JP5929764B2 - フェライト焼結磁石及びその製造方法 - Google Patents
フェライト焼結磁石及びその製造方法 Download PDFInfo
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Description
0.3≦1-x-y≦0.75、
0.2≦x≦0.65、
0≦y≦0.2、
0.25≦z≦0.65、及び
3≦n≦6
を満足する数値であり、1質量%を超え1.8質量%以下のSiO2を含有するのが好ましい。
0.3≦1-x-y<0.65、
0.3<x≦0.65、
1-x-y<x、
0≦y≦0.2、
0.25≦z≦0.65、及び
4.5≦n≦7
を満足するように原料粉末を準備する工程、
前記原料粉末を仮焼し、仮焼体を得る仮焼工程、
前記仮焼体を粉砕し、粉末を得る粉砕工程、
前記粉末を成形し、成形体を得る成形工程、
前記成形体を焼成し、焼結体を得る焼成工程を含み、
前記粉砕工程の前に、前記仮焼体に、仮焼体100質量%に対して、1質量%を超え1.8質量%以下のSiO2及びCaO換算で1質量%以上2質量%以下のCaCO3を添加することを特徴とする。
本発明のフェライト焼結磁石は、六方晶のM型マグネトプランバイト構造を有するフェライト相を主相とし、SiとCaとを含み前記主相よりもLaの原子比率が低い粒界相と、Laを含み前記主相よりもLaの原子比率が高い第3相を有することを特徴とする。
前記1-x-y、x、y及びz、並びにモル比を表わすnが、
0.3≦1-x-y≦0.75、
0.2<x≦0.65、
0≦y≦0.2、
0.25≦z≦0.65、及び
3≦n≦6
を満足する数値であり、1質量%を超え1.8質量%以下のSiO2を含有する。
Caと、Laと、Ba及び/又はSrであるA元素と、Feと、Coとを含み、主相、粒界相及び第3相を有する本発明のフェライト焼結磁石を製造する方法は、
前記金属元素の組成比を原子比率で表す一般式:Ca1-x-yLaxAyFe2n-zCozにおいて、前記1-x-y、x、y及びz、並びにモル比を表わすnが、
0.3≦1-x-y<0.65、
0.3<x≦0.65、
1-x-y<x、
0≦y≦0.2、
0.25≦z≦0.65、及び
4.5≦n≦7
を満足するように原料粉末を準備する工程、
前記原料粉末を仮焼し、仮焼体を得る仮焼工程、
前記仮焼体を粉砕し、粉末を得る粉砕工程、
前記粉末を成形し、成形体を得る成形工程、
前記成形体を焼成し、焼結体を得る焼成工程を含み、
前記粉砕工程の前に、前記仮焼体に、仮焼体100質量%に対して、1質量%を超え1.8質量%以下のSiO2及びCaO換算で1質量%以上2質量%以下のCaCO3を添加することを特徴とする。各工程について以下に説明する。
Caの化合物、Laの化合物、Ba及び/又はSrの化合物、Feの化合物及びCoの化合物を、金属元素が一般式:Ca1-x-yLaxAyFe2n-zCoz(原子比率)[ただし、1-x-y、x、y及びz並びにモル比を表わすnは、
0.3≦1-x-y<0.65、
0.3<x≦0.65、
1-x-y<x、
0≦y≦0.2、
0.25≦z≦0.65、及び
4.5≦n≦7
を満足する数値である。]で表される組成比となるように混合し、原料粉末を準備する。
一般式:Ca1-x-yLaxAyFe2n-zCozOα(原子比率)[ただし、1-x-y、x、y、z及びα、並びにモル比を表わすnは、
0.3≦1-x-y<0.65、
0.3<x≦0.65、
1-x-y<x、
0≦y≦0.2、
0.25≦z≦0.65、及び
4.5≦n≦7
を満たし、LaとFeが3価でCoが2価であり、x=yでかつn=6の時の化学量論組成比を示した場合はα=19である。]
混合後の原料粉末は、電気炉、ガス炉等を用いて加熱することによって、固相反応し、六方晶のM型マグネトプランバイト構造のフェライト化合物を形成する。このプロセスを「仮焼」と呼び、得られた化合物を「仮焼体」と呼ぶ。
本発明の製造方法は、粉砕工程の前に、仮焼体100質量%に対して、1質量%を超え1.8質量%以下のSiO2及びCaO換算で1質量%以上2質量%以下のCaCO3を添加する。これが本発明の製造方法における第2の特徴である。これによって、HcJが特異的に向上する。
仮焼体は、振動ミル、ボールミル、アトライター等によって粉砕し、粉砕粉とする。粉砕粉の平均粒度は0.4〜0.8μm程度(空気透過法)にするのが好ましい。粉砕工程は、乾式粉砕及び湿式粉砕のいずれもよいが、双方を組み合わせて行うのが好ましい。
粉砕後のスラリーは、水(溶剤)を除去しながら磁界中又は無磁界中でプレス成形する。磁界中でプレス成形することにより、粉末粒子の結晶方位を整列(配向)させることができ、磁石特性を飛躍的に向上させることができる。さらに、配向を向上させるために、分散剤、潤滑剤を0.01〜1質量%添加しても良い。また成形前にスラリーを必要に応じて濃縮してもよい。濃縮は遠心分離、フィルタープレス等により行うのが好ましい。
