMBEVAICCR-UHFFFAOYSA-N hexa-1,5-diene Chemical group C=CCCC=C PYGSKMBEVAICCR-UHFFFAOYSA-N 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 150000003949 imides Chemical class 0.000 description 1
- XWHPIFXRKKHEKR-UHFFFAOYSA-N iron silicon Chemical compound [Si].[Fe] XWHPIFXRKKHEKR-UHFFFAOYSA-N 0.000 description 1
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 1
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- CAQIWIAAHXOQOS-UHFFFAOYSA-N octadecanoic acid;propan-2-ol;titanium Chemical compound [Ti].CC(C)O.CCCCCCCCCCCCCCCCCC(O)=O.CCCCCCCCCCCCCCCCCC(O)=O.CCCCCCCCCCCCCCCCCC(O)=O CAQIWIAAHXOQOS-UHFFFAOYSA-N 0.000 description 1
- MSRJTTSHWYDFIU-UHFFFAOYSA-N octyltriethoxysilane Chemical compound CCCCCCCC[Si](OCC)(OCC)OCC MSRJTTSHWYDFIU-UHFFFAOYSA-N 0.000 description 1
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- BPCXHCSZMTWUBW-UHFFFAOYSA-N triethoxy(1,1,2,2,3,3,4,4,5,5,8,8,8-tridecafluorooctyl)silane Chemical compound CCO[Si](OCC)(OCC)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)CCC(F)(F)F BPCXHCSZMTWUBW-UHFFFAOYSA-N 0.000 description 1
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- Powder Metallurgy (AREA)
- Soft Magnetic Materials (AREA)
Description
本発明は、耐食性及び耐熱性に優れた絶縁層を有する軟磁性粒子粉末、該軟磁性粒子粉末の製造法、並びに該軟磁性粒子粉末を含有する、耐食性に優れた高温で焼成した場合においても比抵抗値が低下しにくい圧粉磁心を提供する。 The present invention provides a soft magnetic particle powder having an insulating layer excellent in corrosion resistance and heat resistance, a method for producing the soft magnetic particle powder, and a case where the soft magnetic particle powder contains the soft magnetic particle powder and is fired at a high temperature excellent in corrosion resistance. Provided is a dust core in which the specific resistance value is unlikely to decrease.
近年、家電及び電子機器の省エネルギー化及び小型化に伴い、これらに使用される磁心材料に対しても、小型で高出力、且つ電力変換効率の高効率化の要求が強まっている。機器サイズの小型化、高出力化及び電力変換効率の高効率化には動作周波数の高周波化が有効であることが知られており、高周波領域においても高い磁束密度及び低鉄損を有する磁心材料が強く求められている。 In recent years, along with energy saving and miniaturization of home appliances and electronic devices, there is an increasing demand for miniaturization, high output, and high efficiency of power conversion efficiency for magnetic core materials used for these. Higher operating frequency is known to be effective in reducing the size of equipment, increasing output, and increasing power conversion efficiency. Magnetic core materials have high magnetic flux density and low iron loss even in the high frequency range. Is strongly demanded.
一般に、磁心材料の鉄損の主要因としては、ヒステリシス損と渦電流損が知られている。渦電流損が作動周波数の２乗に比例するのに対して、ヒステリシス損は作動周波数の１乗に比例するため、従来のように作動周波数が数百Ｈｚ以下の帯域ではヒステリシス損が支配的であり、この周波数帯域においては、ヒステリシス損が小さいケイ素鋼板を用いた積層型磁心等が使用されている。しかしながら、積層型磁心は動作周波数が高くなるに従って、磁心内部で発生する渦電流損失が増大するという欠点を有している。 In general, hysteresis loss and eddy current loss are known as main causes of iron loss of magnetic core materials. The eddy current loss is proportional to the square of the operating frequency, whereas the hysteresis loss is proportional to the square of the operating frequency. Therefore, the hysteresis loss is dominant in the band where the operating frequency is several hundred Hz or less as in the conventional case. In this frequency band, a laminated magnetic core using a silicon steel sheet having a small hysteresis loss is used. However, the laminated magnetic core has a drawback that eddy current loss generated inside the magnetic core increases as the operating frequency increases.
そのため、近年の小型で高出力の要求に対しては、積層型磁心に比べて高周波領域での鉄損が低いと共に成形性に優れた、粉末状の軟磁性粉末をフェノール樹脂やエポキシ樹脂等の絶縁性樹脂で被覆し圧縮成形した圧粉磁心が、積層型磁心の代替品として広く用いられている。 Therefore, in response to the recent demands for small size and high output, powdered soft magnetic powders with low iron loss in the high frequency region and excellent moldability compared with laminated magnetic cores, such as phenol resin and epoxy resin, etc. A dust core coated with an insulating resin and compression-molded is widely used as an alternative to a laminated core.
一般的に、軟磁性粉末としては、鉄、鉄−ケイ素合金、センダスト合金、パーマロイ合金及び鉄系非晶質合金等に代表される、飽和磁束密度の高いＦｅ基合金の粉末が用いられているが、成分組成的に酸化しやすく耐食性に問題があった。 Generally, as a soft magnetic powder, an Fe-based alloy powder having a high saturation magnetic flux density, such as iron, iron-silicon alloy, Sendust alloy, permalloy alloy, and iron-based amorphous alloy, is used. However, it is easy to oxidize in terms of composition and has a problem in corrosion resistance.
また、上記軟磁性粉末を用いた圧粉磁心を搭載する製品の使用環境も厳しくなっており、圧粉磁心としての耐食性も重要となってきている。 In addition, the use environment of products equipped with a powder magnetic core using the soft magnetic powder has become severe, and corrosion resistance as a powder magnetic core has become important.
一方、圧粉磁心に対して、更なる小型化及び高性能化、即ち、高磁束密度化が望まれており、このような高磁束密度化のために、軟磁性粉末の充填密度を増大させることが行われている。 On the other hand, further miniaturization and higher performance, that is, higher magnetic flux density is desired for the powder magnetic core. For such higher magnetic flux density, the packing density of the soft magnetic powder is increased. Things have been done.
しかしながら、軟磁性粉末を高充填するために高圧で圧縮成形を行うため、軟磁性粉末には歪みが残り、ヒステリシス損の増大を招くことが知られている。そのため、歪みによるヒステリシス損を低減することを目的として、通常、成形品に対して熱処理（焼鈍し）による歪みの除去が行われており、熱処理時の温度を高く設定すれば歪み除去の効果は大きくなり、ヒステリシス損を低減させることができる。 However, it is known that since compression molding is performed at a high pressure in order to highly fill the soft magnetic powder, strain remains in the soft magnetic powder, leading to an increase in hysteresis loss. Therefore, for the purpose of reducing the hysteresis loss due to distortion, distortion is usually removed from the molded product by heat treatment (annealing). If the temperature during heat treatment is set high, the effect of distortion removal is This increases the hysteresis loss.
上記熱処理は、一般には５００℃以上、好ましくは６００℃、もしくはそれ以上の温度が効果的であるとされているが、熱処理時の温度を高く設定しすぎると、軟磁性粉末のバインダーとしての結合樹脂や上記粒子間の絶縁のために絶縁性樹脂を使用した場合、樹脂が分解したり劣化したりして、成形体が脆くなると共に、絶縁性が低下してしまうため渦電流損が増大する原因となる。従って、このような問題が生じることのない温度範囲でしか熱処理を行なうことができず、ヒステリシス損と渦電流損の両方を同時に低減することは困難であった。 The above heat treatment is generally effective at a temperature of 500 ° C. or higher, preferably 600 ° C. or higher, but if the temperature during the heat treatment is set too high, the soft magnetic powder is bound as a binder. When an insulating resin is used for insulation between the resin and the particles, the resin is decomposed or deteriorated, the molded body becomes brittle, and the insulating property is lowered, so that eddy current loss increases. Cause. Therefore, heat treatment can be performed only in a temperature range where such a problem does not occur, and it has been difficult to simultaneously reduce both hysteresis loss and eddy current loss.
これまでに、耐食性に優れた軟磁性粉末として、特定量のＣｒとＳｉ、Ａｌのうち一つ以上の元素を含有するＦｅ基金属磁性粉末（特許文献１）及び非晶質磁性合金粉末と結晶質Ｆｅ−Ｃｒ系合金粉末を混合した磁性材料粉末（特許文献２）が開示されている。 To date, as soft magnetic powders excellent in corrosion resistance, Fe-based metal magnetic powders (Patent Document 1) containing one or more elements of a specific amount of Cr, Si, and Al, and amorphous magnetic alloy powders and crystals Magnetic material powder (Patent Document 2) in which a high quality Fe-Cr alloy powder is mixed is disclosed.
また、Ｆｅ基軟磁性合金粉末を空気中で８０℃以上の温度で熱処理することにより、粉体表層の不動態膜を強固にする方法（特許文献３）が開示されている。 Further, a method (Patent Document 3) is disclosed in which an Fe-based soft magnetic alloy powder is heat-treated in air at a temperature of 80 ° C. or higher to strengthen the passive film on the powder surface layer.
