JPH09106904A - Ferrite powder for bonded magnet and bonded magnet using thereof - Google Patents
Ferrite powder for bonded magnet and bonded magnet using thereofInfo
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- JPH09106904A JPH09106904A JP7288163A JP28816395A JPH09106904A JP H09106904 A JPH09106904 A JP H09106904A JP 7288163 A JP7288163 A JP 7288163A JP 28816395 A JP28816395 A JP 28816395A JP H09106904 A JPH09106904 A JP H09106904A
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- ferrite
- average particle
- bonded magnet
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は，ＡＶ，ＯＡ機器，
自動車電装部品等に使用される小型モーターや，複写機
のマグネットロール等に使用される高磁力のボンド磁石
を構成するためのフエライト粉末に関する。TECHNICAL FIELD The present invention relates to AV, OA equipment,
TECHNICAL FIELD The present invention relates to a ferrite powder for constituting a small motor used for automobile electrical components and the like, and a high magnetic bond magnet used for a magnet roll of a copying machine.
【０００２】[0002]
【従来の技術】一般に，磁石の磁力を示す最大エネルギ
ー積（ＢＨ）ｍａｘは，残留磁束密度Ｂｒと保磁力ｉＨ
ｃにより決まる。残留磁束密度Ｂｒは磁石の密度ρと磁
粉の飽和磁化σｓ，配向度（Ｂｒ／４πＩｓ）により下
式で表される。 Ｂｒ＝４π×（ρ）×（σｓ）×（配向度）2. Description of the Related Art Generally, the maximum energy product (BH) max, which indicates the magnetic force of a magnet, is determined by the residual magnetic flux density Br and the coercive force iH.
determined by c. The residual magnetic flux density Br is represented by the following equation based on the density ρ of the magnet, the saturation magnetization σs of the magnetic powder, and the orientation degree (Br / 4πIs). Br = 4π × (ρ) × (σs) × (degree of orientation)
【０００３】一方，保磁力ｉＨｃはフエライト系の場
合，結晶異方性と形状異方性および単磁区構造の理論で
説明されている。On the other hand, the coercive force iHc is explained by the theory of crystal anisotropy, shape anisotropy and single domain structure in the case of a ferrite system.
【０００４】ボンド磁石と焼結磁石の大きな違いは密度
ρである。フエライト系焼結磁石の密度５.０ｇ／ｃｍ
3 に対し，ボンド磁石では樹脂やゴム等のバインダーが
入るため当然密度はこれより低くなり，磁力は下がる。
したがって，ボンド磁石の磁力を高くするには，フエラ
イト粉末の含有率を増やすことが必須の課題となる。し
かし，フエライト粉末の含有率を増やすとバインダーと
の混練時に高粘度となり，負荷が増大して混練物の生産
性が低下し，極端な場合には混練不可になる。そして，
混練物の成形時にも流動性が悪いのでやはり生産性が低
下し，極端な場合には成形不可になる。A big difference between the bonded magnet and the sintered magnet is the density ρ. Density of sintered ferrite magnets 5.0g / cm
On the other hand, in the case of bonded magnets, since binders such as resin and rubber enter the bonded magnets, the density naturally becomes lower than this and the magnetic force decreases.
Therefore, in order to increase the magnetic force of the bond magnet, increasing the content rate of the ferrite powder is an essential issue. However, if the content of the ferrite powder is increased, the viscosity becomes high during kneading with the binder, the load increases, and the productivity of the kneaded product decreases, and in extreme cases, the kneading becomes impossible. And
Since the fluidity of the kneaded product is poor even when it is molded, the productivity is reduced, and in extreme cases, molding becomes impossible.
【０００５】このボンド磁石特有の課題を解決するため
に，バインダーの選定やフエライト粉末の表面処理等の
面での改良が行われているが，基本的にはフエライト粉
末自身の高充填性を確保することが最も重要である。フ
エライト粉末の充填性は一般的には粒度分布と圧縮密度
との関連性が高い。In order to solve the problems peculiar to the bonded magnet, the selection of the binder and the surface treatment of the ferrite powder have been improved, but basically, the high filling property of the ferrite powder itself is ensured. To do is most important. The filling property of the ferrite powder is generally highly related to the particle size distribution and the compressed density.
【０００６】従来，このようなフエライト粉末の製造方
法として例えば特公昭５５−２６６０５号公報および特
公昭６３−３４６１０号公報に記載された方法が知られ
ている。前者は高温で焼成して粗大結晶粒子を成長さ
せ，これを粉砕して粗大粒子の間隙を埋めるような微粒
子を作る方法であり，後者は平均粒径０.５〜１.５μｍ
のフエライト微粉末と平均粒径３０〜２５０μｍのフエ
ライト粗粉とを配合する方法である。Conventionally, as a method for producing such a ferrite powder, for example, the methods described in JP-B-55-26605 and JP-B-63-34610 are known. The former is a method of firing at high temperature to grow coarse crystal grains and crushing them to make fine particles that fill the gaps between the coarse grains, and the latter is an average grain size of 0.5 to 1.5 μm.
Of fine ferrite powder and coarse ferrite powder having an average particle diameter of 30 to 250 μm.
【０００７】これらの方法でも圧縮密度が高く，高充填
性のフエライト粉末は得られるが，充填性以外にボンド
磁石として高磁力化に必要な特性要因についての考慮が
不充分で，得られるボンド磁石の最大エネルギー積（Ｂ
Ｈ）ｍａｘは最高レベルでも２.２〜２.３ＭＧＯｅが限
度であった。With these methods, ferrite powder having a high compression density and a high packing property can be obtained. However, in addition to the packing property, the bond magnet obtained can not be sufficiently considered in terms of the characteristic factors necessary for increasing the magnetic force of the bond magnet. Maximum energy product of (B
H) max was limited to 2.2 to 2.3 MGOe even at the highest level.
【０００８】例えば単に圧縮密度だけを追求したフエラ
イト粉末では，バインダーとの混練負荷を下げたり，そ
の混練物の流動性を上げて成形性を改善するには十分で
はない。粉体の混練性や流動性は確かに圧縮密度によっ
ても影響も受けるが，その他の要因として粒子形状，粒
子の表面状態の影響も無視できないからである。また粒
子形状や粒子の表面状態は配向度および保磁力との関連
性も強い。For example, a ferrite powder that pursues only the compression density is not sufficient to reduce the kneading load with the binder or increase the fluidity of the kneaded product to improve the moldability. This is because the kneadability and fluidity of the powder are certainly affected by the compression density, but other factors such as the particle shape and the surface condition of the particles cannot be ignored. Further, the particle shape and the surface condition of the particles are closely related to the degree of orientation and the coercive force.
【０００９】粒子形状の点からフエライト粒子を見る
と，配向に適した粒子形状はＣ軸方向の異方性が高い六
角板状であるが，射出成形等の磁場配向タイプでは板状
比（ａ軸方向の粒径／ｃ軸方向の粒径）が小さいほど，
粒子が動き易く高流動性が得られる。また，当然粒子間
焼結が少ないほど配向しやすい。Looking at the ferrite particles in terms of particle shape, the particle shape suitable for orientation is a hexagonal plate shape with high anisotropy in the C-axis direction, but in the magnetic field orientation type such as injection molding, the plate shape ratio (a The smaller the axial grain size / c-axis grain size, the more
The particles move easily and high fluidity is obtained. Naturally, the less the interparticle sintering, the easier the orientation.
