JP2017119908A - 圧粉磁心用粉末およびその製造方法ならびに圧粉磁心およびその製造方法 - Google Patents
圧粉磁心用粉末およびその製造方法ならびに圧粉磁心およびその製造方法 Download PDFInfo
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- JP2017119908A JP2017119908A JP2016103244A JP2016103244A JP2017119908A JP 2017119908 A JP2017119908 A JP 2017119908A JP 2016103244 A JP2016103244 A JP 2016103244A JP 2016103244 A JP2016103244 A JP 2016103244A JP 2017119908 A JP2017119908 A JP 2017119908A
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- powder
- ferrite
- magnetic core
- heat treatment
- soft magnetic
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- Granted
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- 239000000843 powder Substances 0.000 title claims abstract description 293
- 238000000034 method Methods 0.000 title claims abstract description 41
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 227
- 238000010438 heat treatment Methods 0.000 claims abstract description 87
- 238000000576 coating method Methods 0.000 claims abstract description 85
- 239000011248 coating agent Substances 0.000 claims abstract description 82
- 238000000137 annealing Methods 0.000 claims abstract description 80
- 239000002923 metal particle Substances 0.000 claims abstract description 53
- 239000013078 crystal Substances 0.000 claims abstract description 45
- 239000010419 fine particle Substances 0.000 claims abstract description 42
- 238000000634 powder X-ray diffraction Methods 0.000 claims abstract description 22
- 229910052596 spinel Inorganic materials 0.000 claims abstract description 15
- 239000011029 spinel Substances 0.000 claims abstract description 15
- 239000006249 magnetic particle Substances 0.000 claims abstract description 11
- 239000000428 dust Substances 0.000 claims description 60
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- 230000008569 process Effects 0.000 claims description 10
- 239000011261 inert gas Substances 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 229910052725 zinc Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 8
- 229910052748 manganese Inorganic materials 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 6
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- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 239000006247 magnetic powder Substances 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 33
- 238000000465 moulding Methods 0.000 abstract description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 53
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- 239000011701 zinc Substances 0.000 description 9
- 229910045601 alloy Inorganic materials 0.000 description 8
