JP6583631B2 - フェライト焼結磁石 - Google Patents
フェライト焼結磁石 Download PDFInfo
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- JP6583631B2 JP6583631B2 JP2016006460A JP2016006460A JP6583631B2 JP 6583631 B2 JP6583631 B2 JP 6583631B2 JP 2016006460 A JP2016006460 A JP 2016006460A JP 2016006460 A JP2016006460 A JP 2016006460A JP 6583631 B2 JP6583631 B2 JP 6583631B2
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Description
Ca1−w−xLawAxFezComO19・・・(1)
前記式(1)中、w、x、zおよびmは、下記式(2)、(3)、(4)および(5)を満たし、
0.30≦w≦0.50 (2)
0.08≦x≦0.20 (3)
8.55≦z≦10.00 (4)
0.20≦m≦0.40 (5)
AはSrおよびBaからなる群より選ばれる少なくとも1種の元素であり、
さらにCrをCr2O3換算で0.058質量%〜0.132質量%含むことを特徴とするフェライト焼結磁石。
前記フェライト焼結磁石中のCr2O3の含有量x1質量%をX軸に表したときに、
x1とy1の関係が、前記X軸およびY軸を持つX−Y座標における6つの点a1(0.058,10.25)、b1(0.119,10.25)、c1(0.132,9.30)、d1(0.119,9.30)、e1(0.100,8.75)およびf1(0.058,8.75)で囲まれる範囲内にある前記[1]に記載のフェライト焼結磁石。
本実施形態に係るフェライト焼結磁石の全体構成について説明する。
Ca1−w−xLawAxFezComO19・・・(1)
0.30≦w≦0.50 (2)
0.08≦x≦0.20 (3)
8.55≦z≦10.00 (4)
0.20≦m≦0.40 (5)
次に、本発明の一実施形態としてのフェライト焼結磁石の製造方法について具体的に説明する。
配合工程では、フェライト焼結磁石の原料を配合して、原料混合物を得る。まず、フェライト焼結磁石の原料としては、これを構成する元素のうちの1種または2種以上を含む化合物(原料化合物)が挙げられる。原料化合物は、例えば粉末状のものが好適である。
仮焼工程では、配合工程で得られた原料粉末を仮焼する。仮焼は、例えば、空気中等の酸化性雰囲気中で行うことが好ましい。仮焼の温度は、1100°C〜1400°Cの温度範囲とすることが好ましく、1100°C〜1300°Cがより好ましく、1150°C〜1300°Cがさらに好ましい。仮焼の時間は、1秒間〜10時間とすることができ、1秒間〜5時間であると好ましい。
粉砕工程では、仮焼工程で顆粒状や塊状となった仮焼体を粉砕し、再び粉末状にする。これにより、後述する成形工程での成形が容易となる。この粉砕工程では、前述したように、配合工程で配合しなかった原料を添加してもよい(原料の後添加)。粉砕工程は、例えば、仮焼体を粗い粉末となるように粉砕(粗粉砕)した後、これをさらに微細に粉砕する(微粉砕)、2段階の工程で行ってもよい。
成形・焼成工程では、粉砕工程後に得られた粉砕材(好ましくは微粉砕材)を成形して成形体を得た後、この成形体を焼成して焼結体を得る。成形は、乾式成形、湿式成形またはCIM成形(Ceramic Injection Molding(セラミック射出成形))のいずれの方法でも行うことができるが、好ましくは、CIM成形または湿式成形であり、特に好ましくはCIM成形である。
CIM成形法によってフェライト焼結磁石を得る場合には、湿式粉砕後、磁性粉末を含む微粉砕スラリーを乾燥させる。乾燥温度は、好ましくは80°C〜500°C、さらに好ましくは100°C〜400°Cである。また、乾燥時間は、好ましくは1秒間〜100時間、さらに好ましくは1秒間〜50時間である。乾燥後の磁性粉末の水分量は、好ましくは1.0質量%以下、さらに好ましくは0.5質量%以下である。乾燥後の磁性粉末の一次粒子の平均粒径は、好ましくは0.08μm〜2μmの範囲内、さらに好ましくは0.1μm〜1μmの範囲内である。
湿式成形法によってフェライト焼結磁石を得る場合は、例えば、上述した微粉砕工程を湿式で行うことでスラリーを得た後、このスラリーを所定の濃度に濃縮して、湿式成形用スラリーを得、これを用いて成形を行うことが好ましい。