【００１０】粒子の表面形態については不明な点が多い
が，バインダーとの親和性から，混練時，成形時におけ
る粘度との関連がありそうである。粘度が低いほど高流
動性となり配向度が上がり，また機械的ストレスが弱い
ので保持力の低下も少ないであろう。Although there are many unclear points regarding the surface morphology of the particles, it is likely that the surface morphology of the particles is related to the viscosity at the time of kneading and molding due to the affinity with the binder. The lower the viscosity, the higher the fluidity, the higher the degree of orientation, and the weaker the mechanical stress, the less the retention will decrease.
【００１１】保磁力ｉＨｃについては，結晶異方性と形
状異方性，単磁区構造等によって説明されている。例え
ばストロンチウムフエライトは，バリウムフエライトよ
りも結晶異方性が大きいので高ｉＨｃが得られる。また
板状比は小さいほど形状異方性による減磁が少ないので
高ｉＨｃになる。粉砕して平均粒子径が小さくなると単
磁区構造に近づくので（ただし，同時に歪みも生じるの
でこの歪みをアニールで除去すると）高ｉＨｃが得られ
る。なお，アニールしたものは混練および成形時に機械
的ストレスを受けてｉＨｃが下がるが，平均粒子径が小
さいとこのストレスを受けにくい。The coercive force iHc is explained by crystal anisotropy, shape anisotropy, single domain structure and the like. For example, strontium ferrite has a larger crystal anisotropy than barium ferrite, so that high iHc can be obtained. Further, the smaller the plate ratio, the less the demagnetization due to the shape anisotropy, and the higher the iHc becomes. When the average particle size is reduced by pulverization, the structure approaches a single domain structure (however, since strain is also generated at the same time, this strain is removed by annealing), a high iHc can be obtained. The annealed material receives mechanical stress during kneading and molding to lower iHc, but if the average particle size is small, this stress is less likely to be received.
【００１２】残留磁束密度Ｂｒについては飽和磁化σｓ
が決め手となる。マグネトプランバイト型（以下Ｍ型と
略称することがある）フエライトにおける飽和磁化σｓ
の理論値としては，ストロンチウムフエライトが７２ｅ
ｍｕ／ｇ，バリウムフエライトが７１ｅｍｕ／ｇである
のに対し，一般市販品は７０ｅｍｕ／ｇ程度とかなり理
論値に近いところまで向上しているので，これ以上のσ
ｓの大幅な向上は難しい。現在，飽和磁化を上げる手段
とし，Ｍ型よりも高い理論値７８ｅｍｕ／ｇを有するＷ
型フエライトも一部検討されているが，製法が複雑でコ
ストも高いため実用化には達してない。Regarding the residual magnetic flux density Br, the saturation magnetization σs
Is the decisive factor. Saturation magnetization σs in magnetoplumbite type (hereinafter sometimes abbreviated as M type) ferrite
The theoretical value of Strontium ferrite is 72e
Mu / g and barium ferrite are 71 emu / g, whereas general commercial products have improved to about 70 emu / g, which is quite close to the theoretical value.
It is difficult to significantly improve s. At present, W having a theoretical value of 78 emu / g higher than that of the M type is used as a means for increasing the saturation magnetization.
Some types of ferrite have been studied, but they have not been put to practical use because the manufacturing method is complicated and the cost is high.
【００１３】以上のように，フエライト粉末の組成，粒
度，粒度分布，表面性は，ボンド磁石の充填性，混練
性，成形性，配向性，保磁力，飽和磁化と複雑に絡んで
おり，これらをバランス良く制御することによって初め
てボンド磁石の高（ＢＨ）ｍａｘ化が達成される。これ
らの制御には，組成（原料，モル比，添加物），焼成，
粉砕，アニール等の単位操作が一般的であるが，これら
の組み合わせを最適化することが重要となる。As described above, the composition, particle size, particle size distribution and surface property of the ferrite powder are intricately involved with the filling property, kneading property, moldability, orientation property, coercive force and saturation magnetization of the bonded magnet. A high (BH) max of the bonded magnet can be achieved only by controlling B in a well-balanced manner. These controls include composition (raw materials, molar ratio, additives), firing,
Unit operations such as crushing and annealing are common, but it is important to optimize these combinations.
【００１４】しかし，前記の特公昭５５−２６６０５号
公報および特公昭６３−３４６１０号公報では，特に充
填性だけを重視し，その他の複数要因については十分に
考慮されていない。そのため，特性を制御する単位操作
も単純すぎるため，複雑な特性要因を十分に制御するの
は困難であり，フエライト系ボンド磁石の（ＢＨ）ｍａ
ｘは２.２〜２.３ＭＧＯｅが最高レベルであった。事
実，現状の市場においても，この最高レベルを超えるフ
エライト系ボンド磁石は出現していない。However, in Japanese Patent Publication No. 55-26605 and Japanese Patent Publication No. 63-34610, only the filling property is emphasized and other factors are not sufficiently taken into consideration. Therefore, it is difficult to sufficiently control the complicated characteristic factors because the unit operation for controlling the characteristic is too simple, and the (BH) ma of the ferrite type bonded magnet is difficult to control.
The highest level of x was 2.2 to 2.3 MGOe. In fact, even in the current market, no ferrite-type bonded magnets exceeding this highest level have appeared.
【００１５】このため，（ＢＨ）ｍａｘ＝２.５〜４.０
ＭＧＯｅが要求される分野ではフエライト系焼結磁石が
使用されている。だが，焼結磁石は欠け割れが発生した
り，研磨が必要なため生産性に劣ることと，複雑な形状
への加工が困難であるという固有の問題がある。最近，
希土類磁石を用いたボンド磁石がこの分野で一部使用さ
れているが，希土類磁石はフエライトの２０倍のコスト
高であり，また錆びやすいという問題がある。Therefore, (BH) max = 2.5-4.0
Ferrite-based sintered magnets are used in fields where MGOe is required. However, sintered magnets have the inherent problems of chipping and cracking, poor productivity due to the need for polishing, and difficulty in processing into complex shapes. Recently,
Bonded magnets using rare earth magnets are partially used in this field, but rare earth magnets are 20 times more expensive than ferrite and have the problem of being easily rusted.
【００１６】このような背景から，加工性が良好で安価
なフエライト系Ｍ型ボンド磁石において（ＢＨ）ｍａｘ
≧２.５ＭＧＯｅを達成することが，ＡＶ，ＯＡ機器，
自動車の電装部品等の小型モーターや複写機のマグネッ
トロールの用途分野で強く要望されている。From such a background, in a ferrite type M-type bonded magnet which has good workability and is inexpensive, (BH) max
Achieving ≧ 2.5 MGOe means AV, OA equipment,
There is a strong demand in the application fields of small motors such as electric components of automobiles and magnet rolls of copying machines.
【００１７】[0017]
【発明が解決しようとする課題】したがって 本発明
は，上記したフエライト系ボンド磁石の問題点を解決
し，前記の要望に応えるべく，従来技術の水準を越える
（ＢＨ）ｍａｘ≧２.５ＭＧＯｅのフエライト系ボンド
磁石の開発を課題としたものである。Therefore, the present invention solves the above-mentioned problems of the ferrite-based bonded magnets, and in order to meet the above-mentioned demand, the ferrite having a (BH) max ≧ 2.5 MGOe exceeding the level of the prior art. The development of bonded magnets is an issue.
