JP6720878B2 - MnZn系フェライトの製造方法及びMnZn系フェライト - Google Patents
MnZn系フェライトの製造方法及びMnZn系フェライト Download PDFInfo
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Description
Ep=4.44×Np×A×f×Bm×10-7
で現される。
主成分としてFe、Mn及びZnを含み、かつ副成分として少なくともCo、Si及びCaを含むMnZn系フェライトの製造方法であって、
前記MnZn系フェライトの主成分が、Fe2O3換算で53〜56モル%のFe、ZnO換算で3〜9モル%のZn及びMnO換算で残部Mnからなり、
成形体を焼結してMnZn系フェライトを得る工程を有し、
前記焼結は、昇温工程と、高温保持工程と、降温工程とを有し、
前記高温保持工程は、保持温度が1050℃超1150℃未満で、雰囲気中の酸素濃度が0.4〜2体積%であり、
前記降温工程中、900℃から400℃まで降温させる際の酸素濃度を0.001〜0.2体積%の範囲とし、
Fe2O3及びZnOのモル%から計算により求められるキュリー温度をTc(℃)としたとき、(Tc+70)℃から100℃までの間の降温速度を、50℃/時間以上とすることを特徴とする。なお前記キュリー温度(Tc)は、MnZn系フェライトの主成分であるFeの酸化物(Fe2O3)及びZnの酸化物(ZnO)のモル%(配合比率)から算出される値である。詳しくは後述する。
式1:Ps1(%)=[(Pcv max1-Pcv min)/Pcv min]×100
で求めた磁心損失の変化率Ps1が、周波数1 MHz及び励磁磁束密度75 mTにおいて150%以下であり、
式2:Ps2(%)=[(Pcv max2-Pcv min)/Pcv min]×100
で求めた磁心損失の変化率Ps2が、周波数1 MHz及び励磁磁束密度75 mTにおいて200%以下であるのが好ましい。
式1:Ps1(%)=[(Pcv max1-Pcv min)/Pcv min]×100
で求めた磁心損失の変化率Ps1が、周波数1 MHz及び励磁磁束密度75 mTにおいて150%以下であり、
式2:Ps2(%)=[(Pcv max2-Pcv min)/Pcv min]×100
で求めた磁心損失の変化率Ps2が、周波数1 MHz及び励磁磁束密度75 mTにおいて200%以下であるMnZn系フェライトが得られる。
MnZn系フェライトとして表1に示すA〜Kの組成となるように原料粉末を秤量した。主成分の原料には、Fe2O3、Mn3O4及びZnOを用い、これらを湿式混合した後乾燥させ、900℃で2時間仮焼成した。次いで、ボールミルに仮焼成粉と、Co3O4、SiO2、CaCO3、V2O5、Ta2O5及びNb2O5を加えて平均粉砕粒径(空気透過法)が0.8〜1.0 μmとなるまで粉砕・混合した。得られた混合物にバインダとしてポリビニルアルコールを加え、スプレードライヤーにて顆粒化した後、196 MPaで加圧成形してリング状の成形体を得た。得られた成形体を雰囲気調整が可能な電気焼結炉にて焼結して、外径φ14 mm×内径φ7 mm×厚み5 mmの磁心を得た。以下、表含めアルファベット符号やNoに“*“が付されたものは比較例を示す。
* 比較例
磁心損失Pcvは岩崎通信機株式会社製のB-Hアナライザ(SY-8232)を用い、一次側巻線と二次側巻線とをそれぞれ3ターン巻回した磁心に、周波数500 kHz及び1 MHzで励磁磁束密度25 mT、50 mT、75 mT及び100 mTの正弦波交流磁界を印加し、周波数2 MHzで励磁磁束密度25 mT、50 mT及び75 mTの正弦波交流磁界を印加して、0〜140℃における磁心損失を20℃刻みで測定した。
式1: Ps1(%)=[(Pcv max1-Pcv min)/Pcv min]×100、及び
式2: Ps2(%)=[(Pcv max2-Pcv min)/Pcv min]×100
により磁心損失の変化率Ps1及びPs2を算出した。
飽和磁束密度(Bs)は、一次側巻線と二次側巻線とをそれぞれ10回巻回した磁心に、1.2 kA/mの磁界を印加し、直流磁化測定試験装置(メトロン技研株式会社製SK-110型)を用いて20℃において測定した。
初透磁率μiは、10回巻回した磁心に0.4 A/mの磁界を印加し、ヒューレッドパッカード製HP-4284Aを用いて、20℃で100 kHzの条件で測定した。
平均結晶粒径は、鏡面研磨した磁心を、サーマルエッチング(950〜1050℃ で1時間、N2中で処理)し、その表面を光学顕微鏡又は走査型電子顕微鏡で2000倍にて写真撮影し、この写真上の60 μm×40 μmの長方形領域を基準に求積法(JIS H0501-1986相当)により算出した。結晶粒径の大きさによって十分な粒子数(300個以上)がカウントできない場合は、観察される粒子数が300個以上となるよう観察領域を適宜調整した。
フェライト(丸善株式会社、昭和61年11月30日発行、第6刷、79頁)に記載の式:
Tc=12.8[x-(2/3)×z]-358(℃)、[ただし、x及びzはそれぞれFe2O3及びZnOのモル%である。]
により計算で求めた。
* 比較例
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表1に記載の材料組成Aを用いて作製した試料No.1の磁心に対して、焼結時の高温保持工程での保持温度を表3に示すように1025〜1175℃の間で変更し、他の条件は試料No.1と同様にしてMnZn系フェライトの磁心を得た。得られた磁心の磁気特性等を表3に示す。なお、表中の“-”は未評価であることを表し、以降同様である。