また、軟磁性粉末の耐酸化性等を改善することを目的として、軟磁性粒子粉末の粒子表面にケイ素からなる無機化合物及びリンからなる無機化合物、又は前記無機化合物の複合体を付着もしくは被覆させた複合粒子粉末（特許文献４）が開示されている。 For the purpose of improving the oxidation resistance of the soft magnetic powder, the surface of the soft magnetic particle powder is adhered or coated with an inorganic compound composed of silicon and an inorganic compound composed of phosphorus, or a composite of the inorganic compound. Composite particle powder (Patent Document 4) is disclosed.
また、圧縮性及び流動性に優れると共に、高温で焼成した場合においても電気抵抗値の変化が少ない軟磁性材料を得ることを目的として、軟磁性粒子粉末の粒子表面が表面改質剤によって被覆されていると共に該被覆に無機化合物が付着している複合粒子粉末（特許文献５）が開示されている。 In addition, the surface of the soft magnetic particle powder is coated with a surface modifier for the purpose of obtaining a soft magnetic material that is excellent in compressibility and fluidity and has little change in electrical resistance even when fired at high temperatures. In addition, a composite particle powder (Patent Document 5) in which an inorganic compound is adhered to the coating is disclosed.
耐食性及び耐熱性に優れた絶縁層を有する軟磁性粒子粉末及び高温で焼成した場合においても比抵抗値が低下しにくい圧粉磁心は、現在最も要求されているところであるが、未だ得られていない。 A soft magnetic particle powder having an insulating layer excellent in corrosion resistance and heat resistance, and a dust core whose specific resistance value is difficult to decrease even when fired at a high temperature are currently most demanded, but have not yet been obtained. .
即ち、特許文献１及び２には、特定量のＣｒとＳｉ、Ａｌのうち一つ以上の元素を含有するＦｅ基金属磁性粉末あるいは非晶質磁性合金粉末と結晶質Ｆｅ−Ｃｒ系合金粉末を混合した磁性材料粉末が記載されているが、いずれの特許文献にも合金粉末表面に耐熱性及び耐食性を付与するための絶縁層を形成することは考慮されていないため、高温（６００℃以上）で焼鈍しを行うと絶縁性が低下してしまったり、高温多湿な環境下での使用によって錆が発生したりするなどの問題を有している。 That is, Patent Documents 1 and 2 include Fe-based metal magnetic powder or amorphous magnetic alloy powder and crystalline Fe-Cr alloy powder containing one or more elements of a specific amount of Cr, Si, and Al. Although mixed magnetic material powders are described, any patent document does not consider the formation of an insulating layer for imparting heat resistance and corrosion resistance to the surface of the alloy powder. When annealing is carried out, there are problems such as deterioration of insulation and rust generated by use in a hot and humid environment.
また、特許文献３には、Ｆｅ基軟磁性合金粉末を空気中で８０℃以上の温度で熱処理することにより、粉体表層の不動態膜を強固にする方法が開示されているが、軟磁性合金粉末表層を酸化させるため、軟磁性合金粉末の非磁性層の増加により軟磁性合金粉末の磁気特性を低下させてしまうと共に、軟磁性合金粉末の流動性や磁性粉の密度を低下させてしまう可能性があり、これを用いて圧粉磁心を形成した際に、圧粉磁心における軟磁性合金粉末の割合が減少するため、高磁束密度化が困難となる。 Patent Document 3 discloses a method of strengthening a passive film on the powder surface layer by heat-treating Fe-based soft magnetic alloy powder in air at a temperature of 80 ° C. or higher. Because the surface layer of the alloy powder is oxidized, an increase in the nonmagnetic layer of the soft magnetic alloy powder decreases the magnetic properties of the soft magnetic alloy powder, and also decreases the fluidity of the soft magnetic alloy powder and the density of the magnetic powder. There is a possibility, and when a powder magnetic core is formed using this, the proportion of the soft magnetic alloy powder in the powder magnetic core is reduced, so that it is difficult to increase the magnetic flux density.
また、特許文献４には、軟磁性金属粒子粉末の粒子表面にケイ素からなる無機化合物及びリンからなる無機化合物、又は前記無機化合物の複合体を付着もしくは被覆させた複合粒子粉末が開示されているが、リン酸系の絶縁被膜は高温で変質してしまうため、６００℃以上の温度での加熱処理は困難である。また、軟磁性金属粉末表面への絶縁層の形成を有機溶剤中で行うことが記載されているが、有機溶剤中にも０．５〜５％程度の水分が含まれており、更にリン酸は水溶液として用いられているため、水分によって軟磁性金属粉末が酸化・腐食し易く磁気特性が劣化すると共に酸化被膜が厚くなるため、これを用いて圧粉磁心を形成した際に圧粉磁心における軟磁性金属粉末の割合が減少するため、高磁束密度化が困難となる。 Patent Document 4 discloses a composite particle powder in which an inorganic compound made of silicon and an inorganic compound made of phosphorus, or a composite of the inorganic compound is attached to or coated on the particle surface of the soft magnetic metal particle powder. However, since the phosphoric acid-based insulating coating changes in quality at high temperatures, it is difficult to perform heat treatment at a temperature of 600 ° C. or higher. In addition, although it is described that an insulating layer is formed on the surface of the soft magnetic metal powder in an organic solvent, the organic solvent also contains about 0.5 to 5% of water, and phosphoric acid. Is used as an aqueous solution, the soft magnetic metal powder is easily oxidized and corroded by moisture, and the magnetic properties are deteriorated and the oxide film is thickened. Since the proportion of the soft magnetic metal powder is reduced, it is difficult to increase the magnetic flux density.
また、特許文献５には、軟磁性粒子粉末の粒子表面が表面改質剤によって被覆されていると共に該被覆に無機化合物が付着している複合粒子粉末が開示されているが、絶縁層を形成している無機化合物があらかじめ表面改質剤によって分散・被覆されていないため、緻密且つ均一な絶縁層を形成することが難しく、後出比較例に示す通り、十分な耐熱性及び耐食性を有する軟磁性粒子粉末を得ることが困難である。 Patent Document 5 discloses a composite particle powder in which the surface of a soft magnetic particle powder is coated with a surface modifier and an inorganic compound adheres to the coating, but an insulating layer is formed. Since the inorganic compound being dispersed is not previously dispersed or coated with the surface modifier, it is difficult to form a dense and uniform insulating layer, and as shown in the comparative examples, a soft and soft material having sufficient heat resistance and corrosion resistance. It is difficult to obtain magnetic particle powder.
そこで、本発明は、耐食性及び耐熱性に優れた絶縁層を有する軟磁性粒子粉末及び高温で焼成した場合においても比抵抗値が低下しにくい圧粉磁心を得ることを技術的課題とする。 Therefore, the present invention has a technical problem to obtain a soft magnetic particle powder having an insulating layer excellent in corrosion resistance and heat resistance, and a dust core in which the specific resistance value does not easily decrease even when fired at a high temperature.
本発明者らは、前記課題を解決すべく鋭意研究を重ねた結果、粒子表面が表面改質剤によって被覆されていると共に該被覆に表面改質剤によって被覆された無機化合物（以下、「表面改質剤被覆無機化合物」という。）が付着している軟磁性粒子粉末は、耐食性及び耐熱性に優れており、また、該軟磁性粒子粉末を圧粉磁心用軟磁性材料として用いることにより、高温で焼成した場合においても比抵抗値が低下しにくい圧粉磁心が得られることを見いだし、本発明をなすに至った。 As a result of intensive studies to solve the above problems, the inventors of the present invention have found that the particle surface is coated with a surface modifier and the coating is coated with an inorganic compound (hereinafter referred to as “surface”). The soft magnetic particle powder to which the modifier-coated inorganic compound is attached) has excellent corrosion resistance and heat resistance, and by using the soft magnetic particle powder as a soft magnetic material for a dust core, It has been found that a powder magnetic core in which the specific resistance value is hardly lowered even when fired at a high temperature is obtained, and the present invention has been made.
即ち、本発明は、軟磁性金属粒子粉末の粒子表面が表面改質剤によって被覆されていると共に該被覆に表面改質剤によって被覆された無機化合物からなる絶縁層が形成されている複合粒子粉末からなる軟磁性粒子粉末であって、該軟磁性粒子粉末の耐熱性は、６００℃で１時間加熱後の比抵抗値が加熱前の比抵抗値に対して８５％以上であることを特徴とする軟磁性粒子粉末である（本発明１）。
That is, the present invention provides a composite particle powder in which the surface of a soft magnetic metal particle powder is coated with a surface modifier and an insulating layer made of an inorganic compound coated with the surface modifier is formed on the coating. The heat resistance of the soft magnetic particle powder is characterized in that the specific resistance value after heating at 600 ° C. for 1 hour is 85% or more of the specific resistance value before heating. Soft magnetic particle powder (Invention 1).
また、本発明は、無機化合物が、アルミニウム、ケイ素、ジルコニウム、チタニウム、カルシウム、セリウム及びマグネシウムから選ばれる元素を含有する１種又は２種以上の化合物からなることを特徴とする本発明１の軟磁性粒子粉末である（本発明２）。 The present invention is also characterized in that the inorganic compound is composed of one or more compounds containing an element selected from aluminum, silicon, zirconium, titanium, calcium, cerium and magnesium. Magnetic particle powder (Invention 2).