【００１８】[0018]
【課題を解決するための手段】前記の課題は，平均粒子
径が０.３０〜０.５０μｍの微粉１５〜４０重量％と，
平均粒子径が１.００〜２.５０μｍの粗粉残部とを混合
して得た平均粒子径が０.９〜１.５μｍであって，粉体
ＰＨが７〜１０の範囲，下記のＭＦＲ測定法に従ってフ
エライト量９３重量％で測定したメルトフローレートが
７ｇ／１０ｍｉｎ以上であるマグネトプランバイト型フ
エライト粉末によって実質上解決できることがわかっ
た。[Means for Solving the Problems] The above problems are as follows: 15 to 40% by weight of fine powder having an average particle size of 0.30 to 0.50 μm,
The average particle size obtained by mixing with the rest of the coarse powder having an average particle size of 1.00 to 2.50 μm is 0.9 to 1.5 μm, the powder PH is in the range of 7 to 10, and the MFR is as follows. It was found that this can be practically solved by a magnetoplumbite type ferrite powder having a melt flow rate of 7 g / 10 min or more measured with a ferrite amount of 93% by weight according to the measuring method.
【００１９】すなわち本発明によれば，マグネトプラン
バイト型フエライトの粉末であって，平均粒子径が０.
９〜１.５μｍ，ＪＩＳ Ｋ−５１０１で測定した粉体
ＰＨが７〜１０，更には下記のＭＦＲ測定法に従ってフ
エライト量９３重量％で測定したメルトフローレートが
７ｇ／１０ｍｉｎ以上である，１ton/ｃｍ2 の圧力で圧
縮したときの圧縮密度が３.４０ｇ／ｃｍ3 以上のボン
ド磁石用フエライト粉末を提供する。That is, according to the present invention, the powder is a magnetoplumbite-type ferrite and has an average particle size of 0.1.
9 to 1.5 μm, the powder PH measured by JIS K-5101 is 7 to 10, and the melt flow rate measured at a ferrite amount of 93% by weight according to the following MFR measuring method is 7 g / 10 min or more, 1 ton / Provided is a ferrite powder for a bonded magnet, which has a compression density of 3.40 g / cm 3 or more when compressed at a pressure of cm 2 .
【００２０】このフエライト粉末の粒度分布の幾何標準
偏差σｇが１.８〜２.５であるのが一層好ましく，また
ＢＥＴ法で測定した比表面積が１.５〜４.０ｍ2/ｇであ
る。It is more preferable that the geometric standard deviation σg of the particle size distribution of this ferrite powder is 1.8 to 2.5, and the specific surface area measured by the BET method is 1.5 to 4.0 m 2 / g. .
【００２１】このフエライト粉末は，平均粒子径が０.
３０〜０.５０μｍのマグネトプランバイト型フエライ
トの微粉と，平均粒子径が１.００〜２.５０μｍのマグ
ネトプランバイト型フエライトの粗粉を準備する工程，
前記の微粉１５〜４０重量％と前記の粗粉残部とを混合
する工程，およびこの混合工程の前または後においてこ
れらの粉体を８００〜１１００℃でアニールする工程，
更には，アニール工程後の粉体のＰＨを７〜１０に調整
する工程からなる製造方法によって製造することができ
る。This ferrite powder has an average particle size of 0.1.
A step of preparing fine powder of magnetoplumbite type ferrite of 30 to 0.50 μm and coarse powder of magnetoplumbite type ferrite having an average particle size of 1.00 to 2.50 μm,
Mixing 15 to 40% by weight of the fine powder with the remainder of the coarse powder, and annealing the powder at 800 to 1100 ° C. before or after the mixing step,
Further, it can be manufactured by a manufacturing method including a step of adjusting the pH of the powder after the annealing step to 7 to 10.
【００２２】そして，本発明によれば，平均粒子径が
０.９〜１.５μｍのマグネトプランバイト型フエライト
の粉末９３重量％以上を樹脂系バインダーを用いて成形
してなる（ＢＨ）ｍａｘが２.５ＭＧＯｅ以上のフエラ
イト系ボンド磁石を提供する。該磁石の成形密度は３.
９０ｇ／ｃｍ3 以上である。According to the present invention, 93% by weight or more of magnetoplumbite-type ferrite powder having an average particle diameter of 0.9 to 1.5 μm is molded by using a resinous binder to obtain (BH) max. Provide a ferrite-based bonded magnet of 2.5 MGOe or more. The molding density of the magnet is 3.
90 g / cm 3 or more.
【００２３】[0023]
【発明の実施の形態】フエライト系ボンド磁石において
高磁力化を達成するには，フエライト粉末のボンド磁石
中へ高充填することと配向度を上げることが必須条件で
ある。そして，高充填性のフエライト粉末を得るには粒
度分布を広くし，圧縮密度を高くする方法が効果的であ
る。BEST MODE FOR CARRYING OUT THE INVENTION In order to achieve a high magnetic force in a ferrite-based bonded magnet, it is essential to highly fill the bonded magnet with a ferrite powder and to increase the degree of orientation. A method of broadening the particle size distribution and increasing the compression density is effective for obtaining highly-filled ferrite powder.
【００２４】Ｆｕｒｎａｓ等によって二成分系のランダ
ム充填モデルが提案されている。最密充填された大粒子
間隙をちょうど満たすように小粒子を最密充填する場
合，大粒子の重量割合が７０％付近で最大充填率を与え
る。ただし，粒径比は０.２以下がであることが必要で
ある。A two-component random packing model has been proposed by Furnas et al. When the close packing of the small particles is performed so as to just fill the gap between the close packed large particles, the maximum packing ratio is given when the weight ratio of the large particles is around 70%. However, the particle size ratio must be 0.2 or less.
【００２５】本発明者らは，マグネトプランバイト型フ
エライト粉末について，充填性と配向度の高い製造条件
を知るべく広汎な試験研究を行った。その結果，平均粒
子径が０.３０〜０.５０μｍのマグネトプランバイト型
フエライトの微粉１５〜４０重量％と，平均粒子径が
１.００〜２.５０μｍのマグネトプランバイト型フエラ
イトの粗粉残部を混合して得た平均粒径０.９〜１.５μ
ｍの粉末が高充填性と高配向度をもたらすことがわかっ
た。The present inventors have conducted extensive test studies on magnetoplumbite type ferrite powder in order to know the manufacturing conditions with high filling property and high degree of orientation. As a result, 15-40% by weight of fine particles of magnetoplumbite-type ferrite having an average particle diameter of 0.30-0.50 μm and the remainder of the coarse particles of magnetoplumbite-type ferrite having an average particle diameter of 1.00-2.50 μm. Average particle size obtained by mixing
It has been found that the m powder gives a high packing property and a high degree of orientation.
【００２６】この場合，粒度分布の幾何標準偏差σｇが
１.８〜２.５の範囲となるものが特に充填性と配向度が
高い。この幾何標準偏差σｇは公知のレーザー回折式粒
度分布測定装置によって測定できる。本発明例では日本
電子株式会社製の商品名“ＨＥＬＯＳ ＆ ＲＯＤＯ
Ｓ”のレーザー回折式粒度分布測定装置を用いてσｇを
測定した。In this case, when the geometric standard deviation σg of the particle size distribution is in the range of 1.8 to 2.5, the filling property and the orientation degree are particularly high. This geometric standard deviation σg can be measured by a known laser diffraction type particle size distribution measuring device. In the example of the present invention, the product name “HELOS & RODO” manufactured by JEOL Ltd.
Σg was measured using an S ″ laser diffraction particle size distribution analyzer.