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 238000001125 extrusion Methods 0.000 description 3
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- 239000011572 manganese Substances 0.000 description 3
- 238000013507 mapping Methods 0.000 description 3
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- 229910020516 Co—V Inorganic materials 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
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- 229910002796 Si–Al Inorganic materials 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
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- LYRFLYHAGKPMFH-UHFFFAOYSA-N octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(N)=O LYRFLYHAGKPMFH-UHFFFAOYSA-N 0.000 description 2
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- 238000000550 scanning electron microscopy energy dispersive X-ray spectroscopy Methods 0.000 description 2
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- 229910017135 Fe—O Inorganic materials 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
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- 238000000921 elemental analysis Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
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- 238000002347 injection Methods 0.000 description 1
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- HGPXWXLYXNVULB-UHFFFAOYSA-M lithium stearate Chemical compound [Li+].CCCCCCCCCCCCCCCCCC([O-])=O HGPXWXLYXNVULB-UHFFFAOYSA-M 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
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- 238000010298 pulverizing process Methods 0.000 description 1
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- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
Classifications
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- H01F10/20—Ferrites
Abstract
【解決手段】圧粉磁心用粉末1は、軟磁性金属粒子21と、軟磁性金属粒子21の表面を被覆するフェライト被膜22とを有する軟磁性粒子2の集合体である。フェライト被膜22は、スピネル構造を有するフェライト結晶粒221より構成されている。圧粉磁心用粉末1は、粉末X線回折パターン10にフェライト結晶粒221に由来する回折ピーク101が存在している。圧粉磁心用粉末1の製造方法では、軟磁性金属粒子21の表面にフェライト微粒子220を多数形成し、フェライト微粒子220を熱処理により粗大結晶化させることにより、フェライト被膜22を形成する。
【選択図】図2
Description
上記フェライト被膜は、スピネル構造を有するフェライト結晶粒(221)より構成されており、
粉末X線回折パターン(10)に上記フェライト結晶粒に由来する回折ピーク(101)が存在している、圧粉磁心用粉末(1)にある。
該原料粉末における各軟磁性金属粒子の表面にフェライト微粒子(220)を多数形成し、
該フェライト微粒子を熱処理により粗大結晶化させ、上記各軟磁性金属粒子の表面にスピネル構造を有するフェライト結晶粒(221)より構成されるフェライト被膜(22)を形成する、圧粉磁心用粉末の製造方法にある。
得られた圧粉成形体を焼鈍する焼鈍工程と、
焼鈍された圧粉成形体に含まれるフェライト被膜に部分的に生じたFeOを熱処理により再フェライト化する変態熱処理工程とを有する、圧粉磁心の製造方法にある。
実施形態1の圧粉磁心用粉末について、図1〜図3を用いて説明する。図1〜図3に例示されるように、本実施形態の圧粉磁心用粉末1は、軟磁性粒子2の集合体である。軟磁性粒子2は、軟磁性金属粒子21と、軟磁性金属粒子21の表面を被覆するフェライト被膜22とを有している。フェライト被膜22は、スピネル構造を有するフェライト結晶粒221より構成されている。圧粉磁心用粉末1は、粉末X線回折パターン10にフェライト結晶粒221に由来する回折ピーク101が存在している。以下、詳説する。