また、本発明は、体積平均粒子径が６．０μｍ以下である表面改質剤被覆無機化合物を用いることを特徴とする本発明１又は本発明２の軟磁性粒子粉末である（本発明３）。 Further, the present invention is the soft magnetic particle powder of the present invention 1 or the present invention 2, wherein a surface modifier-coated inorganic compound having a volume average particle diameter of 6.0 μm or less is used (the present invention 3). .
また、本発明は、無機化合物が表面改質剤によってあらかじめ分散されたものであることを特徴とする本発明１乃至本発明３のいずれかに記載の軟磁性粒子粉末である（本発明４）。 Further, the present invention is the soft magnetic particle powder according to any one of the present invention 1 to the present invention 3, wherein the inorganic compound is previously dispersed by a surface modifier (Invention 4). .
また、本発明は、軟磁性金属粒子粉末と表面改質剤とを混合し、軟磁性金属粒子粉末の粒子表面を表面改質剤によって被覆し、次いで、表面改質剤によって被覆された軟磁性金属粒子粉末と無機化合物を混合することによって軟磁性粒子粉末を得る製造法において、前記無機化合物が表面改質剤によってあらかじめ分散されていることを特徴とする本発明１乃至本発明４のいずれかに記載の軟磁性粒子粉末の製造法である（本発明５）。 The present invention also includes mixing soft magnetic metal particle powder and a surface modifier, coating the particle surface of the soft magnetic metal particle powder with the surface modifier, and then coating the soft magnetic with the surface modifier. Either of the present invention 1 to the present invention 4, wherein the inorganic compound is dispersed in advance by a surface modifier in the production method of obtaining the soft magnetic particle powder by mixing the metal particle powder and the inorganic compound. (The present invention 5).
また、本発明は、本発明１乃至本発明４のいずれかに記載の軟磁性材粒子粉末を圧縮成形してなる圧粉磁心である（本発明６）。 Moreover, this invention is a powder magnetic core formed by compression-molding the soft-magnetic material particle powder in any one of this invention 1 thru | or this invention 4 (this invention 6).
本発明に係る軟磁性粒子粉末は、耐食性及び耐熱性に優れた絶縁層を有しているので圧粉磁心用軟磁性材料として好適である。 Since the soft magnetic particle powder according to the present invention has an insulating layer excellent in corrosion resistance and heat resistance, it is suitable as a soft magnetic material for a dust core.
本発明に係る軟磁性粒子粉末の製造法によって絶縁層を軟磁性金属粒子粉末の表面に形成した場合、従来の処理方法に比べてより高い耐食性と耐熱性を付与することができるので、圧粉磁心用軟磁性粒子粉末の製造法として好適である。 When the insulating layer is formed on the surface of the soft magnetic metal particle powder by the method for producing the soft magnetic particle powder according to the present invention, higher corrosion resistance and heat resistance can be imparted compared to the conventional processing method. It is suitable as a method for producing soft magnetic particle powder for magnetic cores.
本発明に係る圧粉磁心は、前記軟磁性粒子粉末を用いたことにより、高温で焼成した場合においても比抵抗値が低下しにくく、また、耐食性も優れているので、高性能圧粉磁心として好適である。 Since the powder magnetic core according to the present invention uses the soft magnetic particle powder, the specific resistance value hardly decreases even when baked at a high temperature, and the corrosion resistance is excellent. Is preferred.
本発明の構成をより詳しく説明すれば次の通りである。 The configuration of the present invention will be described in more detail as follows.
先ず、本発明に係る軟磁性粒子粉末について述べる。 First, the soft magnetic particle powder according to the present invention will be described.
本発明に係る軟磁性粒子粉末は、芯粒子である軟磁性金属粒子粉末の粒子表面が表面改質剤によって被覆されていると共に該被覆に表面改質剤被覆無機化合物からなる絶縁層が形成されている複合粒子粉末からなっている。 In the soft magnetic particle powder according to the present invention, the surface of the soft magnetic metal particle powder as the core particle is coated with a surface modifier, and an insulating layer made of a surface modifier-coated inorganic compound is formed on the coating. It is made of composite particle powder.
本発明における無機化合物としては、アルミニウム、ケイ素、ジルコニウム、チタニウム、カルシウム、イットリウム、セリウム及びマグネシウムから選ばれる元素を含有する１種又は２種以上の化合物を用いることができ、好ましくはアルミニウム、ジルコニウム及びケイ素から選ばれる元素を含有する１種又は２種以上の化合物である。 As the inorganic compound in the present invention, one or more compounds containing an element selected from aluminum, silicon, zirconium, titanium, calcium, yttrium, cerium and magnesium can be used, preferably aluminum, zirconium and It is 1 type, or 2 or more types of compounds containing the element chosen from silicon.
本発明に係る軟磁性粒子粉末の絶縁層を形成する表面改質剤被覆無機化合物の体積平均粒子径は６．０μｍ以下であり、好ましくは５．０μｍ以下、より好ましくは４．０μｍ以下である。体積平均粒子径が６．０μｍを超える場合には、軟磁性金属粒子表面への均一な処理が困難となり、耐食性及び耐熱性を付与することのできる十分な絶縁層を形成することが困難である。 The volume average particle diameter of the surface modifier-coated inorganic compound forming the insulating layer of the soft magnetic particle powder according to the present invention is 6.0 μm or less, preferably 5.0 μm or less, more preferably 4.0 μm or less. . When the volume average particle diameter exceeds 6.0 μm, it is difficult to uniformly treat the surface of the soft magnetic metal particles, and it is difficult to form a sufficient insulating layer capable of imparting corrosion resistance and heat resistance. .
本発明に係る軟磁性粒子粉末の絶縁層を形成する表面改質剤被覆無機化合物の平均粒子径は１００ｎｍ未満であることが好ましく、より好ましくは１〜８０ｎｍ、更により好ましくは３〜５０ｎｍである。無機化合物の平均粒子径が１００ｎｍ以上の場合には、軟磁性金属粒子表面への粒子表面が表面改質剤によって被覆された無機化合物からなる絶縁層の均一な形成が困難となる。 The average particle diameter of the surface modifier-coated inorganic compound forming the insulating layer of the soft magnetic particle powder according to the present invention is preferably less than 100 nm, more preferably 1 to 80 nm, and even more preferably 3 to 50 nm. . When the average particle size of the inorganic compound is 100 nm or more, it is difficult to uniformly form an insulating layer made of an inorganic compound in which the surface of the soft magnetic metal particles is coated with a surface modifier.
本発明に係る軟磁性粒子粉末の絶縁層を形成する表面改質剤被覆無機化合物の付着量は、被処理粒子である軟磁性金属粒子粉末の比表面積にもよるが、各無機化合物の元素換算で０．００５〜５．０重量％が好ましい。０．００５〜５．０重量％の範囲で絶縁層を形成することにより、耐熱性の優れた軟磁性粒子粉末を得ることができる。５．０重量％を超える場合には、磁性に関与しない無機化合物が増加し、圧粉磁心中に占める軟磁性金属粉末の容積割合が低下するために磁気特性が低下する。得られる軟磁性粒子粉末の磁気特性を考慮した場合、０．０７５〜４．０重量％がより好ましく、更により好ましくは０．０１〜３．０重量％である。 The adhesion amount of the surface modifying agent-coated inorganic compound forming the insulating layer of the soft magnetic particle powder according to the present invention depends on the specific surface area of the soft magnetic metal particle powder that is the particle to be treated, but the element conversion of each inorganic compound 0.005 to 5.0% by weight is preferable. By forming the insulating layer in the range of 0.005 to 5.0% by weight, a soft magnetic particle powder having excellent heat resistance can be obtained. When the content exceeds 5.0% by weight, the number of inorganic compounds not involved in magnetism increases, and the volume ratio of the soft magnetic metal powder in the dust core decreases, so that the magnetic properties deteriorate. In consideration of the magnetic properties of the obtained soft magnetic particle powder, the amount is more preferably 0.075 to 4.0% by weight, still more preferably 0.01 to 3.0% by weight.
本発明に係る軟磁性粒子粉末の平均粒子径は、用途や特性に応じて選べばよいが、１．０〜５００．０μｍの範囲が好ましい。平均粒子径が５００．０μｍを超える場合には粒子径が大きすぎ、圧粉磁心に用いた場合、成形体充填密度が下がるため好ましくない。平均粒子径が１．０μｍ未満の場合には粒子径が小さすぎ、圧縮成形性が低下するため好ましくない。より好ましくは２．０〜４００．０μｍ、更により好ましくは３．０〜３００．０μｍである。 The average particle size of the soft magnetic particle powder according to the present invention may be selected according to the use and characteristics, but is preferably in the range of 1.0 to 500.0 μm. When the average particle diameter exceeds 500.0 μm, the particle diameter is too large, and when used in a dust core, the compact filling density is lowered, which is not preferable. When the average particle size is less than 1.0 μm, the particle size is too small, and the compression moldability is deteriorated. More preferably, it is 2.0-400.0 micrometers, More preferably, it is 3.0-300.0 micrometers.