【００２７】この充填性と配向度の高いマグネトプラン
バイト型フエライト粉末を得るには，先ず微粉原料とし
て，平均粒子径０.８〜１.５μｍの例えばストロンチウ
ムフエライトまたはバリウムフエライトを使用し，これ
を粉砕するか或いは粉砕後に分級して平均粒子径０.３
０〜０.５０μｍの範囲に入る微粉を準備する。この粉
砕時に平均粒子径を０.３μｍ未満にまで粉砕すること
は必要ではない。このような超微粉にまで粉砕すると，
粉砕時間が長くなり生産性の観点からマイナスであるば
かりでなく，ボンド磁石化後の磁気特性も低下する。他
方，０.５μｍを越える場合には，粗粉との混合したと
きに圧縮密度が低くなりボンド磁石への高充填に不適当
となる。In order to obtain the magnetoplumbite type ferrite powder having a high packing property and a high degree of orientation, first, for example, strontium ferrite or barium ferrite having an average particle diameter of 0.8 to 1.5 μm is used as a fine powder raw material. Average particle size of 0.3 after crushing or after crushing
Prepare a fine powder that falls within the range of 0 to 0.50 μm. It is not necessary to grind the average particle diameter to less than 0.3 μm during this grinding. When crushed to such an ultrafine powder,
Not only is the crushing time longer and the productivity is negative, but the magnetic properties after forming a bonded magnet also deteriorate. On the other hand, when it exceeds 0.5 μm, the compression density becomes low when mixed with coarse powder, which is not suitable for high filling of the bonded magnet.
【００２８】一方，粗粉原料としては平均粒子径３.０
〜４.０μｍの例えばストロンチウムフエライトまたは
バリウムフエライトを使用し，これを粉砕するか或いは
粉砕後に分級して平均粒子径１.００〜２.５０μｍの範
囲に入る粗粉を得る。１.００μｍ未満では微粉との混
合粉は圧縮密度が低くなり，ボンド磁石への高充填に不
適当である。他方，２.５０μｍを越える場合はボンド
磁石化後の配向度と保磁力が著しく低下するようにな
る。On the other hand, as the coarse powder raw material, the average particle diameter is 3.0.
.About.4.0 .mu.m, for example, strontium ferrite or barium ferrite, is crushed or classified after crushing to obtain a coarse powder having an average particle size in the range of 1.00 to 2.50 .mu.m. If it is less than 1.00 μm, the mixed powder with the fine powder has a low compression density and is unsuitable for high filling of the bonded magnet. On the other hand, when it exceeds 2.50 μm, the orientation degree and the coercive force after forming the bond magnet are remarkably lowered.
【００２９】このようにして準備した平均粒子径０.３
０〜０.５０μｍの微粉と，平均粒子径１.００〜２.５
０μｍの粗粉を用いて，微粉１５〜４０重量％で残部が
粗粉となる混合比率を有するフエライト粉末を作る。微
粉が１５重量％未満では混合粉の圧縮密度が低く高充填
に不適当となり，またボンド磁石に成形後の保磁力も低
くなる。他方微粉が４０重量％を越えると，ボンド磁石
製造の際，バインダーとの混練および成形時の粘度が高
くなりすぎてボンド磁石化が困難になり，また成形でき
ても磁粉の配向度が低くなって残留磁束密度Ｂｒが下が
る。The average particle size thus prepared is 0.3
Fine powder of 0-0.50 μm and average particle size of 1.0-2.5
Using 0 μm of coarse powder, ferrite powder having a mixing ratio of 15 to 40% by weight of fine powder and the balance being coarse powder is prepared. If the fine powder is less than 15% by weight, the compression density of the mixed powder is low and it is not suitable for high filling, and the coercive force after molding into a bonded magnet is also low. On the other hand, if the amount of fine powder exceeds 40% by weight, the viscosity during kneading with a binder and during molding becomes too high during bond magnet production, making it difficult to form a bond magnet, and even if molding is possible, the degree of orientation of magnetic powder becomes low. As a result, the residual magnetic flux density Br decreases.
【００３０】以上のような混合比で微粉と粗粉を混合後
にアニール処理を施すか，或いは微粉と粗粉を別々にア
ニール処理してから混合する。このアニール処理によっ
て，微粉・粗粉製造時の粉砕の際に結晶粒子中に発生し
た歪みを除去することができる。アニール温度は８００
〜１１００℃が好ましい。８００℃未満ではアニールの
効果が十分に達成されず，保磁力と飽和磁化が低くな
る。また１１００℃を越えると焼結が進んで，圧縮密度
と配向性が低下する。The fine powder and the coarse powder are mixed at the above mixing ratio and then annealed, or the fine powder and the coarse powder are separately annealed and then mixed. By this annealing treatment, it is possible to remove the strain generated in the crystal grains during the pulverization during the production of fine and coarse powders. Annealing temperature is 800
~ 1100 ° C is preferred. If the temperature is lower than 800 ° C, the effect of annealing is not sufficiently achieved, and the coercive force and the saturation magnetization are lowered. On the other hand, if the temperature exceeds 1100 ° C., the sintering proceeds, and the compression density and orientation decrease.
【００３１】そして，最終的に粉体のＰＨを７〜１０に
調整する。このＰＨ調整には水洗や酸性物質による処理
等が採用できる。酸性物質としては，塩酸，硫酸，硝酸
等の無機酸が好ましい。カップリング剤等の有機物の表
面処理剤はフエライト粉末の表面に付着残留することに
よってその効果が発揮されるが，水洗および酸性物質に
よるＰＨ調整後には，かようなカップリング剤の使用量
を減らすことができるため，ボンド磁石における磁粉の
含有率低下を抑えられる。本発明粉の場合，アニール後
の粉体ＰＨは１１以上となり，この状態ではバインダー
との親和性に問題があり，高充填での混練および成形が
困難になる。粉体ＰＨを７〜１０に調整するとバインダ
ーとの親和性が増し粘度が下がるため，混練時の負荷を
下げ，成形時の流動性を上げることができる。なおＰＨ
値はＪＩＳ Ｋ−５１０１に規定の測定方法による。Finally, the pH of the powder is adjusted to 7-10. For this pH adjustment, washing with water or treatment with an acidic substance can be adopted. As the acidic substance, inorganic acids such as hydrochloric acid, sulfuric acid and nitric acid are preferable. The effect of organic surface treatment agents such as coupling agents is exhibited by remaining on the surface of the ferrite powder, but after washing and adjusting the pH with acidic substances, the amount of such coupling agents used is reduced. Therefore, it is possible to suppress a decrease in the content ratio of the magnetic powder in the bonded magnet. In the case of the powder of the present invention, the powder PH after annealing becomes 11 or more, and in this state, there is a problem with the affinity with the binder, and it becomes difficult to knead and mold with high filling. When the powder PH is adjusted to 7 to 10, the affinity with the binder increases and the viscosity decreases, so that the load during kneading can be reduced and the fluidity during molding can be increased. PH
The value is based on the measuring method specified in JIS K-5101.
【００３２】このようにして，平均粒子径が０.９〜１.
５μｍ，比表面積が１.５〜４.０ｍ2／ｇ，粒度分布の
幾何標準偏差が１.８〜２.５，圧縮密度が３.４０〜３.
６０ｇ／ｃｍ3 ，粉体ＰＨが７〜１０のマグネトプラン
バイト型フエライト粉末が得られる。ここで，平均粒子
径は空気透過法による比表面積測定装置で測定できる。
かような測定装置として例えば島津製作所製の商品名Ｓ
Ｓ−１００型の装置がある。また，比表面積はＢＥＴ法
によって測定したものを意味する。この比表面積測定装
置としては，例えばユアサアイオニクス株式会社製のモ
ノソーブが使用できる。In this way, the average particle size is 0.9-1.