<配合工程>
出発原料として、CaCO3、La2O3、SrCO3、Fe2O3(不純物としてAlを含む)、Co3O4を準備し、表1〜表4に記載の各試料の組成になるように秤量した。また、Cr2O3を表1〜表4に記載の各試料の組成になるように秤量した。また、Si成分としてSiO2を前記出発原料100質量%に対して0.33質量%秤量した。
この原料混合物を乾燥後、大気中、1200°Cで2時間保持する仮焼処理を行い、仮焼体を得た。
得られた仮焼体をロッドミルにて粗粉砕し、粗粉砕材を得た。焼成後のフェライト焼結磁石を構成する金属元素の比率が、表1〜表4に記載の各試料に示す値となるように、得られた粗粉砕材に対して、CaCO3、La2O3、SrCO3、Fe2O3(不純物としてAlを含む)、Co3O4、SiO2およびCr2O3を、それぞれ適宜添加した。
次に、湿式磁場成形機を使用して予備成形体を得た。成形圧力は、50MPa、印加磁場は800kA/mとした。また、成形時の加圧方向と磁場印加方向は、同一方向に設定した。湿式成形で得られた予備成形体は円板状であり、直径30mm、高さ15mmであった。
実施例2では、表5に示す通り、A元素種としてSrとBaを用い、Srの原子比率を0.08として、Baの原子比率を0.07として、「Aの原子比率x」を0.15(=0.08+0.07)とした以外は、実施例1と同様にしてフェライト焼結磁石を得た。
実施例3では、表6に示すとおり、Feの原子比率(z)を変化させた試料を作製した以外は実施例1と同様にしてフェライト焼結磁石を得た。
実施例4は、配合工程において、出発原料およびCr2O3の他に、SiO2を準備し、SiO2を表7に記載の各試料の組成になるように秤量し、仮焼工程において、出発原料、Cr2O3の他に、SiO2の粉末を湿式アトライタにて混合等して、実施例1と同様にして仮焼体を得た。また、実施例4では、粉砕工程において、表7に記載の各試料に示す値となるように、得られた粗粉砕材に対して、CaCO3、La2O3、SrCO3、Fe2O3(不純物としてAlを含む)、Co3O4、Cr2O3およびSiO2を、適宜添加等して実施例1と同様にしてフェライト材料粉末を得た。実施例4では、上記した工程以外は実施例1と同様にしてフェライト焼結磁石を得た。
実施例5では、表8に示す通り、Cr2O3の含有量とFeの原子比率(z)を変化させた試料を作製した以外は実施例1と同様にしてフェライト焼結磁石を得た。
実施例6は、配合工程において、出発原料およびCr2O3の他に、Sを準備し、Sを表9に記載の各試料の組成になるように秤量し、仮焼工程において、出発原料、Cr2O3の他に、Sの粉末を湿式アトライタにて混合等して、実施例1と同様にして仮焼体を得た。また、実施例6では、粉砕工程において、表9に記載の各試料に示す値となるように、得られた粗粉砕材に対して、CaCO3、La2O3、SrCO3、Fe2O3(不純物としてAlを含む)、Co3O4、Cr2O3およびSを、適宜添加等して実施例1と同様にしてフェライト材料粉末を得た。実施例5では、上記した工程以外は実施例1と同様にしてフェライト焼結磁石を得た。
実施例7の試料番号171〜180は、実施例1と同様にしてフェライト焼結磁石を得た。試料番号171〜180のフェライト焼結磁石に含まれるAl2O3は主にFe2O3の不純物に由来する。
実施例1〜実施例7の各フェライト焼結磁石の上下面を加工した後、25°Cの大気雰囲気中にて、最大印加磁場1989kA/mのB−Hトレーサを使用して磁気特性(残留磁束密度Br、保磁力HcJ、角形比Hk/HcJ)を測定した。実施例1〜実施例5の結果を表1〜表8に示す。また、実施例6および実施例7の結果を後述する。ここで、Hkは磁気ヒステリシスループの第2象限において、磁束密度が残留磁束密度の90%になるときの外部磁界強度である。
実施例6では、下記の方法により、配管腐食を評価した。
実施例6の予備成形体を100個準備し、大気雰囲気中の焼成炉で100回繰り返し焼成した後、焼成炉の排気口の配管を目視にて確認した。表9では、配管に腐食がない場合を最も良い場合としてAとし、腐食が若干ある場合を非常に良い場合としてBとし、腐食がある場合を良い場合としてCとし、腐食が多い場合を普通の場合としてDとした。
実施例6では、下記の方法により、焼成温度依存性を評価した。