本発明に係る軟磁性粒子粉末の耐熱性は、６００℃で１時間加熱後の比抵抗値が加熱前の比抵抗値に対して８５％以上であることが好ましい。耐熱性が８５％未満の場合には、絶縁層の耐熱性が十分とは言えず、圧縮成形後に軟磁性金属粒子粉末に加えられた歪みを開放するための高温での焼鈍しを行うことができない。そのため、これにより得られた軟磁性金属粒子粉末を用いて作製された圧粉磁心は、ヒステリシス損を低減することができないため、鉄損を低減することが困難となる。より好ましくは９０％以上であり、更により好ましくは９５％以上である。 The heat resistance of the soft magnetic particle powder according to the present invention is preferably such that the specific resistance value after heating at 600 ° C. for 1 hour is 85% or more with respect to the specific resistance value before heating. If the heat resistance is less than 85%, the heat resistance of the insulating layer cannot be said to be sufficient, and annealing at a high temperature to release strain applied to the soft magnetic metal particle powder after compression molding may be performed. Can not. For this reason, the dust core produced using the soft magnetic metal particle powder thus obtained cannot reduce the hysteresis loss, and thus it is difficult to reduce the iron loss. More preferably, it is 90% or more, and still more preferably 95% or more.
本発明に係る軟磁性粒子粉末の耐食性は、後述する評価方法において、錆の発生の目視観察の程度が、△（軟磁性粒子粉末に若干の変色が認められる）、○（軟磁性粒子粉末の変色がほとんど認められない）もしくは◎（軟磁性粒子粉末の変色が認められない）のレベルであることが好ましく、より好ましくは○（軟磁性粒子粉末の変色がほとんど認められない）もしくは◎（軟磁性粒子粉末の変色が認められない）のレベルである。 Corrosion resistance of the soft magnetic particle powder according to the present invention is evaluated by the evaluation method described later, in which the degree of visual observation of the occurrence of rust is Δ (slight discoloration is observed in the soft magnetic particle powder), ○ (soft magnetic particle powder It is preferably at a level of ◎ (almost no discoloration is observed) or ◎ (no discoloration of soft magnetic particle powder is observed), more preferably ○ (almost no discoloration of soft magnetic particle powder is observed) or ◎ (soft The discoloration of the magnetic particle powder is not observed).
本発明における表面改質剤としては、軟磁性粒子粉末の粒子表面へ表面改質剤被覆無機化合物からなる絶縁層を形成できるもの、もしくは、無機化合物を所望の程度まで分散することができるものであれば何を用いてもよく、好ましくはアルコキシシラン、フルオロアルキルシラン、シラン系カップリング剤及びオルガノポリシロキサン等の有機ケイ素化合物、チタネート系、アルミネート系及びジルコネート系などのカップリング剤、低分子あるいは高分子界面活性剤等の一種又は二種以上であり、より好ましくはアルコキシシラン、フルオロアルキルシラン、シラン系カップリング剤、オルガノポリシロキサン等の有機ケイ素化合物、チタネート系、アルミネート系及びジルコネート系の各種カップリング剤である。軟磁性粒子粉末の粒子表面へ表面改質剤被覆無機化合物を付着するための表面改質剤と無機化合物をあらかじめ分散するための表面改質剤とは同じてあっても異なっていてもかまわない。 The surface modifier in the present invention can form an insulating layer made of a surface modifier-coated inorganic compound on the surface of the soft magnetic particle powder, or can disperse the inorganic compound to a desired degree. Any of them may be used, preferably alkoxysilane, fluoroalkylsilane, silane coupling agent and organopolysiloxane such as organopolysiloxane, titanate, aluminate and zirconate coupling agents, low molecular weight Or it is 1 type, or 2 or more types, such as polymeric surfactant, More preferably, alkoxysilane, fluoroalkylsilane, silane coupling agent, organosilicon compounds such as organopolysiloxane, titanate, aluminate and zirconate Coupling agents. The surface modifier for attaching the surface modifier-coated inorganic compound to the surface of the soft magnetic particle powder and the surface modifier for predispersing the inorganic compound may be the same or different. .
有機ケイ素化合物としては、テトラエトキシシラン、テトラメトキシシラン、メチルトリエトキシシラン、ジメチルジエトキシシラン、フェニルトリエトキシシラン、ジフェニルジエトキシシラン、メチルトリメトキシシラン、ジメチルジメトキシシラン、フェニルトリメトキシシラン、ジフェニルジメトキシシラン、エチルトリエトキシシラン、プロピルトリエトキシシラン、ブチルトリエトキシシラン、イソブチルトリメトキシシラン、ヘキシルトリエトキシシラン、オクチルトリエトキシシラン及びデシルトリエトキシシラン等のアルコキシシラン、トリフルオロプロピルトリメトキシシラン、トリデカフルオロオクチルトリメトキシシラン、ヘプタデカフルオロデシルトリメトキシシラン、トルフルオロプロピルトリエトキシシラン、ヘプタデカフルオロデシルトリエトキシシラン及びトリデカフルオロオクチルトリエトキシシラン等のフルオロアルキルシラン、ビニルトリメトキシシラン、ビニルトリエトキシシラン、γ―アミノプロピルトリエトキシシラン、γ―グリシドキシプロピルトリメトキシシラン、γ―メルカプトプロピルトリメトキシシラン、γ―メタクロイルオキシプロピルトリメトキシシラン、Ｎ−（β−アミノエチル）−γ−アミノプロピルトリメトキシシラン、γ−グリシドキシプロピルメチルジメトキシシラン、γ−クロロプロピルトリメトキシシラン等のシラン系カップリング剤、ポリシロキサン、メチルハイドロジェンポリシロキサン、変性ポリシロキサン等のオルガノポリシロキサン等が挙げられる。 Examples of organosilicon compounds include tetraethoxysilane, tetramethoxysilane, methyltriethoxysilane, dimethyldiethoxysilane, phenyltriethoxysilane, diphenyldiethoxysilane, methyltrimethoxysilane, dimethyldimethoxysilane, phenyltrimethoxysilane, and diphenyldimethoxy. Silane, ethyltriethoxysilane, propyltriethoxysilane, butyltriethoxysilane, isobutyltrimethoxysilane, hexyltriethoxysilane, octyltriethoxysilane, decyltriethoxysilane and other alkoxysilanes, trifluoropropyltrimethoxysilane, trideca Fluorooctyltrimethoxysilane, heptadecafluorodecyltrimethoxysilane, trifluoropropyltriethoxysilane Fluoroalkylsilanes such as heptadecafluorodecyltriethoxysilane and tridecafluorooctyltriethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, γ-aminopropyltriethoxysilane, γ-glycidoxypropyltrimethoxysilane, γ -Mercaptopropyltrimethoxysilane, γ-methacryloyloxypropyltrimethoxysilane, N- (β-aminoethyl) -γ-aminopropyltrimethoxysilane, γ-glycidoxypropylmethyldimethoxysilane, γ-chloropropyltrimethoxy Examples thereof include silane coupling agents such as silane, organopolysiloxanes such as polysiloxane, methyl hydrogen polysiloxane, and modified polysiloxane.
チタネート系カップリング剤としては、イソプロピルトリステアロイルチタネート、イソプロピルトリス（ジオクチルパイロホスフェート）チタネート、イソプロピルトリ（Ｎ−アミノエチル・アミノエチル）チタネート、テトラオクチルビス（ジトリデシルホスフェートチタネート、テトラ（２，２ジアリルオキシメチル−１−ブチル）ビス（ジトリデシル）ホスフェートチタネート、ビス（ジオクチルパイロホスフェート）オキシアセテートチタネート、ビス（ジオクチルパイロホスフェート）エチレンチタネート等が挙げられる。 Titanate coupling agents include isopropyl tristearoyl titanate, isopropyl tris (dioctyl pyrophosphate) titanate, isopropyl tri (N-aminoethyl / aminoethyl) titanate, tetraoctyl bis (ditridecyl phosphate titanate, tetra (2,2 diallyl) Examples include oxymethyl-1-butyl) bis (ditridecyl) phosphate titanate, bis (dioctylpyrophosphate) oxyacetate titanate, and bis (dioctylpyrophosphate) ethylene titanate.
アルミネート系カップリング剤としては、アセトアルコキシアルミニウムジイソプロピレート、アルミニウムジイソプロポキシモノエチルアセトアセテート、アルミニウムトリスエチルアセトアセテート、アルミニウムトリスアセチルアセトネート等が挙げられる。 Examples of the aluminate coupling agent include acetoalkoxy aluminum diisopropylate, aluminum diisopropoxy monoethyl acetoacetate, aluminum trisethyl acetoacetate, aluminum trisacetylacetonate and the like.
ジルコネート系カップリング剤としては、ジルコニウムテトラキスアセチルアセトネート、ジルコニウムジブトキシビスアセチルアセトネート、ジルコニウムテトラキスエチルアセトアセテート、ジルコニウムトリボトキシモノエチルアセトアセテート、ジルコニウムトリブトキシアセチルアセトネート等が挙げられる。 Examples of the zirconate coupling agent include zirconium tetrakisacetylacetonate, zirconium dibutoxybisacetylacetonate, zirconium tetrakisethylacetoacetate, zirconium tribotoxymonoethylacetoacetate, zirconium tributoxyacetylacetonate and the like.