5 μm, specific surface area 1.5-4.0 m 2 / g, geometric standard deviation of particle size distribution 1.8-2.5, compression density 3.40-3.
A magnetoplumbite-type ferrite powder having a powder PH of 60 g / cm 3 and 7 to 10 is obtained. Here, the average particle diameter can be measured by a specific surface area measuring device by the air permeation method.
As such a measuring device, for example, product name S manufactured by Shimadzu Corporation
There is an S-100 type device. Further, the specific surface area means that measured by the BET method. As this specific surface area measuring device, for example, a monosorb manufactured by Yuasa Ionics Co., Ltd. can be used.
【００３３】本発明のフエライト粉末は，メルトフロー
レート（ＭＦＲ）が従来品のものにはない高い値を示す
という特質がある。その具体例は，後記実施例にも示す
が，従来品の水準を超えるフエライト量９３重量％で測
定したメルトフローレートが７ｇ／１０ｍｉｎ以上の高
流動を示す。ここで，ＭＦＲの値は，ＪＩＳ Ｋ−７２
１０に規定の熱可塑性プラスチックの流れ試験方法に準
じてフエライト粉末と樹脂のコンパウンドの流動性を測
定したものを意味する。その具体的な試験例を以下に挙
げる。The ferrite powder of the present invention has the characteristic that it has a high melt flow rate (MFR), which is not found in conventional products. Specific examples thereof are shown in Examples below, but the melt flow rate measured at a ferrite amount of 93% by weight, which exceeds the level of conventional products, shows a high flow of 7 g / 10 min or more. Here, the value of MFR is JIS K-72.
It means that the fluidity of the compound of the ferrite powder and the resin was measured according to the flow test method for thermoplastics specified in 10. The specific test example is given below.
【００３４】メルトフローレート (ＭＦＲ) の測定 ＪＩＳ Ｋ−７２１０に規定の熱可塑性プラスチックの
流れ試験方法に準じてフエライト粉末と樹脂のコンパウ
ンドの流動性を評価するにあたり，フエライト粉末試料
を，次の条件で１次表面処理，乾燥，樹脂調合，２次表
面処理，乾燥，混練の工程を順次経たうえ，これをＭＦ
Ｒ測定装置でメルトフローレートを測定する。Measurement of Melt Flow Rate (MFR) In order to evaluate the fluidity of a compound of a ferrite powder and a resin in accordance with the flow test method for thermoplastics specified in JIS K-7210, a ferrite powder sample was subjected to the following conditions. Then, the primary surface treatment, drying, resin blending, secondary surface treatment, drying, and kneading are sequentially performed, and then MF is applied.
The melt flow rate is measured with an R measuring device.
【００３５】 (1) フエライト粉末：２５００ｇ採取 (2) １次表面処理：Ｓ−３２０ ２０ｇ 水 １０ｇ メタノール ２３.８ｇ 処理装置；ハイスピードミキサー (3) 乾燥 ：１００℃×９０分 (4) 樹脂混合 ：前記の乾燥粉 ２４５０ｇ １２−ナイロン １５７.８ｇ（フエライト９３％の場合） 混合装置；ハイスピードミキサー（実施例記載のもの） (5) ２次表面処理：該樹脂と粉末の混合粉 全量 ２６０７.８ｇ 処理剤：オレイン酸 ９.７ｇ メタノール ２４.８ｇ 処理装置；ハイスピードミキサー (6) 乾燥 ：１００℃×３０分 (7) 混練 ：温度 ２２０℃ 混練装置 ＫＣＫ７０−２２ＶＥＸ（６） (8) ＭＦＲ測定 ：温度 ２７０℃ 荷重 １０Ｋｇ 試料挿入量 １５ｇ 測定装置 メルトインデクサー(1) Ferrite powder: 2500 g (2) Primary surface treatment: S-320 20 g Water 10 g Methanol 23.8 g Treatment device; High-speed mixer (3) Drying: 100 ° C. × 90 minutes (4) Resin mixing : Dry powder 2450 g 12-nylon 157.8 g (in the case of 93% ferrite) Mixing device: High speed mixer (as described in the examples) (5) Secondary surface treatment: Total amount of mixed powder of the resin and powder 2607. 8g Treatment agent: Oleic acid 9.7g Methanol 24.8g Treatment device; High speed mixer (6) Drying: 100 ° C x 30 minutes (7) Kneading: Temperature 220 ° C Kneading device KCK70-22VEX (6) (8) MFR measurement : Temperature 270 ° C. Load 10 Kg Sample insertion amount 15 g Measuring device Melt indexer
【００３６】この測定に使用する樹脂と装置の具体例は
後記の実施例に記載した。本発明のフエライト粉はフエ
ライト９３重量％で残部が樹脂のコンパウンドでも流動
性を示し，ＭＦＲ値が７ｇ／１０ｍｉｎ以上となるのに
対し，従来品はフエライト９３重量％では全く流動性を
示さない。Specific examples of the resin and the apparatus used for this measurement are described in the examples below. The ferrite powder of the present invention is 93% by weight of ferrite and shows fluidity even when the balance is resin compound, and the MFR value is 7 g / 10 min or more, whereas the conventional product does not show fluidity at 93% by weight of ferrite.
【００３７】この流動特性を有した本発明のフエライト
粉は，これをフエライト９３重量％以上となるように樹
脂系バインダーを用いて成形することによって（ＢＨ）
ｍａｘが２.５ＭＧＯｅ以上のフエライト系ボンド磁石
が得られる。この場合の成形密度は３.９０ｇ／ｃｍ3
以上である。The ferrite powder of the present invention having this fluidity characteristic is molded by using a resin binder so that the ferrite content is 93% by weight or more (BH).
A ferrite bonded magnet having a max of 2.5 MGOe or more can be obtained. The molding density in this case is 3.90 g / cm 3.
That is all.
【００３８】以下に本発明の実施例を挙げて，その効果
を具体的に示す。The effects of the present invention will be specifically described below with reference to examples of the present invention.
【００３９】[0039]
〔実施例１〕 (1)微粉の製造 酸化鉄と炭酸ストロンチウムをモル比で５.２になるよ
うに秤量して混合し，これを水で造粒し，乾燥後，電気
炉中１０００℃で２時間焼成した。この焼成品をハンマ
ーミル（商品名サンプルミル）で粉砕し，さらに湿式粉
砕機（商品名ウエットミル）で湿式粉砕し，平均粒子径
が０.４３μｍのストロンチウムフエライト微粉を得
た。[Example 1] (1) Manufacture of fine powder Iron oxide and strontium carbonate were weighed and mixed in a molar ratio of 5.2, granulated with water, dried, and then in an electric furnace at 1000 ° C. It was baked for 2 hours. This fired product was crushed with a hammer mill (trade name sample mill) and further wet crushed with a wet crusher (trade name wet mill) to obtain strontium ferrite fine powder having an average particle diameter of 0.43 μm.
【００４０】(2)粗粉の製造 酸化鉄と炭酸ストロンチウムをモル比で５.７になるよ
うに秤量して混合し，これを水で造粒し，乾燥後，電気
炉中１２００℃で２時間焼成した。この焼成品をサンプ
ルミルで粉砕し，さらに該ウエットミルで湿式粉砕し
て，平均粒子径が１.６１μｍのストロンチウムフエラ
イト粗粉を得た。(2) Manufacture of coarse powder Iron oxide and strontium carbonate were weighed and mixed so that the molar ratio was 5.7, and this was granulated with water, dried, and then dried at 1200 ° C. in an electric furnace at 2 ° C. Burned for hours. The calcined product was pulverized with a sample mill and further wet pulverized with the wet mill to obtain strontium ferrite coarse powder having an average particle diameter of 1.61 μm.
