JP2005213100A - MnZnフェライトの製造方法及びMnZnフェライト - Google Patents
MnZnフェライトの製造方法及びMnZnフェライト Download PDFInfo
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- JP2005213100A JP2005213100A JP2004022453A JP2004022453A JP2005213100A JP 2005213100 A JP2005213100 A JP 2005213100A JP 2004022453 A JP2004022453 A JP 2004022453A JP 2004022453 A JP2004022453 A JP 2004022453A JP 2005213100 A JP2005213100 A JP 2005213100A
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- mnzn ferrite
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 46
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- 239000002245 particle Substances 0.000 claims abstract description 45
- 239000000843 powder Substances 0.000 claims abstract description 39
- 230000004907 flux Effects 0.000 claims abstract description 37
- 238000010304 firing Methods 0.000 claims abstract description 13
- 238000004438 BET method Methods 0.000 claims abstract description 6
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 16
- 238000000465 moulding Methods 0.000 claims description 9
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 7
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 7
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims description 4
- 238000000034 method Methods 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 3
- 238000005056 compaction Methods 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 20
- 238000001354 calcination Methods 0.000 description 13
- 239000002994 raw material Substances 0.000 description 11
- 239000013078 crystal Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 230000007423 decrease Effects 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000011812 mixed powder Substances 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000006866 deterioration Effects 0.000 description 3
- 239000007769 metal material Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 229910020599 Co 3 O 4 Inorganic materials 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 230000002250 progressing effect Effects 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- -1 CaCO 3 Inorganic materials 0.000 description 1