低分子系界面活性剤としては、アルキルベンゼンスルホン酸塩、ジオクチルスルホンコハク酸塩、アルキルアミン酢酸塩、アルキル脂肪酸塩等が挙げられる。高分子系界面活性剤としては、ポリビニルアルコール、ポリアクリル酸塩、カルボキシメチルセルロース、アクリル酸−マレイン酸塩コポリマー、オレフィン−マレイン酸塩コポリマー等が挙げられる。 Examples of the low molecular surfactant include alkylbenzene sulfonate, dioctyl sulfone succinate, alkylamine acetate, alkyl fatty acid salt and the like. Examples of the polymeric surfactant include polyvinyl alcohol, polyacrylate, carboxymethylcellulose, acrylic acid-maleate copolymer, and olefin-maleate copolymer.
軟磁性金属粒子粉末に対する表面改質剤の被覆量は、表面改質剤被覆軟磁性金属粒子粉末に対して各表面改質剤が含有する金属の元素換算で０．００１〜３．０重量％が好ましく、より好ましくは０．００２〜２．０重量％、最も好ましくは０．００３〜１．０重量％である。また、金属を含有しない表面改質剤の場合、表面改質剤被覆軟磁性金属粒子粉末に対してＣ換算で０．００１〜３．０重量％が好ましく、より好ましくは０．００２〜２．０重量％、更に好ましくは０．００３〜１．０重量％である。各表面改質剤が含有する金属の元素換算で０．００１重量％未満又はＣ換算で０．００１重量％未満の場合には、軟磁性金属粒子粉末表面に耐食性及び耐熱性を付与することのできる十分な絶縁層を形成することが困難である。また、各表面改質剤が含有する金属の元素換算で３．０重量％又はＣ換算で３．０重量％を超える場合には、磁性に関与しない有機物成分が増加するため好ましくない。 The coating amount of the surface modifier on the soft magnetic metal particle powder is 0.001 to 3.0% by weight in terms of the element of the metal contained in each surface modifier on the surface modifier coated soft magnetic metal particle powder. Is preferable, more preferably 0.002 to 2.0% by weight, and most preferably 0.003 to 1.0% by weight. Moreover, in the case of the surface modifier which does not contain a metal, 0.001-3.0 weight% is preferable in conversion of C with respect to the surface modifier covering soft magnetic metal particle powder, More preferably, it is 0.002-2. It is 0% by weight, more preferably 0.003 to 1.0% by weight. In the case of less than 0.001% by weight in terms of element of metal contained in each surface modifier or less than 0.001% by weight in terms of C, the surface of the soft magnetic metal particles is imparted with corrosion resistance and heat resistance. It is difficult to form a sufficient insulating layer. Moreover, when it exceeds 3.0 weight% in conversion of the element of the metal which each surface modifier contains, or 3.0 weight% in conversion of C, it is not preferable since the organic matter component which does not participate in magnetism increases.
無機化合物に対する表面改質剤の被覆量は、表面改質剤被覆無機化合物に対して各表面改質剤が含有する金属の元素換算で０．００１〜５．０重量％が好ましく、より好ましくは０．００５〜４．０重量％、最も好ましくは０．０１〜３．０重量％である。また、金属を含有しない表面改質剤の場合、表面改質剤被覆無機化合物に対してＣ換算で０．００１〜５．０重量％が好ましく、より好ましくは０．００５〜４．０重量％、更に好ましくは０．０１〜３．０重量％である。各表面改質剤が含有する金属の元素換算で０．００１重量％未満又はＣ換算で０．００１重量％未満の場合には、無機化合物を前分散させる効果が不十分であり、挙動粒子径を６．０μｍ以下とすることが困難である。また、各表面改質剤が含有する金属の元素換算で５．０重量％又はＣ換算で５．０重量％を超える場合には、磁性に関与しない有機物成分が増加するため好ましくない。 The coating amount of the surface modifier with respect to the inorganic compound is preferably 0.001 to 5.0% by weight in terms of metal element contained in each surface modifier with respect to the surface modifier coated inorganic compound, more preferably 0.005 to 4.0 wt%, most preferably 0.01 to 3.0 wt%. Moreover, in the case of the surface modifier which does not contain a metal, 0.001-5.0 weight% is preferable in conversion of C with respect to a surface modifier coating inorganic compound, More preferably, 0.005-4.0 weight% More preferably, it is 0.01 to 3.0% by weight. In the case of less than 0.001% by weight in terms of element of metal contained in each surface modifier or less than 0.001% by weight in terms of C, the effect of predispersing the inorganic compound is insufficient, and the behavior particle size Is less than 6.0 μm. Moreover, when it exceeds 5.0 weight% in element conversion of the metal which each surface modifier contains, or 5.0 weight% in C conversion, since the organic substance component which does not participate in magnetism increases, it is unpreferable.
次に、本発明に係る軟磁性粒子粉末の製造法について述べる。 Next, a method for producing the soft magnetic particle powder according to the present invention will be described.
本発明に係る軟磁性粒子粉末は、軟磁性金属粒子粉末と表面改質剤とを混合し、軟磁性粒子粉末の粒子表面を表面改質剤によって被覆し、次いで、表面改質剤によって被覆された軟磁性金属粒子粉末とあらかじめ表面改質剤によって分散処理された無機化合物を混合することによって得ることができる。 The soft magnetic particle powder according to the present invention is obtained by mixing soft magnetic metal particle powder and a surface modifier, coating the particle surface of the soft magnetic particle powder with the surface modifier, and then coating with the surface modifier. It can be obtained by mixing a soft magnetic metal particle powder and an inorganic compound that has been previously dispersed with a surface modifier.
無機化合物の表面改質剤による前分散処理は、無機化合物と表面改質剤とを機械的に混合攪拌すればよい。また、軟磁性金属粒子粉末の粒子表面への表面改質剤による被覆は、軟磁性金属粒子粉末と表面改質剤とを機械的に混合攪拌すればよい。 The pre-dispersion treatment of the inorganic compound with the surface modifier may be performed by mechanically mixing and stirring the inorganic compound and the surface modifier. Further, the surface of the soft magnetic metal particle powder with the surface modifier may be mechanically mixed and agitated with the soft magnetic metal particle powder and the surface modifier.
本発明における軟磁性金属粒子粉末としては、アトマイズ鉄粉、還元鉄粉、カルボニル鉄粉等の各種製法による鉄粉、珪素鋼粉、センダスト粉、パーマロイ粉、パーメンダー粉等を用いることができる。軟磁性金属粒子粉末の平均粒子径は、１．０〜５００．０μｍが好ましく、より好ましくは２．０〜４００．０μｍ、更により好ましくは３．０〜３００．０μｍである。 As the soft magnetic metal particle powder in the present invention, iron powder by various production methods such as atomized iron powder, reduced iron powder, carbonyl iron powder, silicon steel powder, sendust powder, permalloy powder, permender powder and the like can be used. The average particle diameter of the soft magnetic metal particle powder is preferably 1.0 to 500.0 μm, more preferably 2.0 to 400.0 μm, and still more preferably 3.0 to 300.0 μm.
無機化合物の表面改質剤による前分散処理、軟磁性金属粒子粉末と表面改質剤との混合攪拌、並びに、表面改質剤被覆無機化合物と粒子表面に表面改質剤が被覆されている軟磁性金属粒子粉末との混合攪拌をするための機器としては、特には限定されないが、粉体層に衝撃力、せん断力、圧縮力、及び／または摩擦力を加えることのできる装置が好ましく、例えば、ボール型混練機、高速せん断ミル、ホイール型混練機、ブレード型混練機、ロール型混練機等を用いることができる。本発明の実施にあたっては、ボール型混練機及び高速せん断ミルがより効果的に使用できる。 Pre-dispersion treatment of the inorganic compound with the surface modifier, mixing and stirring of the soft magnetic metal particle powder and the surface modifier, and the surface modifier coated inorganic compound and the surface of the particle coated with the surface modifier The apparatus for mixing and stirring with the magnetic metal particle powder is not particularly limited, but an apparatus that can apply impact force, shear force, compressive force, and / or friction force to the powder layer is preferable. A ball-type kneader, a high-speed shear mill, a wheel-type kneader, a blade-type kneader, a roll-type kneader, or the like can be used. In carrying out the present invention, a ball-type kneader and a high-speed shear mill can be used more effectively.
前記ホイール型混練機としては、具体的に、エッジランナー（「ミックスマラー」、「シンプソンミル」、「サンドミル」と同義語である）、マルチマル、ストッツミル、ウエットパンミル、コナーミル、リングマラー等があり、好ましくはエッジランナー、マルチマル、ストッツミル、ウエットパンミル、リングマラー、であり、より好ましくはエッジランナーである。前記高速せん断ミルとしては、ハイブリダイザー（奈良機械製作所製）、ノビルタ（ホソカワミクロン製）等がある。前記ボール型混練機としては、転動ボールミル、振動ボールミル、遊星ミル等がある。前記ブレード型混練機としては、ヘンシェルミキサー、プラネタリーミキサー、ナウターミキサー等がある。前記ロール型混練機としては、エクストルーダー等がある。 Specific examples of the wheel-type kneader include edge runners (synonymous with “mix muller”, “Simpson mill”, “sand mill”), multi-mal, stotz mill, wet pan mill, conner mill, ring muller, and the like. , Preferably an edge runner, multi-mal, Stots mill, wet pan mill, and ring muller, and more preferably an edge runner. Examples of the high-speed shear mill include a hybridizer (manufactured by Nara Machinery Co., Ltd.) and nobilta (manufactured by Hosokawa Micron). Examples of the ball kneader include a rolling ball mill, a vibrating ball mill, a planetary mill, and the like. Examples of the blade-type kneader include a Henschel mixer, a planetary mixer, and a nauter mixer. Examples of the roll-type kneader include an extruder.