【００４１】(3)混合粉（フエライト粉末）の製造 (1)の微粉３０重量％と(2)の粗粉残部（７０重量％）を
秤量し，これを良く混合し，その混合粉を電気炉中９５
０℃で１時間焼成（アニール）した。得られた焼成品を
２０％の濃度になるように水中でリパルプ水洗した。こ
れを濾過，乾燥し，解砕して最終粉末として，次のスト
ロンチウムフエライト粉末を得た。 平均粒子径：１.２７μｍ， 比表面積 ：２.３５ｍ2／ｇ， 粒度分布の幾何標準偏差：２.０４， 圧縮密度 ：３.４４ｇ／ｃｍ3 ， 粉体ＰＨ ：９.５(3) Production of mixed powder (ferrite powder) 30% by weight of the fine powder of (1) and the rest (70% by weight) of the coarse powder of (2) were weighed and mixed well, and the mixed powder was electrically mixed. 95 in the furnace
It was baked (annealed) at 0 ° C. for 1 hour. The obtained fired product was washed with repulp in water to a concentration of 20%. This was filtered, dried, and crushed to obtain the following strontium ferrite powder as the final powder. Average particle size: 1.27 μm, specific surface area: 2.35 m 2 / g, geometric standard deviation of particle size distribution: 2.04, compression density: 3.44 g / cm 3 , powder PH: 9.5
【００４２】(4)ボンド磁石の製造 前記の(3)で得られたフエライト粉末９３部をミキサー
で攪拌しながらシラン系カップリング剤０.６部で表面
処理し，粉末状の１２−ナイロン６.０４部を混合し,
さらにオレイン酸０.３６部を添加する。次いで, 混練
機で２２０℃で混練ペレット化した後，１２ＫＯｅの磁
界中で射出成形し，直径１５ｍｍ×高さ８ｍｍの円柱状
異方性ボンド磁石を得た。この磁石をＢＨトレーサーで
測定したところ，最大エネルギー積（ＢＨ）ｍａｘ＝
２.６３ＭＧＯｅの高磁力品であった。(4) Production of Bonded Magnet 93 parts of the ferrite powder obtained in (3) above was surface-treated with 0.6 part of a silane coupling agent while stirring with a mixer, and powdered 12-nylon 6 Mix .04 parts,
Further, 0.36 part of oleic acid is added. Then, after kneading and pelletizing at 220 ° C. with a kneader, injection molding was performed in a magnetic field of 12 KOe to obtain a cylindrical anisotropic bonded magnet having a diameter of 15 mm and a height of 8 mm. When this magnet was measured with a BH tracer, the maximum energy product (BH) max =
The product had a high magnetic force of 2.63 MGOe.
【００４３】(5)メルトフローレート (ＭＦＲ) の測定 ＪＩＳ Ｋ−７２１０に規定の熱可塑性プラスチックの
流れ試験方法に準じてフエライト粉末と樹脂のコンパウ
ンドの流動性を評価する。フエライト粉末試料を本文に
記載したＭＦＲの測定順序(1) 〜(7) に従って処理し，
前記(8) のＭＦＲ値を測定する。ここで，使用した処理
装置および樹脂は次のとおりである。(5) Measurement of melt flow rate (MFR) The fluidity of the compound of the ferrite powder and the resin is evaluated according to the flow test method for thermoplastics defined in JIS K-7210. The ferrite powder sample was processed according to the MFR measurement sequence (1) to (7) described in the text,
The MFR value in (8) above is measured. The processing equipment and resin used here are as follows.
【００４４】１次表面処理，樹脂混合および２次表面処
理に使用したハイスピードミキサーとして，深江工業株
式会社製の商品名ＦＳ−ＧＣ−５ＪＤを使用した。この
ミキサーは缶体全容量が１１リットルのインペラー型高
速攪拌装置であり，いずれの処理も周速：８ｍ／ｓｅ
ｃ，処理時間：５分である。As the high speed mixer used for the primary surface treatment, the resin mixing and the secondary surface treatment, Fukae Industry Co., Ltd. trade name FS-GC-5JD was used. This mixer is an impeller-type high-speed agitator with a total can volume of 11 liters.
c, processing time: 5 minutes.
【００４５】混練に使用した混練装置はＫＣＫ株式会社
製の連続混練押出式の型式：ＫＣＫ７０−２２ＶＥＸ
（６）を用いた。The kneading device used for kneading is a continuous kneading extrusion type model: KCK70-22VEX manufactured by KCK Corporation.
(6) was used.
【００４６】ＭＦＲの測定に用いたメルトインデクサー
は，東洋精機株式会社製の型式：Ｃ−５０５９Ｄ２を用
いた。この装置の構造はＪＩＳ−Ｋ７２１０に準ずるも
のである。The melt indexer used for the measurement of MFR was Model C-5059D2 manufactured by Toyo Seiki Co., Ltd. The structure of this device conforms to JIS-K7210.
【００４７】１次表面処理に使用したＳ−３２０は，チ
ッソ株式会社製のシラン系カップリング剤である。ま
た，樹脂混合工程で使用した樹脂は１２−ナイロン樹脂
（比重１.０２〜１.０４）である。S-320 used for the primary surface treatment is a silane coupling agent manufactured by Chisso Corporation. The resin used in the resin mixing step is 12-nylon resin (specific gravity 1.02 to 1.04).
【００４８】この条件でメルトフローレート（ＭＦＲ
値）を測定したところ，本例のＭＦＲ値は１０.３ｇ／
１０ｍｉｎであった。Under these conditions, the melt flow rate (MFR
Value), the MFR value of this example was 10.3 g /
It was 10 minutes.
【００４９】〔実施例２〜５〕微粉の平均粒子径と混合
比率を変えた以外は，実施例１と同様にして混合フエラ
イト粉末およびボンド磁石を得た。得られたフエライト
粉末およびボンド磁石の特性を表１および表２に示し
た。また，各フエライト粉末のＭＦＲ値を表２に示し
た。表示のように，実施例２〜５のボンド磁石はいずれ
も（ＢＨ）ｍａｘが２.５ＭＧＯｅ以上の高磁力品であ
った。[Examples 2 to 5] A mixed ferrite powder and a bonded magnet were obtained in the same manner as in Example 1 except that the average particle diameter of fine powder and the mixing ratio were changed. The properties of the obtained ferrite powder and the bonded magnet are shown in Tables 1 and 2. The MFR value of each ferrite powder is shown in Table 2. As shown, all the bonded magnets of Examples 2 to 5 were high magnetic force products having a (BH) max of 2.5 MGOe or more.
【００５０】〔比較例１〜４〕微粉の平均粒子径と混合
比率を変えた以外は，実施例１と同様にして混合フエラ
イト粉末およびボンド磁石を得た。得られたフエライト
粉末およびボンド磁石の特性を表１および表２に，また
各フエライト粉末のＭＦＲ値を表２に示した。比較例１
は微粉の混合比率が低いもの，比較例２は微粉の混合比
率が高いもの，比較例３は微粉の平均粒子径が小さいも
の，そして比較例４は微粉の平均粒子径が大きいもので
ある。比較例３で得られたボンド磁石は（ＢＨ）ｍａｘ
が２.３ＭＧＯｅ台と低かった。また，比較例１，２お
よび４で得られたフエライト粉末のＭＦＲは測定不可で
あり，これを射出成形したら流動性が悪いため成形機に
詰まり成形不可であった。[Comparative Examples 1 to 4] A mixed ferrite powder and a bonded magnet were obtained in the same manner as in Example 1 except that the average particle diameter of fine powder and the mixing ratio were changed. The properties of the obtained ferrite powder and the bonded magnet are shown in Tables 1 and 2, and the MFR value of each ferrite powder is shown in Table 2. Comparative Example 1
Indicates that the mixing ratio of fine powder is low, Comparative Example 2 indicates that the mixing ratio of fine powder is high, Comparative Example 3 indicates that the average particle size of fine powder is small, and Comparative Example 4 indicates that the average particle size of fine powder is large. The bonded magnet obtained in Comparative Example 3 has (BH) max
Was as low as 2.3 MGOe. In addition, the MFR of the ferrite powders obtained in Comparative Examples 1, 2 and 4 could not be measured, and injection molding thereof resulted in poor flowability, resulting in clogging in a molding machine and molding was impossible.