* 比較例
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表1に記載の材料組成Aを用いて作製した試料No.1の磁心(Tc=282℃)に対して、150℃/時間の降温速度で352℃まで降温した後、352℃から100℃までの降温速度を表5に示すように5〜300℃/時間の間で変更した以外は試料No.1と同様にしてMnZn系フェライトの磁心を作製した。得られた磁心の磁気特性等を表5に示す。No.1、No.26及びNo.28の磁心損失の温度特性を図3に示す。第2降温工程における降温速度と磁心損失が極小となる温度との関係を図4に示す。
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Claims (8)
- 主成分としてFe、Mn及びZnを含み、かつ副成分として少なくともCo、Si及びCaを含むMnZn系フェライトの製造方法であって、
前記MnZn系フェライトの主成分が、Fe2O3換算で53〜56モル%のFe、ZnO換算で3〜9モル%のZn及びMnO換算で残部Mnからなり、
前記副成分が、前記主成分の酸化物100質量%に対して、Co 3 O 4 換算で0.05〜0.4質量%のCo、SiO 2 換算で0.003〜0.01質量%のSi、CaCO 3 換算で0.06〜0.3質量%のCa、V 2 O 5 換算で0〜0.1質量%のV、並びに合計で0〜0.3質量%のNb (Nb 2 O 5 換算)及び/又はTa (Ta 2 O 5 換算)を含み、
成形体を焼結してMnZn系フェライトを得る工程を有し、
前記焼結は、昇温工程と、高温保持工程と、降温工程とを有し、
前記高温保持工程は、保持温度が1070〜1140℃で、雰囲気中の酸素濃度が0.6〜2体積%であり、
前記降温工程中、900℃から400℃まで降温させる際の酸素濃度を0.001〜0.2体積%の範囲とし、
前記MnZn系フェライトの主成分に含まれるFe2O3及びZnOのモル%から計算により求められるキュリー温度をTc(℃)としたとき、(Tc+70)℃から100℃までの間の降温速度を、50℃/時間以上300℃/時間以下とすることを特徴とするMnZn系フェライトの製造方法。 - 請求項1に記載のMnZn系フェライトの製造方法において、前記高温保持工程は、保持温度が1070〜1130℃であることを特徴とするMnZn系フェライトの製造方法。
- 請求項1又は2に記載のMnZn系フェライトの製造方法において、(Tc+70)℃から100℃までの間の降温速度を、100℃/時間以上150℃/時間以下とすることを特徴とするMnZn系フェライトの製造方法。
- 請求項1〜3のいずれかに記載のMnZn系フェライトの製造方法において、前記降温工程中、900℃での酸素濃度を0.001〜0.1体積%とすることを特徴とするMnZn系フェライトの製造方法。
- 請求項4に記載のMnZn系フェライトの製造方法において、前記降温工程中、900℃での酸素濃度を、0.01〜0.1体積%とすることを特徴とするMnZn系フェライトの製造方法。
- 請求項1〜5のいずれかに記載のMnZn系フェライトの製造方法において、前記昇温工程中、少なくとも900℃以上で、雰囲気中の酸素濃度を0.4〜2体積%の範囲とすることを特徴とするMnZn系フェライトの製造方法。
- 請求項1〜6のいずれかに記載のMnZn系フェライトの製造方法において、
前記副成分が、前記主成分の酸化物100質量%に対して、Co3O4換算で0.05〜0.4質量%のCo、SiO2換算で0.003〜0.015質量%のSi、CaCO3換算で0.06〜0.3質量%のCa、V2O5換算で0〜0.1質量%のV、並びに合計で0〜0.3質量%のNb (Nb2O5換算)及び/又はTa (Ta2O5換算)を含むことを特徴とするMnZn系フェライトの製造方法。 - 主成分としてFe、Mn及びZnを含み、かつ副成分として少なくともCo、Si及びCaを含むMnZn系フェライトであって、
前記主成分が、Fe2O3換算で54〜55モル%のFe、ZnO換算で5〜8モル%のZn及びMnO換算で残部Mnからなり、
前記副成分が、前記主成分の酸化物100質量%に対して、Co3O4換算で0.05〜0.4質量%のCo、SiO2換算で0.003〜0.01質量%のSi、CaCO3換算で0.06〜0.3質量%のCa、V2O5換算で0〜0.1質量%のV、並びに合計で0〜0.3質量%のNb (Nb2O5換算)及び/又はTa (Ta2O5換算)を含み、
平均結晶粒径が2.3〜5μmであって、
磁心損失が極小となる温度が30〜100℃の間にあり、
周波数1 MHz及び励磁磁束密度75 mTにおいて0〜140℃の間の磁心損失Pcvが2090 kW/m3 以下であり、
前記極小となる温度における磁心損失をPcv min、
20〜120℃の間の磁心損失の最大値をPcv max1、及び
0〜140℃の間の磁心損失の最大値をPcv max2としたとき、
式1:Ps1(%)=[(Pcv max1-Pcv min)/Pcv min]×100
で求めた磁心損失の変化率Ps1が、周波数1 MHz及び励磁磁束密度75 mTにおいて150%以下であり、
式2:Ps2(%)=[(Pcv max2-Pcv min)/Pcv min]×100
で求めた磁心損失の変化率Ps2が、周波数1 MHz及び励磁磁束密度75 mTにおいて200%以下であることを特徴とするMnZn系フェライト。
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