なお、表面改質剤によって被覆された軟磁性金属粒子粉末と表面改質剤被覆無機化合物を混合攪拌する際の混練機として高速せん断ミルを用いる場合には、表面改質剤によって被覆された軟磁性金属粒子粉末と表面改質剤被覆無機化合物とをプレミックスした後、圧縮・せん断力よりなる機械的エネルギーを作用させて軟磁性金属粒子粉末の粒子表面に表面改質剤被覆無機化合物からなる絶縁層を形成することが好ましい。 When a high-speed shear mill is used as a kneader for mixing and stirring the soft magnetic metal particle powder coated with the surface modifier and the surface modifier-coated inorganic compound, the soft magnetic metal particle powder coated with the surface modifier is used. After premixing the magnetic metal particle powder and the surface modifier-coated inorganic compound, the surface of the soft magnetic metal particle powder is composed of the surface modifier-coated inorganic compound by applying mechanical energy consisting of compression and shear force. It is preferable to form an insulating layer.
表面改質剤によって被覆された軟磁性金属粒子粉末と表面改質剤被覆無機化合物とをプレミックスするための機器としては、容器回転式が好ましく、外部容器が回転もしくは転動するタイプのミルやミキサ（例えば、コンクリートミキサ等の重力式ミキサ）及びブレンダーを用いることが好ましい。 As a device for premixing the soft magnetic metal particle powder coated with the surface modifier and the surface modifier-coated inorganic compound, a container rotating type is preferable, and a mill of a type in which an outer container rotates or rolls, It is preferable to use a mixer (for example, a gravitational mixer such as a concrete mixer) and a blender.
軟磁性金属粒子粉末の粒子表面に表面改質剤を被覆した後、表面改質剤によって分散処理された無機化合物を添加し、混合攪拌して表面改質剤被覆軟磁性金属粒子粉末表面に表面改質剤被覆無機化合物からなる絶縁層を形成する。 After the surface of the soft magnetic metal particle powder is coated with a surface modifier, an inorganic compound dispersed by the surface modifier is added, mixed and stirred, and then the surface of the surface of the soft magnetic metal particle powder is coated with the surface modifier. An insulating layer made of a modifier-coated inorganic compound is formed.
表面改質剤被覆軟磁性金属粒子粉末に表面改質剤被覆無機化合物からなる絶縁層を形成した後、必要により更に、乾燥処理を行ってもよい。乾燥処理を行う場合の加熱温度は、通常、４０〜２００℃が好ましく、より好ましくは６０〜１５０℃であり、加熱雰囲気は、空気中及びＮ２ガスなどの不活性ガス雰囲気下のいずれでも行うことができるが、好ましくはＮ２ガス等の不活性ガス雰囲気下である。 After forming an insulating layer made of a surface modifier-coated inorganic compound on the surface modifier-coated soft magnetic metal particle powder, if necessary, a drying treatment may be performed. The heating temperature in the case of performing the drying treatment is usually preferably 40 to 200 ° C, more preferably 60 to 150 ° C, and the heating atmosphere is performed in air or in an inert gas atmosphere such as N 2 gas. However, it is preferably in an inert gas atmosphere such as N 2 gas.
次に、本発明に係る圧粉磁心について述べる。 Next, the dust core according to the present invention will be described.
本発明に係る圧粉磁心は、本発明に係る軟磁性粒子粉末に、必要により、ステアリン酸亜鉛等の潤滑剤や結合剤樹脂等の添加剤を混合し、該混合粒子粉末を圧縮成形した後、加熱処理することによって得ることができる。 The powder magnetic core according to the present invention is obtained by mixing the soft magnetic particle powder according to the present invention with an additive such as a lubricant such as zinc stearate and a binder resin, if necessary, and compressing the mixed particle powder. It can be obtained by heat treatment.
本発明に係る圧粉磁心は、本発明に係る軟磁性粒子粉末に、必要により、ステアリン酸亜鉛等の潤滑剤や結合剤樹脂等の添加剤を混合し、該混合粒子粉末を圧縮成形した後、加熱処理することによって得ることができる。 The powder magnetic core according to the present invention is obtained by mixing the soft magnetic particle powder according to the present invention with an additive such as a lubricant such as zinc stearate and a binder resin, if necessary, and compressing the mixed particle powder. It can be obtained by heat treatment.
結合剤樹脂としては、エポキシ樹脂、イミド樹脂、フェノール樹脂、又はシリコーン樹脂等を単独又は混合して用いることができる。 As the binder resin, an epoxy resin, an imide resin, a phenol resin, a silicone resin, or the like can be used alone or in combination.
圧縮成形は、通常行われている、金型を用いた圧縮成形法で行うことができる。なお、成形圧は、用途に応じて適宜選べばよい。 The compression molding can be performed by a compression molding method using a mold that is usually performed. In addition, what is necessary is just to select a shaping | molding pressure suitably according to a use.
圧縮成形後の歪み取りのための焼鈍温度は、磁性粒子自体が熱拡散による粒子成長が起こらない高温が望ましい。好ましくは５００〜１２００℃であり、より好ましくは６００〜１０００℃である。焼鈍の雰囲気は、窒素やＡｒガスなどの不活性ガス雰囲気中、水素などの還元性雰囲気中、あるいは真空などの非酸化性雰囲気中で行うことが望ましい。 The annealing temperature for strain relief after compression molding is preferably a high temperature at which the magnetic particles themselves do not cause particle growth due to thermal diffusion. Preferably it is 500-1200 degreeC, More preferably, it is 600-1000 degreeC. The annealing atmosphere is desirably performed in an inert gas atmosphere such as nitrogen or Ar gas, in a reducing atmosphere such as hydrogen, or in a non-oxidizing atmosphere such as vacuum.
本発明に係る圧粉磁心は、高温（６００℃及び７００℃）における焼鈍後の比抵抗値が、未処理の軟磁性金属粒子粉末を用いて得られた圧粉磁心の比抵抗値と比べて高い値を有している。 In the dust core according to the present invention, the specific resistance value after annealing at high temperatures (600 ° C. and 700 ° C.) is compared with the specific resistance value of the dust core obtained by using the untreated soft magnetic metal particle powder. It has a high value.
本発明に係る圧粉磁心の耐食性は、後述する評価方法において、目視観察で錆の発生の程度が、○（錆の発生がほとんど認められない）もしくは◎（錆の発生が認められない）のレベルであることが好ましく、未処理、もしくは他の処理の軟磁性金属粒子粉末と比べて優れた耐食性を有している。 Corrosion resistance of the powder magnetic core according to the present invention is such that, in the evaluation method described later, the degree of occurrence of rust by visual observation is ○ (the occurrence of rust is hardly recognized) or ◎ (the occurrence of rust is not recognized). It is preferably at a level, and has excellent corrosion resistance compared to untreated or other treated soft magnetic metal particle powders.
＜作用＞
本発明における最も重要な点は、軟磁性金属粒子粉末と表面改質剤とを混合し、軟磁性粒子粉末の粒子表面を表面改質剤によって被覆し、次いで、表面改質剤によって被覆された軟磁性金属粒子粉末とあらかじめ表面改質剤によって分散処理された無機化合物を混合することによって得られた軟磁性粒子粉末は、耐食性及び耐熱性に優れているという事実である。
<Action>
The most important point in the present invention is that the soft magnetic metal particle powder and the surface modifier are mixed, the particle surface of the soft magnetic particle powder is coated with the surface modifier, and then coated with the surface modifier. The fact is that the soft magnetic particle powder obtained by mixing the soft magnetic metal particle powder and the inorganic compound dispersed in advance with the surface modifier is excellent in corrosion resistance and heat resistance.
本発明に係る軟磁性粒子粉末の耐食性及び耐熱性が優れている理由として、本発明者は、無機化合物を表面改質剤によってあらかじめ分散・被覆しておくことで、無機化合物の挙動粒子における平均粒子径（体積平均粒子径）を未処理の無機化合物のそれと比べてより微細にできるため、表面改質剤によって被覆された軟磁性金属粒子粉末と共に混合した場合に、より緻密な絶縁層を形成することができたことによるものと考えている。 The reason for the excellent corrosion resistance and heat resistance of the soft magnetic particle powder according to the present invention is that the present inventor pre-dispersed and coated the inorganic compound with a surface modifier to obtain an average of the behavior particles of the inorganic compound. Since the particle size (volume average particle size) can be made finer than that of untreated inorganic compounds, a denser insulating layer is formed when mixed with soft magnetic metal particle powder coated with a surface modifier. I believe that it was possible to do it.
以下、本発明における実施例を示し、本発明を具体的に説明する。 Hereinafter, the present invention will be described in detail with reference to examples.
軟磁性金属粒子粉末、表面改質剤被覆無機化合物及び軟磁性粒子粉末の平均粒子径は、いずれも電子顕微鏡写真に示される粒子５０〜３５０個の粒子径をそれぞれ測定し、その平均値で示した。 The average particle diameters of the soft magnetic metal particle powder, the surface modifier-coated inorganic compound, and the soft magnetic particle powder are all measured by measuring the particle diameters of 50 to 350 particles shown in the electron micrographs, and the average value is shown. It was.