【００５１】[0051]
【表１】 [Table 1]
【００５２】[0052]
【表２】 [Table 2]
【００５３】〔実施例６〜８〕粗粉の平均粒子径を変更
した以外は，実施例１と同様にして混合フエライト粉末
およびボンド磁石を得た。得られたフエライト粉末およ
びボンド磁石の特性を表３および表４に，また各フエラ
イト粉末のＭＦＲ値を表４に示した。表４に見られるよ
うに，実施例６〜８のボンド磁石はいずれも（ＢＨ）ｍ
ａｘが２.５ＭＧＯｅ以上の高磁力品であった。[Examples 6 to 8] A mixed ferrite powder and a bonded magnet were obtained in the same manner as in Example 1 except that the average particle diameter of the coarse powder was changed. The properties of the obtained ferrite powder and the bonded magnet are shown in Tables 3 and 4, and the MFR value of each ferrite powder is shown in Table 4. As can be seen from Table 4, the bonded magnets of Examples 6 to 8 all have (BH) m.
The product had a high magnetic force of ax of 2.5 MGOe or more.
【００５４】〔比較例５〜６〕粗粉の平均粒子径を変更
した以外は，実施例１と同様にして混合フエライト粉末
およびボンド磁石を得た。得られたフエライト粉末およ
びボンド磁石の特性を表３および表４に，また各フエラ
イト粉末のＭＦＲ値を表４に示した。表示のように，比
較例５は粗粉の平均粒子径が小さいものであり，得られ
たフエライト粉末は成形不可であった。また，比較例６
は粗粉の平均粒子径が大きいものであるが，得られたボ
ンド磁石の（ＢＨ）ｍａｘは２.３２ＭＧＯｅであっ
た。[Comparative Examples 5-6] A mixed ferrite powder and a bonded magnet were obtained in the same manner as in Example 1 except that the average particle size of the coarse powder was changed. The properties of the obtained ferrite powder and the bonded magnet are shown in Tables 3 and 4, and the MFR value of each ferrite powder is shown in Table 4. As shown, in Comparative Example 5, the coarse powder had a small average particle diameter, and the obtained ferrite powder could not be molded. In addition, Comparative Example 6
Although the average particle diameter of the coarse powder was large, the (BH) max of the obtained bonded magnet was 2.32 MGOe.
【００５５】[0055]
【表３】 [Table 3]
【００５６】[0056]
【表４】 [Table 4]
【００５７】〔実施例９〜１０〕アニール温度を変えた
以外は，実施例１と同様にして混合フエライト粉および
ボンド磁石を得た。得られたフエライト粉末およびボン
ド磁石の特性を表５および表６に，また各フエライト粉
末のＭＦＲ値を表６に示した。表示のように，実施例９
〜１０のボンド磁石は，いずれも（ＢＨ）ｍａｘが２.
５ＭＧＯｅ以上の高磁力品であった。[Examples 9 to 10] A mixed ferrite powder and a bonded magnet were obtained in the same manner as in Example 1 except that the annealing temperature was changed. The characteristics of the obtained ferrite powder and the bonded magnet are shown in Tables 5 and 6, and the MFR value of each ferrite powder is shown in Table 6. As in the display, Example 9
(BH) max is 2. for all of the bonded magnets # 10 to # 10.
The product had a high magnetic force of 5 MGOe or more.
【００５８】〔実施例１１〕実施例１で得られたアニー
ル後のフエライト粉末について，次のように粉体ＰＨを
調整した。すなわち，フエライト粉末が２０％の濃度と
なるように水中でリパルプしたスラリーに，１％濃度の
希塩酸を滴下し，スラリーＰＨが６.０になるように調
整した。これを濾過，乾燥し，解砕して得られたフエラ
イト粉末およびこのフエライト粉末を用いて実施例１と
同様な方法で製造したボンド磁石の特性を表５および表
６に示した。フエライト粉末のＰＨは８.３であり，ボ
ンド磁石の（ＢＨ）ｍａｘは２.６４ＭＧＯｅの高磁力
品であった。Example 11 With respect to the annealed ferrite powder obtained in Example 1, the powder PH was adjusted as follows. That is, 1% dilute hydrochloric acid was added dropwise to a slurry repulped in water so that the ferrite powder had a concentration of 20%, and the slurry PH was adjusted to 6.0. Table 5 and Table 6 show the properties of the ferrite powder obtained by filtering, drying, and crushing this and the bonded magnet produced by the same method as in Example 1 using this ferrite powder. The ferrite powder had a PH of 8.3, and the bond magnet had a (BH) max of 2.64 MGOe, which was a high magnetic force product.
【００５９】〔比較例７〜８〕アニール温度を変えた以
外は，実施例１と同様にして混合フエライト粉およびボ
ンド磁石を得た。得られたフエライト粉末およびボンド
磁石の特性を表５および表６に，また各フエライト粉末
のＭＦＲ値を表６に示した。比較例７はアニール温度が
低いもの，比較例８はアニール温度が高いものである。
表示のように比較例７のボンド磁石の（ＢＨ）ｍａｘは
２.３１ＭＧＯｅであった。また比較例８で得られたフ
エライト粉末は成形不可であった。[Comparative Examples 7 to 8] A mixed ferrite powder and a bonded magnet were obtained in the same manner as in Example 1 except that the annealing temperature was changed. The characteristics of the obtained ferrite powder and the bonded magnet are shown in Tables 5 and 6, and the MFR value of each ferrite powder is shown in Table 6. Comparative Example 7 has a low annealing temperature, and Comparative Example 8 has a high annealing temperature.
As shown, the (BH) max of the bonded magnet of Comparative Example 7 was 2.31 MGOe. Further, the ferrite powder obtained in Comparative Example 8 could not be molded.
【００６０】〔比較例９〕実施例１で得られたアニール
後のフエライト粉末について，次のように粉体ＰＨを調
整した。フエライト粉末が２０％の濃度となるように水
中でリパルプしたスラリーに，１％濃度の希塩酸を滴下
し，スラリーＰＨが４.０になるように調整した。これ
を濾過，乾燥し，解砕して得られた最終粉末の特性を表
５に示した。この粉体のＰＨは５.７であった。このフ
エライト粉末を用いて，実施例１と同様にボンド磁石の
製造を試みたが，バインダーとの混練物の流動性が悪い
ために，射出成形できなかった。またＭＦＲの測定もで
きなかった。[Comparative Example 9] With respect to the annealed ferrite powder obtained in Example 1, the powder PH was adjusted as follows. Dilute hydrochloric acid having a concentration of 1% was added dropwise to a slurry repulped in water so that the ferrite powder had a concentration of 20%, and the slurry PH was adjusted to be 4.0. The characteristics of the final powder obtained by filtering, drying and crushing this are shown in Table 5. The pH of this powder was 5.7. Using this ferrite powder, an attempt was made to manufacture a bonded magnet in the same manner as in Example 1, but injection molding could not be performed because the kneaded material with the binder had poor fluidity. Also, the MFR could not be measured.