- 229910004140 HfO Inorganic materials 0.000 description 1
- 229910018068 Li 2 O Inorganic materials 0.000 description 1
- 229910021380 Manganese Chloride Inorganic materials 0.000 description 1
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 description 1
- 229910015621 MoO Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 229940099607 manganese chloride Drugs 0.000 description 1
- 235000002867 manganese chloride Nutrition 0.000 description 1
- 239000011565 manganese chloride Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
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Abstract
【課題】 数十kHzから数百kHzの周波数帯域における損失が低く、かつ100℃近傍における飽和磁束密度の高いMnZnフェライトを提供する。
【解決手段】 比表面積(BET法による)が2.0〜5.0m2/g、50%粒径が0.7〜2.0μmである成形用粉末を所定形状の成形体に成形する工程と、成形体を焼成して焼成体を得る工程と、を備えることを特徴とするMnZnフェライトの製造方法。MnZnフェライトとしては、Fe2O3:54〜57mol%、ZnO:5〜10mol%、NiO:4mol%以下(但し、0%を含まず)、残部実質的にMnOを主成分とするものが望ましい。
【選択図】図1
Description
これらトランスやリアクタに使用される材料としては、軟磁性金属材料とMnZnフェライトがある。MnZnフェライトはMnZn系フェライトとNi系フェライトに分類される。
軟磁性金属材料はフェライトに比べて飽和磁束密度が高いため、より大きな電流を流しても磁気飽和を起さない利点がある。しかしながら、軟磁性金属材料は、一般的に損失が大きい、値段が高い、比重が大きい、防錆性に劣るといった問題がある。
一方、フェライトはコストパフォーマンスに優れ、数十kHzから数百kHzの周波数帯域において損失が低いという利点がある。また、Ni系フェライトより飽和磁束密度の高いMnZn系フェライトが一般的に大電流用のトランス及びチョークコイルに使用されている。
また、特許第3389170号公報(特許文献2)は、MnZn系フェライトにNiOを置換することにより飽和磁束密度Bsが440mT以上で直流重畳特性が優れ、広い温度域で使用できることを開示している。
さらに、特開平11−255501号公報(特許文献3)ではMnZn系フェライトにCoOを添加することにより、20〜100℃の広い温度域における電力損失の著しい低減、ならびに温度変化の緩和を達成し、具体的には、電力損失の最小値が400kW/m3以下、かつ、電力損失の最大値と最小値の差が150kW/m3以下の特性を得ている。
また、室温における飽和磁束密度が高くても、一般的なトランス、リアクタ用コアが使用される温度域(80〜120℃)において飽和磁束密度が低下してしまうと、所望するトランス、リアクタ用コアの性能を発揮することができなくなる。特許文献5に開示されたMnZn系フェライトは、数十kHzから数百kHzの周波数帯域における損失は優れているものの、100℃近傍における飽和磁束密度に関する考慮はなされていない。
本発明は、このような技術的課題に基づいてなされたもので、数十kHzから数百kHzの周波数帯域における損失が低く、かつ100℃近傍における飽和磁束密度の高いMnZn系フェライトを提供することを目的とする。
本発明におけるMnZnフェライトは、Fe2O3:54〜57mol%、ZnO:5〜10mol%、NiO:4mol%以下(但し、0%を含まず)、残部実質的にMnOを主成分とすることが望ましい。
また、本発明において、成形用粉末は、90%粒径が4.0μm以下であることが望ましい。さらに、本発明において、成形体の焼成は1250〜1450℃の保持温度で行われることが望ましい。
はじめに成分の限定理由について説明する。
<Fe2O3>
Fe2O3の量が多いと高温域における飽和磁束密度が向上する一方、損失が劣化する傾向にある。Fe2O3が54mol%より少ないと高温域における飽和磁束密度が低下する。一方、Fe2O3が57mol%を超えると損失の増大が顕著となる。したがって、本発明ではFe2O3を54〜57mol%とする。この範囲では、Fe2O3量の増加に伴ってボトム温度は低温側へシフトするが、Fe2O3量が54〜57mol%の範囲内にある場合には、磁気特性を維持し、又は磁気特性の低下を可能な限り抑制しつつ、ボトム温度を85〜120℃の範囲に設定することができる。望ましいFe2O3の量は54.5〜56.5mol%、さらに望ましいFe2O3の量は54.5〜55.5mol%である。