無機化合物及び表面改質剤被覆無機化合物の体積平均粒子径（Ｄ５０）は、「レーザー回折式粒度分布測定装置 ｍｏｄｅｌ ＨＥＬＯＳ ＬＡ／ＫＡ」（ＳＹＭＰＡＴＥＣ社製）の乾式分散ユニットを用いて、分散圧０．１ＭＰａ（１ｂａｒ）にて測定した。尚、体積平均粒子径（Ｄ５０）は粒子粉末の全体積を１００％として粒子径に対する累積割合を求めたときの累積割合が５０％となる粒子径である。 The volume average particle size (D 50 ) of the inorganic compound and the surface modifier-coated inorganic compound is determined by using a dry dispersion unit of “Laser diffraction type particle size distribution measuring device model HELOS LA / KA” (manufactured by SYMPATEC). Measurement was performed at 0.1 MPa (1 bar). The volume average particle diameter (D 50 ) is a particle diameter at which the cumulative ratio is 50% when the cumulative ratio with respect to the particle diameter is determined with the total volume of the particle powder being 100%.
軟磁性金属粒子粉末及び無機化合物の粒子表面に被覆されている表面改質剤の被覆量は、金属元素を含有している場合、各表面改質剤に含有されている金属について、「蛍光Ｘ線分析装置３０６３Ｍ型」（理学電機工業株式会社製）を使用し、ＪＩＳ Ｋ０１１９の「けい光Ｘ線分析通則」に従って測定した。また、表面改質剤が金属元素を含有していない場合には、「堀場金属炭素・硫黄分析装置ＥＭＩＡ−２２００型」（株式会社堀場製作所製）を用いて炭素量を測定することにより求めた。 The coating amount of the surface modifying agent coated on the surface of the soft magnetic metal particle powder and the inorganic compound particle, when containing a metal element, is “fluorescence X” for the metal contained in each surface modifying agent. The measurement was performed in accordance with JIS K0119 “General Rules for Fluorescence X-ray Analysis” using a “line analyzer 3063M type” (manufactured by Rigaku Corporation). Moreover, when the surface modifier did not contain a metal element, it was determined by measuring the carbon amount using “Horiba Metal Carbon / Sulfur Analyzer EMIA-2200 Model” (manufactured by Horiba, Ltd.). .
軟磁性粒子粉末の粒子表面に形成されている表面改質剤被覆無機化合物からなる絶縁層の被覆量は、「蛍光Ｘ線分析装置３０６３Ｍ型」（理学電機工業株式会社製）を使用し、ＪＩＳ Ｋ０１１９の「けい光Ｘ線分析通則」に従って測定した。 The coating amount of the insulating layer made of the surface modifier-coated inorganic compound formed on the surface of the soft magnetic particle powder is “JIS X-ray fluorescence analyzer 3063M” (manufactured by Rigaku Denki Kogyo Co., Ltd.). The measurement was carried out in accordance with K0119 "General X-ray fluorescence analysis rules".
軟磁性金属粒子粉末及び軟磁性粒子粉末の比抵抗値は、試料粉体を試料台にセットし、荷重を０〜４０ＭＰａまで加えながら４端子法にて測定を行い、４０ＭＰａにおける比抵抗値を用いた。 The specific resistance values of the soft magnetic metal particle powder and the soft magnetic particle powder are measured by the four-terminal method while setting the sample powder on the sample stage and applying a load from 0 to 40 MPa, and the specific resistance value at 40 MPa is used. It was.
軟磁性金属粒子粉末及び軟磁性粒子粉末の耐熱性は、未加熱の軟磁性粒子粉末の比抵抗値（ρ１）と６００℃で１時間加熱した後の軟磁性粒子粉末の比抵抗値（ρ２）をそれぞれ測定し、下記数１にそれぞれの値を挿入して、求めた値を耐熱性（加熱前後の比抵抗値の変化率）（％）として示した。 The heat resistance of the soft magnetic metal particle powder and the soft magnetic particle powder is determined by the specific resistance value (ρ1) of the unheated soft magnetic particle powder and the specific resistance value (ρ2) of the soft magnetic particle powder after heating at 600 ° C. for 1 hour. Was measured, and each value was inserted into the following formula 1, and the obtained value was shown as heat resistance (change rate of specific resistance value before and after heating) (%).
＜数１＞
耐熱性（％）＝（ρ２／ρ１）×１００
<Equation 1>
Heat resistance (%) = (ρ2 / ρ1) × 100
軟磁性金属粒子粉末及び軟磁性粒子粉末の耐食性は、１００ｍｌビーカーを用い、室温において純水２０ｍｌ中に試料粉体３ｇを３時間浸漬した後、９０℃で６時間乾燥させたものを目視で観察し、試料粉体が茶色く変色しているものを×、試料粉体に若干の変色が認められるものを△、試料粉体の変色がほとんど認められないものを○、試料粉体の変色が認められないものを◎とした。 The corrosion resistance of the soft magnetic metal particle powder and the soft magnetic particle powder was visually observed using a 100 ml beaker and 3 g of sample powder immersed in 20 ml of pure water at room temperature for 3 hours and then dried at 90 ° C. for 6 hours. X, when the sample powder is discolored brown, Δ when the sample powder is slightly discolored, ○ when the sample powder is hardly discolored, and discoloration of the sample powder Those that could not be marked as ◎.
圧粉磁心の比抵抗値は、まず、軟磁性粒子粉末６．０ｇを測り取り、外径２０ｍｍ、内径１０ｍｍのリング成形金型を用いて、１０トンプレスにて成形圧力６８６ＭＰａで加圧成形を行い、リング成形体を複数個作製し、該リング成形体のプレス面を１ｍｍピッチの４端子電気抵抗測定装置（ロレスタＧＰ／ＭＣＰ−Ｔ６００、三菱化成製）で１０Ｖの電圧を印加して測定した。 The specific resistance value of the powder magnetic core is obtained by first measuring 6.0 g of soft magnetic particle powder, and using a ring molding die having an outer diameter of 20 mm and an inner diameter of 10 mm, press molding at a molding pressure of 686 MPa using a 10-ton press. A plurality of ring molded bodies were prepared, and the press surface of the ring molded body was measured by applying a voltage of 10 V with a 4-terminal electrical resistance measuring device (Loresta GP / MCP-T600, manufactured by Mitsubishi Kasei) with a pitch of 1 mm. .
圧粉磁心の焼鈍後における比抵抗値は、上述で作製したリング成形体を、窒素雰囲気下にて６００℃及び７００℃でそれぞれ１時間加熱処理を行った後、上述の比抵抗値の測定と同様にして求めた。 The specific resistance value after annealing of the dust core is obtained by subjecting the ring molded body produced above to heat treatment at 600 ° C. and 700 ° C. for 1 hour in a nitrogen atmosphere, and then measuring the above specific resistance value. It calculated | required similarly.
圧粉磁心の耐食性は、１００ｍｌビーカーを用い、室温において純水２０ｍｌ中に上述のリング成形体のうち未加熱のものを１時間浸漬した後取り出し、目視で観察した。リング成形体に著しく錆が発生しているものを×、若干の錆の発生が認められるものを△、錆の発生がほとんど認められないものを○、錆の発生が認められないものを◎とした。 The corrosion resistance of the dust core was observed by visual observation using a 100 ml beaker after immersing an unheated ring-molded product in 20 ml of pure water at room temperature for 1 hour. Ring molded body with markedly rusted ×, slightly rusted △, almost no rusted ◯, no rusted ◎ did.
＜実施例１−１：軟磁性粒子粉末の製造＞
まず、あらかじめ無機化合物１（種類：Ａｌ２Ｏ３、粒子形状：粒状、平均粒子径：１３ｎｍ、体積平均粒子径：６．９１μｍ）３５０ｇに、メチルハイドロジェンポリシロキサン（商品名：ＴＳＦ４８４、ＧＥ東芝シリコーン株式会社製）１０．５ｇを加えた後、振動ボールミルを用いて２０分間混合・分散を行い、表面改質剤被覆無機化合物（無機化合物５）を得た。
<Example 1-1: Production of soft magnetic particle powder>
First, 350 g of inorganic compound 1 (type: Al 2 O 3 , particle shape: granular, average particle size: 13 nm, volume average particle size: 6.91 μm) is added to methyl hydrogen polysiloxane (trade name: TSF484, GE Toshiba). After adding 10.5 g (manufactured by Silicone Co., Ltd.), the mixture was dispersed and dispersed for 20 minutes using a vibration ball mill to obtain a surface modifier-coated inorganic compound (inorganic compound 5).
得られた表面改質剤被覆無機化合物（無機化合物５）は、平均粒子径が１３ｎｍであり、体積平均粒子径は２．３８μｍであった。メチルハイドロジェンポリシロキサンの被覆量はＳｉ換算で１．２２重量％であった。 The obtained surface modifier-coated inorganic compound (inorganic compound 5) had an average particle size of 13 nm and a volume average particle size of 2.38 μm. The coating amount of methyl hydrogen polysiloxane was 1.22% by weight in terms of Si.