異なる焼成温度で予備成型体を大気中で焼成し、それぞれ磁気特性を測定した。それぞれのHcJの差分(ΔHcJ)と焼成温度の差分(ΔT)を除して焼成温度依存性と定義した。焼成温度依存性が小さいほど焼成温度が変化してもHcJは変化しし難くなり、安定したHcJを得られやすくなる。
表9では、焼成温度依存性の評価結果が最も良い場合をAとして、非常に良い場合をBとして、良い場合をCとして、普通の場合をDとした。
フェライト磁石のHcJを調整する方法として、Al2O3を添加する方法が挙げられる。Al2O3を添加する際は、一般的に白色粉末が用いられる。しかしフェライト磁石の原料として白色粉末のCaCO3が用いられるため、CaCO3とAl2O3を取り違えて誤添加し、不良品を作る危険性がある。このため、実施例7において、Al2O3をほとんど添加しない場合(試料番号172〜180)を誤添加の危険性が低いと判断してAと評価し、Al2O3を添加する場合(試料番号181)を誤添加の危険性が高いと判断してDと評価した。
実施例7では、Cr2O3添加によるHcJ調整余力を評価した。
表10では、Cr2O3添加によるHcJ調整余力の評価結果が最も良い場合をAとして、非常に良い場合をBとして、良い場合をCとして、普通の場合をDとした。また、Cr2O3は緑なのでCr2O3を添加することで誤添加の危険性も低くなる。
実施例7では、下記の方法により、コストを評価した。
Al2O3が不純物として含まれる原料の価格を基準にコスト評価を実施した。
表10では、コストの評価結果が最も良い場合をAとして、非常に良い場合をBとして、良い場合をCとして、普通の場合をDとした。
Claims (6)
- 下記式(1)で表される組成を有し、
Ca1−w−xLawAxFezComO19・・・(1)
前記式(1)中、w、x、zおよびmは、下記式(2)、(3)、(4)および(5)を満たし、
0.30≦w≦0.50 (2)
0.08≦x≦0.20 (3)
8.55≦z≦10.00 (4)
0.20≦m≦0.40 (5)
AはSrおよびBaからなる群より選ばれる少なくとも1種の元素であり、
さらにCrをCr2O3換算で0.058質量%〜0.132質量%含むフェライト焼結磁石であって、
前記フェライト焼結磁石中のzとmの合計量y1をY軸に表し、
前記フェライト焼結磁石中のCr2O3の含有量x1質量%をX軸に表したときに、
x1とy1の関係が、前記X軸およびY軸を持つX−Y座標における6つの点a1(0.058,10.25)、b1(0.119,10.25)、c1(0.132,9.30)、d1(0.119,9.30)、e1(0.100,8.75)およびf1(0.058,8.75)で囲まれる範囲内にあることを特徴とするフェライト焼結磁石。 - x1とy1の関係が、前記X軸およびY軸を持つX−Y座標における4つの点a3(0.058,10.25)、b3(0.100,10.25)、c3(0.100,8.95)およびd3(0.058,8.95)で囲まれる範囲内にある請求項1に記載のフェライト焼結磁石。
- w/mが0.98〜2.00である請求項1または2に記載のフェライト焼結磁石。
- さらにSiをSiO2換算で0.55質量%〜1.12質量%含む請求項1〜3のいずれかに記載のフェライト焼結磁石。
- さらにSを0ppmを超え、100ppm未満含む請求項1〜4のいずれかに記載のフェライト焼結磁石。
- AlをAl2O3換算で0.01質量%〜0.97質量%含む請求項1〜5のいずれかに記載のフェライト焼結磁石。
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JP2016006460A JP6583631B2 (ja) | 2016-01-15 | 2016-01-15 | フェライト焼結磁石 |
US15/400,459 US10373746B2 (en) | 2016-01-15 | 2017-01-06 | Ferrite sintered magnet |
KR1020170003509A KR101913024B1 (ko) | 2016-01-15 | 2017-01-10 | 페라이트 소결 자석 |
DE102017200454.1A DE102017200454A1 (de) | 2016-01-15 | 2017-01-12 | Gesinterter Ferritmagnet |
CN201710026066.1A CN107039138B (zh) | 2016-01-15 | 2017-01-13 | 铁氧体烧结磁铁 |
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