実施形態2の圧粉磁心用粉末の製造方法について、図4を用いて説明する。なお、実施形態2以降において用いられる符号のうち、既出の実施形態において用いた符号と同一のものは、特に示さない限り、既出の実施形態におけるものと同様の構成要素等を表す。
実施形態2の圧粉磁心について、図5を用いて説明する。図5に例示されるように、本実施形態の圧粉磁心4は、圧粉磁心用粉末1の圧粉成形体であり、かつ、歪が除去されている。本実施形態では、圧粉磁心4を構成する圧粉磁心用粉末1として、実施形態1の圧粉磁心用粉末を用いることができる。
実施形態4の圧粉磁心について、図5を用いて説明する。本実施形態の圧粉磁心4は、粉末X線回折パターンにFeOに由来する回折ピークが存在していない。なお、圧粉磁心4の粉末X線回折パターンは、Cu管球をX線源とした粉末X線回折装置(Rigaku社製、「RINT2000」)またはこれと同等の装置を用い、圧粉磁心4の破断面試料にて測定される。その他の構成は、実施形態3と同様である。
実施形態5の圧粉磁心の製造方法について説明する。本実施形態の圧粉磁心の製造方法は、圧粉成形工程と、焼鈍工程と、変態熱処理工程とを有している。
<実験例1>
ガス水アトマイズ法を用いて、純鉄粒子の集合体より構成される原料粉末を準備した。上述した方法により特定される純鉄粒子の粒子径は、150μmであった。
圧粉磁心用粉末におけるフェライト被膜の圧縮強度を向上させるための製造条件について検討するため、以下の基礎実験を行った。
実験例1で作製したフェライト被覆粉末(熱処理なし)、試料1の圧粉磁心用粉末(600℃で熱処理)、および、試料2の圧粉磁心用粉末(400℃で熱処理)を準備した。これら各粉末を圧粉成形した後、所定の焼鈍温度で焼鈍することにより、複数の圧粉磁心を作製し、渦損失を測定した。本実験例は、圧粉磁心の耐熱性を評価するためのものである。
圧粉成形後の圧粉成形体に対して焼鈍を行った後、さらに変態熱処理を実施した場合の効果について検討するため、以下の基礎実験を行った。
2.5時間変態熱処理を施した。これにより、試験体3を得た。その後、試験体2(600℃焼鈍後)および試験体3(500℃変態熱処理後)の体積固有抵抗を測定した。その結果、試験体2の体積固有抵抗は、6.08×103[μΩ・m]、試験体3の体積固有抵抗は、4.42×105[μΩ・m]であった。このことから、圧粉成形体の歪取り焼鈍後に、変態熱処理を施すことにより、圧粉磁心の比抵抗を回復させることが可能であることが確認された。そこで、変態熱処理前後のフェライト被膜の被膜構造を分析するため、試験体2(600℃焼鈍後)および試験体3(500℃変態熱処理後)について、上記と同様にして、SEM−EDX分析による元素分析と粉末X線回折による結晶構造分析を行った。その結果を、図19、図20に示す。
2 軟磁性粒子
21 軟磁性金属粒子
22 フェライト被膜
221 フェライト結晶粒
10 粉末X線回折パターン
101 回折ピーク
3 原料粉末
220 フェライト微粒子
4 圧粉磁心
Claims (15)
- 軟磁性金属粒子(21)と、該軟磁性金属粒子の表面を被覆するフェライト被膜(22)とを有する軟磁性粒子(2)の集合体であって、
上記フェライト被膜は、スピネル構造を有するフェライト結晶粒(221)より構成されており、
粉末X線回折パターン(10)に上記フェライト結晶粒に由来する回折ピーク(101)が存在している、圧粉磁心用粉末(1)。 - 上記フェライト結晶粒の大きさは、10nm以上である、請求項1に記載の圧粉磁心用粉末。
- 上記フェライト被膜は、断面視で、上記フェライト結晶粒同士の界面(222)が直線状を呈する部分を含む、請求項1または2に記載の圧粉磁心用粉末。
- 上記回折ピークの半値幅は、0.5°以下である、請求項1〜3のいずれか1項に記載の圧粉磁心用粉末。
- 上記フェライト被膜の化学組成は、MXFe2O4、但し、Mは、Fe、Cu、Mg、Ni、Zn、および、Mnからなる群より選択される少なくとも1種の金属元素であり、0<X≦1である、請求項1〜4のいずれか1項に記載の圧粉磁心用粉末。
- 上記金属元素Mは、MnおよびZn、または、NiおよびZnを含む、請求項5に記載の圧粉磁心用粉末。
- 上記フェライト被膜の膜厚は、20nm〜600nmの範囲内にある、請求項1〜6のいずれか1項に記載の圧粉磁心用粉末。
- 軟磁性金属粒子(21)の集合体より構成される原料粉末(3)を準備し、
該原料粉末における各軟磁性金属粒子の表面にフェライト微粒子(220)を多数形成し、
該フェライト微粒子を熱処理により粗大結晶化させ、上記各軟磁性金属粒子の表面にスピネル構造を有するフェライト結晶粒(221)より構成されるフェライト被膜(22)を形成する、圧粉磁心用粉末の製造方法。 - 上記熱処理時の熱処理温度は、400〜900℃の範囲内にある、請求項8に記載の圧粉磁心用粉末の製造方法。
- 上記熱処理時の雰囲気は、不活性ガス雰囲気、または、真空雰囲気である、請求項8または9に記載の圧粉磁心用粉末の製造方法。
- 請求項1〜7に記載の圧粉磁心用粉末の圧粉成形体であり、かつ、歪が除去されている、圧粉磁心(4)。
- 粉末X線回折パターンにFeOに由来する回折ピークが存在していない、請求項11に記載の圧粉磁心。
- 請求項1〜7に記載の圧粉磁心用粉末を圧粉成形する圧粉成形工程と、
得られた圧粉成形体を焼鈍する焼鈍工程と、
焼鈍された圧粉成形体に含まれるフェライト被膜に部分的に生じたFeOを熱処理により再フェライト化する変態熱処理工程とを有する、圧粉磁心の製造方法。 - 上記変態熱処理工程における熱処理温度は、560℃以下である、請求項13に記載の圧粉磁心の製造方法。
- 上記変態熱処理工程における雰囲気は、水蒸気雰囲気、または、不活性ガス雰囲気である、請求項13または14に記載の圧粉磁心の製造方法。
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