次いで、軟磁性金属粒子粉末１（種類：鉄粉、粒子形状：粒状、平均粒子径：１１５．０μｍ、比抵抗値：１１６．２ｍΩ・ｃｍ、耐熱性：５９％、耐食性：×）３ｋｇに、メチルハイドロジェンポリシロキサン（商品名：ＴＳＦ４８４、ＧＥ東芝シリコーン株式会社製）１５ｇを加えた後、振動ボールミルを用いて２０分間混合・攪拌を行い、表面改質剤被覆軟磁性金属粒子粉末を得た。このときのメチルハイドロジェンポリシロキサンの被覆量はＳｉ換算で０．２１重量％であった。 Next, 3 kg of soft magnetic metal particle powder 1 (type: iron powder, particle shape: granular, average particle diameter: 115.0 μm, specific resistance value: 116.2 mΩ · cm, heat resistance: 59%, corrosion resistance: ×), After adding 15 g of methyl hydrogen polysiloxane (trade name: TSF484, manufactured by GE Toshiba Silicone Co., Ltd.), the mixture was stirred and mixed for 20 minutes using a vibration ball mill to obtain a surface modifier-coated soft magnetic metal particle powder. . The coating amount of methyl hydrogen polysiloxane at this time was 0.21% by weight in terms of Si.
次に、前述のあらかじめ表面改質剤によって分散・被覆された無機化合物（無機化合物５）３００ｇを、上記で得られた表面改質剤被覆軟磁性金属粒子粉末に添加し、更に６０分間振動ボールミルを用いて混合・攪拌を行い、メチルハイドロジェンポリシロキサンで被覆された軟磁性金属粒子粉末の表面に表面改質剤被覆無機化合物からなる絶縁層が形成された複合粒子粉末を得た。 Next, 300 g of the inorganic compound (inorganic compound 5) previously dispersed and coated with the surface modifier is added to the surface modifier-coated soft magnetic metal particle powder obtained above, and a vibration ball mill for 60 minutes. Was mixed and stirred to obtain a composite particle powder in which an insulating layer made of a surface modifier-coated inorganic compound was formed on the surface of the soft magnetic metal particle powder coated with methylhydrogenpolysiloxane.
得られた軟磁性粒子粉末は、平均粒子径が１１５．３μｍの粒状粒子であり、比抵抗値は５．８Ω・ｃｍ、耐熱性は６８２％であり、耐食性は◎であった。絶縁層を構成するＡｌ２Ｏ３の付着量は、Ａｌ換算で０．５１重量％であった。 The obtained soft magnetic particle powder was a granular particle having an average particle diameter of 115.3 μm, a specific resistance value of 5.8 Ω · cm, a heat resistance of 682%, and a corrosion resistance of ◎. The adhesion amount of Al 2 O 3 constituting the insulating layer was 0.51% by weight in terms of Al.
＜実施例２−１：圧粉磁心の製造＞
前記軟磁性粒子粉末６．０ｇを秤量し、ステアリン酸亜鉛を塗布した金型を用い、成形圧力６８６ＭＰａでリング状（φ２０×φ１０ｍｍ）に圧縮成形し、圧粉磁心（リング成形体）を得た。
<Example 2-1: Production of dust core>
6.0 g of the soft magnetic particle powder was weighed and compression molded into a ring shape (φ20 × φ10 mm) at a molding pressure of 686 MPa using a die coated with zinc stearate to obtain a dust core (ring compact). .
得られた圧粉磁心の、６００℃で１時間焼鈍後の比抵抗値（６００℃）は２１５ｍΩ・ｃｍ、７００℃で１時間焼鈍後の比抵抗値（７００℃）は１０３ｍΩ・ｃｍであった。また、耐食性は前述の評価方法により、目視観察の結果◎であった。 The specific resistance value (600 ° C.) after annealing at 600 ° C. for 1 hour of the obtained dust core was 215 mΩ · cm, and the specific resistance value (700 ° C.) after annealing at 700 ° C. for 1 hour was 103 mΩ · cm. . Further, the corrosion resistance was ◎ as a result of visual observation by the aforementioned evaluation method.
前記実施例１−１及び２−１に従って軟磁性粒子粉末及び圧粉磁心を作製した。各製造条件及び得られた軟磁性粒子粉末及び圧粉磁心の諸特性を示す。 Soft magnetic particle powders and dust cores were prepared according to Examples 1-1 and 2-1. Various characteristics of each production condition and the obtained soft magnetic particle powder and dust core are shown.
軟磁性金属粒子１〜５：
被処理粒子粉末として表１に示す特性を有する軟磁性金属粒子粉末を用意した。
Soft magnetic metal particles 1-5:
A soft magnetic metal particle powder having the characteristics shown in Table 1 was prepared as a particle to be treated.
無機化合物１〜４：
無機化合物として表２に示す特性を有する無機化合物を用意した。
Inorganic compounds 1-4:
An inorganic compound having the characteristics shown in Table 2 was prepared as the inorganic compound.
無機化合物５〜９：
無機化合物の種類、表面改質剤の種類及び添加量、並びに混練機の種類を種々変化させた以外は、前記実施例１−１と同様にして表面改質剤被覆無機化合物を得た。
Inorganic compounds 5-9:
A surface modifier-coated inorganic compound was obtained in the same manner as in Example 1-1 except that the kind of inorganic compound, the kind and addition amount of the surface modifier, and the kind of kneader were varied.
このときの製造条件及び得られた表面改質剤被覆無機化合物の諸特性を表３に示す。 Table 3 shows the production conditions at this time and various characteristics of the obtained surface modifier-coated inorganic compound.
実施例１−２〜１−６、比較例１−１及び１−２：
軟磁性金属粒子粉末の種類、表面改質剤の種類及び添加量、無機化合物の種類及び添加量、並びに混練機の種類を種々変化させた以外は、前記実施例１−１と同様にして軟磁性粒子粉末を得た。
Examples 1-2 to 1-6, Comparative Examples 1-1 and 1-2:
The soft magnetic metal particle powder, the kind and addition amount of the surface modifier, the kind and addition amount of the inorganic compound, and the kind of the kneader were changed variously in the same manner as in Example 1-1. Magnetic particle powder was obtained.
なお、比較例１−１は、特開２００５−２６４１９２号公報に記載の製造法に準じて製造したものである。 In addition, Comparative Example 1-1 is manufactured according to the manufacturing method described in JP-A-2005-264192.
このときの製造条件を表４に、得られた軟磁性粒子粉末の諸特性を表５に示す。 The production conditions at this time are shown in Table 4, and various characteristics of the obtained soft magnetic particle powder are shown in Table 5.
実施例２−２〜２−６及び比較例２−１〜２−７：
軟磁性粒子粉末の種類を種々変化させた以外は、前記実施例２−１と同様にして圧粉磁心を得た。
Examples 2-2 to 2-6 and comparative examples 2-1 to 2-7:
A dust core was obtained in the same manner as in Example 2-1, except that various types of soft magnetic particle powder were used.
得られた圧粉磁心の諸特性を表６に示す。 Table 6 shows various properties of the obtained dust core.
表６の実施例と比較例より、あらかじめ表面改質剤によって分散・被覆された無機化合物からなる絶縁層を有する軟磁性粒子粉末を用いて得られた圧粉磁心の高温（６００℃以上）における焼鈍し後の比抵抗値は、未処理の軟磁性金属粒子粉末もしくは比較例の軟磁性粒子粉末を用いて得られた圧粉磁心のそれと比べて高い値を維持していると共に、優れた耐食性を有していることがわかる。 From the examples and comparative examples in Table 6, at a high temperature (600 ° C. or higher) of a dust core obtained by using a soft magnetic particle powder having an insulating layer made of an inorganic compound previously dispersed and coated with a surface modifier. The specific resistance value after annealing maintains a high value compared with that of the powder magnetic core obtained by using the untreated soft magnetic metal particle powder or the soft magnetic particle powder of the comparative example, and has excellent corrosion resistance. It can be seen that
本発明に係る軟磁性粒子粉末は、耐食性及び耐熱性に優れた絶縁層を有しているので圧粉磁心用軟磁性材料として好適である。 Since the soft magnetic particle powder according to the present invention has an insulating layer excellent in corrosion resistance and heat resistance, it is suitable as a soft magnetic material for a dust core.
本発明に係る軟磁性粒子粉末の製造法によって絶縁層を軟磁性金属粒子粉末の表面に形成した場合、従来の処理方法に比べてより高い耐食性と耐熱性を付与することができるので、圧粉磁心用軟磁性粒子粉末の製造法として好適である。 When the insulating layer is formed on the surface of the soft magnetic metal particle powder by the method for producing the soft magnetic particle powder according to the present invention, higher corrosion resistance and heat resistance can be imparted compared to the conventional processing method. It is suitable as a method for producing soft magnetic particle powder for magnetic cores.
本発明に係る圧粉磁心は、前記軟磁性粒子粉末を用いたことにより、高温で焼成した場合においても比抵抗値が低下しにくく、また、耐食性も優れているので、高性能圧粉磁心として好適である。 Since the powder magnetic core according to the present invention uses the soft magnetic particle powder, the specific resistance value hardly decreases even when baked at a high temperature, and the corrosion resistance is excellent. Is preferred.
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