ZnOの量も飽和磁束密度及び損失に影響を与える。ZnOが5mol%より少ないと飽和磁束密度が低下するとともに、損失が大きくなる。また、ZnOが10mol%を超えても飽和磁束密度が低下するとともに、損失が大きくなる。したがって本発明ではZnOを5〜10mol%とする。ZnO量の増加に伴ってボトム温度は低温側へシフトするが、ZnO量が5〜10mol%の範囲内にある場合には、磁気特性を維持し、又は磁気特性の低下を可能な限り抑制しつつ、ボトム温度を85〜120℃の範囲に設定することができる。望ましいZnOの量は6〜9mol%、さらに望ましいZnOの量は7〜8mol%である。
NiOは、キュリー温度を上昇させることにより飽和磁束密度を向上させることができる。但し、NiOの含有量が4mol%を超えると損失が大きくなる。したがって本発明では、飽和磁束密度の向上及び低損失という効果を享受するために、NiOを4mol%以下(但し、0を含まず)の範囲内で含有させる。望ましいNiOの量は0.2〜4mol%、さらに望ましいNiOの量は0.5〜3mol%である。
なお、SiとCaを複合添加する場合には、Si、CaをそれぞれSiO2換算、CaCO3換算でSiO2/CaCO3(重量比)が0.04〜0.25、より望ましくは0.05〜0.2の範囲になるように設定することが有効である。
主成分の原料としては、酸化物又は加熱により酸化物となる化合物の粉末を用いる。具体的には、Fe2O3粉末、Mn3O4粉末、ZnO粉末、NiO粉末等を用いることができる。
主成分の原料粉末を湿式混合した後、仮焼きを行う。仮焼きの保持温度は700〜1000℃の範囲内で、また雰囲気はN2〜大気とすればよい。仮焼きの保持時間は0.5〜5.0時間の範囲で適宜選択すればよい。仮焼き後に仮焼き物を粉砕する。なお、本発明では、上述の主成分の原料に限らず、2種以上の金属を含む複合酸化物の粉末を主成分の原料としてもよい。例えば、塩化鉄、塩化マンガンを含有する水溶液を酸化培焼することによりFe、Mnを含む複合酸化物の粉末が得られる。この粉末とZnO粉末を混合して主成分原料としてもよい。このような場合には、仮焼きは不要である。
主成分及び副成分からなる混合粉末は、比表面積(BET法による)が2.0〜5.0m2/g、50%粒径が0.7〜2.0μmとする。ここで、比表面積(BET法による)が2.0m2/g未満又は5.0m2/gを超えると損失が大きくなる。また、比表面積が2.0m2/g未満になると飽和磁束密度が小さくなる。一方、50%粒径が0.7μm未満又は2.0μmを超えると、損失が大きくなる。また、50%粒径が2.0μmを超えると飽和磁束密度が小さくなる。望ましい比表面積(BET法による)は2.5〜4.0m2/g、望ましい50%粒径は0.9〜1.5μmである。なお、50%粒径とは、累積個数が50%となる粒子の粒径をいう。
成形に供される混合粉末をこのような特性とするためには、仮焼き後の粉砕条件を調整する、あるいは分級する等の公知の手段を適用すればよい。
仮焼き物を粉砕した後に、成形工程を円滑に実行するために顆粒に造粒される。造粒は例えばスプレードライヤを用いて行なうことができる。混合粉末に適当な結合材、例えばポリビニルアルコール(PVA)を少量添加し、これをスプレードライヤで噴霧、乾燥する。顆粒の粒径は80〜200μm程度とすることが望ましい。
焼成工程においては、焼成温度と焼成雰囲気を制御する必要がある。
焼成は1250〜1450℃の範囲で所定時間保持すればよい。本発明のMnZnフェライトの効果を十分に引き出すには、1300〜1400℃の範囲で保持、焼成することが望ましい。
本発明によるMnZnフェライトは、平均結晶粒径が5〜35μmの範囲とすることが望ましい。結晶粒径が小さいとヒステリシス損失が大きくなり、一方結晶粒径が大きいと渦電流損失が大きくなるからである。望ましい平均結晶粒径は8〜30μm、より望ましい平均結晶粒径は10〜25μmである。
本発明のように、焼成前の成形用粉末を上述したように特定することによって、100℃における飽和磁束密度が440mT以上、損失が最小値を示す温度であるボトム温度が85〜120℃、損失の最小値(100kHz、200mT)が350kW/m3以下の特性を有するMnZnフェライトを得ることができる。
次いで、主成分の原料の仮焼き物と副成分の原料とを混合した。副成分の原料として、SiO2粉末、CaCO3粉末、Nb2O5粉末、ZrO2粉末及びCo3O4粉末を用いた。主成分原料の仮焼き物に副成分の原料を添加して、粉砕しながら混合した。なお、粉砕後の混合粉末の比表面積(BET)、50%粒径、90%粒径を測定し、その結果を表1及び表3に示した。得られた混合物にバインダを加え、顆粒化した後、成形してトロイダル形状の成形体を得た。