プレス成形により得られた成形体は、必要に応じて脱脂した後、焼成する。焼成は、電気炉、ガス炉等を用いて行う。焼成は、酸素濃度が10%以上の雰囲気中で行うのが好ましい。酸素濃度が10%未満であると、異常粒成長、異相の生成等を招き、磁石特性が劣化する。酸素濃度は、より好ましくは20%以上であり、最も好ましくは100%である。焼成温度は、1150℃〜1250℃が好ましい。焼成時間は、0.5〜2時間が好ましい。焼成工程によって得られる焼結磁石の平均結晶粒径は約0.5〜2μmである。
本発明を実施例によりさらに詳細に説明するが、本発明はそれらに限定されるものではない。
組成式:Ca1-x-yLaxAyFe2n-zCozOδにおいて、x=0.55、y=0、z=0.3、n=5.2及びδ≧0になるようにCaCO3粉末、La(OH)3粉末、Fe2O3粉末及びCo3O4粉末を配合し、前記配合後の粉末の合計100質量%に対してH3BO3粉末を0.1質量%添加し原料粉末を得た。この原料粉末を湿式ボールミルで4時間混合し、乾燥して整粒した。次いで、大気中において1300℃で3時間仮焼し、得られた仮焼体をハンマーミルで粗粉砕して粗粉砕粉を得た。
組成式:Ca1-x-yLaxAyFe2n-zCozOδにおいて、x=0.5、y=0、z=0.3、n=5.2及びδ≧0、すなわちCa含有量 (1-x-y)とLa含有量 (x)とが同じ値になるようにCaCO3粉末、La(OH)3粉末、Fe2O3粉末及びCo3O4粉末を配合した以外は実施例1と同様にして、円柱状の焼結磁石を得た。得られた円柱状の焼結磁石のLa分布を、実施例1と同様にして、FE-SEM(電界放射型走査電子顕微鏡)を用いて求めた。結果を図3(A)〜(D)及び図4(A)〜(D)に示す。図3(A)〜(D)がc面、及び図4(A)〜(D)がab面を示す。
実施例1において、反射電子像の組成コントラストにより求めた主相よりもLaの原子比率が高い第3相及びその周辺に対して、FIB(収束イオンビーム)加工を施して表面を切削し、FE-TEM(電界放射型透過電子顕微鏡)による組織観察、及びEDS(エネルギー分散型X線分光法)による組成分析を行った。前記組織観察の結果を図5〜7に示し、前記組成分析の結果を表2に示す。なお、表2の数値は全て原子比率(%)で示した。
組成式:Ca1-x-yLaxSry'Bay''Fe2n-zCozOδ(δ≧0)において、1-x-y、x、y’、y’’、z及びnが表3に示す値となるようにCaCO3粉末、La(OH)3粉末、Fe2O3粉末及びCo3O4粉末を配合し、粉砕時に添加するSiO2及びCaCO3の添加量、及び焼成温度を表3に示すように変更した以外は、実施例1と同様にして焼結磁石を得た。第3相の有無は、実施例1と同様の方法で反射電子像の組成コントラストにより評価し、体積比率で0.5%〜5%存在するものを「有」、及び体積比率で0.5%未満のものを「無」とした。得られた焼結磁石の磁石特性を表3に示す。なお、Hk/HcJにおいて、Hkは、J(磁化の大きさ)-H(磁界の強さ)曲線の第2象限において、Jが0.95Brの値になる位置のHの値である。
Claims (6)
- 六方晶のM型マグネトプランバイト構造を有するフェライトからなる主相と、Si及びCaを含み前記主相よりもLaの原子比率が低い粒界相と、La、Ca、Si及びFeを含み、前記元素の合計量を100原子%として、8原子%〜50原子%のLa、20原子%〜45原子%のCa、20原子%〜45原子%のSi、及び4原子%〜20原子%のFeからなる構成比率を有し、前記主相よりもLaの原子比率が高い第3相とを有し、前記第3相の存在量が体積比率で0.5%〜5%であることを特徴とするフェライト焼結磁石。
- 請求項1に記載のフェライト焼結磁石において、前記第3相の存在量が体積比率で1%〜3%であることを特徴とするフェライト焼結磁石。
- 請求項1又は2に記載のフェライト焼結磁石において、Caと、Laと、Ba及び/又はSrであるA元素と、Feと、Coとを含み、前記金属元素の組成比が、原子比率で一般式:Ca1-x-yLaxAyFe2n-zCozにより表され、
前記1-x-y、x、y及びz、並びにモル比を表わすnが、
0.3≦1-x-y≦0.75、
0.2≦x≦0.65、
0≦y≦0.2、
0.25≦z≦0.65、及び
3≦n≦6
を満足する数値であり、1質量%を超え1.8質量%以下のSiO2を含有することを特徴とするフェライト焼結磁石。 - 六方晶のM型マグネトプランバイト構造を有するフェライトからなる主相と、Si及びCaを含み前記主相よりもLaの原子比率が低い粒界相と、La、Ca、Si及びFeを含み、前記元素の合計量を100原子%として、8原子%〜50原子%のLa、20原子%〜45原子%のCa、20原子%〜45原子%のSi、及び4原子%〜20原子%のFeからなる構成比率を有し、前記主相よりもLaの原子比率が高い第3相とを有し、前記第3相の存在量が体積比率で0.5%〜5%であり、