得られた成形体を酸素分圧制御下において、1300℃(5時間保持、酸素分圧1.5%)及び1325℃(5時間保持、酸素分圧2%)で焼成することにより、フェライトコアを得た。
また、このフェライトコアを用いて、初透磁率(μi,測定温度:25℃、測定周波数:100kHz)、25℃(RT)及び100℃における飽和磁束密度(Bs,測定磁界:1194A/m)、25〜120℃におけるコア損失(Pcv,測定条件:100kHz、200mT)を測定した。その結果を表2(表1の粉末を1300℃で焼成)及び表4(表3の粉末を1325℃で焼成)に示す。表1及び表3より、仮焼き温度が低いほど、また粉砕時間が長いほど粉末の比表面積(BET)が大きくなることが確認できた。
BET:2.5〜4.0m2/g
50%粒径:0.7〜1.5μm
90%粒径:1.0〜4.0μm
次に、ZnOが4.5mol%と少ない場合には、損失が大きくなる。一方、ZnOが11mol%と多い場合には、飽和磁束密度(Bs)が低くなる。
また、NiOが4.5mol%と多くなると損失が大きくなる。
BET:2.5〜4.0m2/g
50%粒径:0.7〜1.5μm
90%粒径:1.0〜4.0μm
また、表7に示すように、CoOを適量添加することにより、ボトム温度における損失を低減できるとともに、25℃〜ボトム温度における損失の変動を低く抑えることができる。
Claims (8)
- 比表面積(BET法による)が2.0〜5.0m2/g、50%粒径が0.7〜2.0μmである成形用粉末を所定形状の成形体に成形する工程と、
前記成形体を焼成して焼成体を得る工程と、
を備えることを特徴とするMnZnフェライトの製造方法。 - 前記MnZnフェライトがFe2O3:54〜57mol%、ZnO:5〜10mol%、NiO:4mol%以下(但し、0%を含まず)、残部実質的にMnOを主成分とすることを特徴とする請求項1に記載のMnZnフェライトの製造方法。
- 前記成形用粉末は、90%粒径が4.0μm以下であることを特徴とする請求項1又は2に記載のMnZnフェライトの製造方法。
- 前記成形体の焼成は、1250〜1450℃の保持温度で行われることを特徴とする請求項1〜3のいずれかに記載のMnZnフェライトの製造方法。
- 第1副成分として、SiをSiO2換算で60〜250ppm及びCaをCaCO3換算で700〜2500ppm含むことを特徴とする請求項1〜4のいずれかに記載のMnZnフェライトの製造方法。
- 第2副成分として、CoO:500〜4000ppm、Nb2O5:50〜500ppm、ZrO2:50〜1000ppm、Ta2O5:50〜1000ppm、V2O5:50〜1000ppm、HfO2:50〜1000ppm、In2O5:50〜2000ppm、MoO3:50〜1000ppm、Bi2O3:50〜1000ppmの1種または2種以上を含むことを特徴とする請求項1〜5のいずれかに記載のMnZnフェライトの製造方法。
- 第3副成分として、SnO2:500〜10000ppm及びTiO2:500〜10000ppmの範囲で1種又は2種を含むことを特徴とする請求項1〜6のいずれかに記載のMnZnフェライトの製造方法。
- Fe2O3:54〜57mol%、ZnO:5〜10mol%、NiO:4mol%以下(但し、0%を含まず)、残部実質的にMnOを主成分とし、かつSiをSiO2換算で60〜250ppm、CaをCaCO3換算で700〜2500ppm及びCoをCoO換算で500〜4000ppmを副成分として含み、平均結晶粒径が5〜35μmである焼成体からなり、
100℃における飽和磁束密度が440mT以上、
損失が最小値を示す温度であるボトム温度が85〜120℃、
損失の最小値(100kHz、200mT)が350kW/m3以下であることを特徴とするMnZnフェライト。
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JP2008127230A (ja) * | 2006-11-17 | 2008-06-05 | Jfe Ferrite Corp | MnZnNiフェライト |
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JP2019006668A (ja) * | 2017-06-23 | 2019-01-17 | Jfeケミカル株式会社 | MnZnNiCo系フェライトおよびその製造方法 |
JP7406022B1 (ja) | 2022-07-26 | 2023-12-26 | Jfeケミカル株式会社 | MnZnCo系フェライト |
WO2024024303A1 (ja) * | 2022-07-26 | 2024-02-01 | Jfeケミカル株式会社 | MnZnCo系フェライト |
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