Caと、Laと、Ba及び/又はSrであるA元素と、Feと、Coとを含むフェライト焼結磁石の製造方法であって、
前記金属元素の組成比を原子比率で表す一般式:Ca1-x-yLaxAyFe2n-zCozにおいて、
前記1-x-y、x、y及びz、並びにモル比を表わすnが、
0.3≦1-x-y<0.65、
0.3<x≦0.65、
1-x-y<x、
0≦y≦0.2、
0.25≦z≦0.65、及び
4.5≦n≦7
を満足するように原料粉末を準備する工程、
前記原料粉末を仮焼し、仮焼体を得る仮焼工程、
前記仮焼体を粉砕し、粉末を得る粉砕工程、
前記粉末を成形し、成形体を得る成形工程、
前記成形体を焼成し、焼結体を得る焼成工程を含み、
前記粉砕工程の前に、前記仮焼体に、仮焼体100質量%に対して、1質量%を超え1.8質量%以下のSiO2及びCaO換算で1質量%以上2質量%以下のCaCO3を添加することを特徴とするフェライト焼結磁石の製造方法。 - 請求項4に記載のフェライト焼結磁石の製造方法において、前記SiO2の添加量が1.1質量%以上1.6質量%以下であることを特徴とするフェライト焼結磁石の製造方法。
- 請求項4又は5に記載のフェライト焼結磁石の製造方法において、前記CaCO3の添加量がCaO換算で1.2質量%以上2質量%以下であることを特徴とするフェライト焼結磁石の製造方法。
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WO2007060757A1 (ja) * | 2005-11-25 | 2007-05-31 | Hitachi Metals, Ltd. | 酸化物磁性材料及びその製造方法、並びにフェライト焼結磁石及びその製造方法 |
JP2008137879A (ja) * | 2005-12-19 | 2008-06-19 | Tdk Corp | フェライト磁性材料 |
WO2008105449A1 (ja) * | 2007-03-01 | 2008-09-04 | Tdk Corporation | フェライト焼結磁石 |
WO2008146712A1 (ja) * | 2007-05-25 | 2008-12-04 | Hitachi Metals, Ltd. | フェライト焼結磁石及びその製造方法、並びに仮焼体及びその製造方法 |
JP2010001171A (ja) * | 2008-06-18 | 2010-01-07 | Hitachi Metals Ltd | 磁気記録媒体用フェライト粒子 |
WO2011001831A1 (ja) * | 2009-06-30 | 2011-01-06 | 日立金属株式会社 | フェライト焼結磁石の製造方法及びフェライト焼結磁石 |
Cited By (3)
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KR20200010264A (ko) * | 2017-05-24 | 2020-01-30 | 히타치 긴조쿠 가부시키가이샤 | 페라이트 소결 자석 |
KR102166901B1 (ko) * | 2017-05-24 | 2020-10-16 | 히타치 긴조쿠 가부시키가이샤 | 페라이트 소결 자석 |
US11289250B2 (en) | 2017-05-24 | 2022-03-29 | Hitachi Metals, Ltd. | Sintered ferrite magnet |
Also Published As
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JPWO2012090935A1 (ja) | 2014-06-05 |
WO2012090935A1 (ja) | 2012-07-05 |
US9401235B2 (en) | 2016-07-26 |
KR20130130766A (ko) | 2013-12-02 |
CN103282977B (zh) | 2016-06-08 |
BR112013016925A2 (pt) | 2020-10-27 |
EP2660830B1 (en) | 2020-12-09 |
EP2660830A4 (en) | 2018-01-31 |
BR112013016925B1 (pt) | 2021-10-26 |
US20130285779A1 (en) | 2013-10-31 |
CN103282977A (zh) | 2013-09-04 |
KR101858484B1 (ko) | 2018-06-27 |
EP2660830A1 (en) | 2013-11-06 |
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