【００６１】〔比較例１０〕実施例１で得られたアニー
ル後のフエライト粉末について，粉体ＰＨの調整をしな
いで，実施例１と同様の方法でボンド磁石を製造するこ
とを試みたが，バインダーとの混練物の流動性が悪いた
めに射出成形できなかった。またＭＦＲの測定もできな
かった。Comparative Example 10 With respect to the annealed ferrite powder obtained in Example 1, an attempt was made to manufacture a bonded magnet by the same method as in Example 1 without adjusting the powder PH. Injection molding could not be performed due to poor fluidity of the kneaded product with the binder. Also, the MFR could not be measured.
【００６２】[0062]
【表５】 [Table 5]
【００６３】[0063]
【表６】 [Table 6]
【００６４】〔実施例１２〕微粉と粗粉を混合してから
アニールする代わりに，微粉と粗粉を混合する前に各々
別々に９５０℃で１時間アニールしてから混合した以外
は，実施例１と同様にして混合フエライト粉およびボン
ド磁石を得た。得られたフエライト粉末とボンド磁石の
特性を表７および表８に，またフエライト粉末のＭＦＲ
値を表８に示した。表示のように得られたボンド磁石の
（ＢＨ）ｍａｘは２.６１ＭＧＯｅの高磁力品であっ
た。[Embodiment 12] Instead of mixing the fine powder and the coarse powder and then annealing, the fine powder and the coarse powder were separately annealed at 950 ° C. for 1 hour and then mixed, respectively. A mixed ferrite powder and a bonded magnet were obtained in the same manner as in 1. The properties of the obtained ferrite powder and the bonded magnet are shown in Tables 7 and 8, and the MFR of the ferrite powder is shown.
The values are shown in Table 8. The (BH) max of the bond magnet obtained as shown in the figure was 2.61 MGOe, which was a high magnetic force product.
【００６５】〔実施例１３〕微粉の原料である炭酸スト
ロンチウムを炭酸バリウムに変えた以外は実施例１と同
様にして混合フエライト粉およびボンド磁石を得た（粗
粉の原料は実施例１と同じである）。得られたフエライ
ト粉末とボンド磁石の特性を表７および表８に，またフ
エライト粉末のＭＦＲ値を表８に示した。表示のよう
に，得られたボンド磁石の（ＢＨ）ｍａｘは２.５９Ｍ
ＧＯｅの高磁力品であった。[Example 13] A mixed ferrite powder and a bonded magnet were obtained in the same manner as in Example 1 except that barium carbonate was used instead of strontium carbonate as a raw material for fine powder (raw powder raw material was the same as in Example 1). Is). The properties of the obtained ferrite powder and the bonded magnet are shown in Tables 7 and 8, and the MFR value of the ferrite powder is shown in Table 8. As shown, the (BH) max of the obtained bonded magnet is 2.59M.
It was a high magnetic force product of GOe.
【００６６】〔実施例１４〕 (1)微粉の製造 酸化鉄と炭酸ストロンチウムをモル比で５.７になるよ
うに秤量して混合し，これを水で造粒し，乾燥後，電気
炉中１１００℃で２時間焼成した。この焼成品をサンプ
ルミルで粉砕し，さらに，ウエットミルで湿式粉砕し
て，平均粒子径が０.８５μｍのストロンチウムフエラ
イト粉末をえた。これを気流式遠心分級機で分級して，
平均粒子径０.４１μｍの微粉を得た。[Example 14] (1) Production of fine powder Iron oxide and strontium carbonate were weighed and mixed so that the molar ratio was 5.7, granulated with water, dried, and then placed in an electric furnace. It was baked at 1100 ° C. for 2 hours. The calcined product was ground with a sample mill and further wet-ground with a wet mill to obtain strontium ferrite powder having an average particle diameter of 0.85 μm. Classify this with an air flow type centrifugal classifier,
A fine powder having an average particle size of 0.41 μm was obtained.
【００６７】(2)粗粉の製造 実施例１で得られた粗粉を気流式遠心分級機で分級し
て，平均粒子径２.１０μｍの粗粉を得た。(2) Manufacture of coarse powder The coarse powder obtained in Example 1 was classified by a gas flow centrifugal classifier to obtain a coarse powder having an average particle size of 2.10 μm.
【００６８】(3)混合粉（フエライト粉末）の製造 前記 (1)の微粉３０重量％と (2)の粗粉残部（７０重量
％）を秤量後，良く混合し，その混合粉を電気炉中９５
０℃で１時間焼成（アニール）した。ついで，焼成品を
２０％の濃度になるように水中でリパルプ水洗した。こ
れを濾過，乾燥し解砕して，最終粉末として，次のスト
ロンチウムフエライト粉末を得た。 平均粒子径：１.３７μｍ， 比表面積：２.３３ｍ2／ｇ， 粒度分布の幾何標準偏差：２.３５， 圧縮密度：３.５８ｇ／ｃｍ3 ， 粉体ＰＨ：９.７(3) Production of mixed powder (ferrite powder) After weighing 30% by weight of the fine powder of (1) and the rest (70% by weight) of the coarse powder of (2), they were mixed well and the mixed powder was heated in an electric furnace. Medium 95
It was baked (annealed) at 0 ° C. for 1 hour. Then, the fired product was washed with repulp in water to a concentration of 20%. This was filtered, dried and crushed to obtain the following strontium ferrite powder as the final powder. Average particle size: 1.37 μm, specific surface area: 2.33 m 2 / g, geometric standard deviation of particle size distribution: 2.35, compression density: 3.58 g / cm 3 , powder PH: 9.7
【００６９】(4)ボンド磁石の製造 前記 (3)のフエライト粉末を用いて実施例１と同様にし
てボンド磁石を製造した。表８に示したように，得られ
たボンド磁石の（ＢＨ）ｍａｘは２.６７ＭＧＯｅの高
磁力品であった。(4) Production of Bonded Magnet A bonded magnet was produced in the same manner as in Example 1 using the ferrite powder of (3) above. As shown in Table 8, the obtained bonded magnet had a (BH) max of 2.67 MGOe and a high magnetic force.
【００７０】〔実施例１５〕ボンド磁石の製造時に，フ
エライト粉末９３.５部，シランン系カップリング剤０.
６部，１２−ナイロン５.５４部，オレイン酸０.３６部
に変更した以外は，実施例１４と同様にボンド磁石を製
造した。表８に示したように，得られたボンド磁石の
（ＢＨ）ｍａｘは２.７７ＭＧＯｅの高磁力品であっ
た。[Embodiment 15] 93.5 parts of ferrite powder and 0.1% of a silane coupling agent were used in the production of a bonded magnet.
A bonded magnet was produced in the same manner as in Example 14 except that 6 parts, 5.54 parts of 12-nylon and 0.36 parts of oleic acid were used. As shown in Table 8, the obtained bonded magnet had a (BH) max of 2.77 MGOe and a high magnetic force.
【００７１】[0071]
【表７】 [Table 7]
【００７２】[0072]
【表８】 [Table 8]
【００７３】[0073]
【発明の効果】以上説明したように，本発明のフエライ
ト粉末は，従来のボンド磁石で達成されたことのない
（ＢＨ）ｍａｘが２.５ＭＧＯｅ以上のボンド磁石が得
られる特性を有する。したがって，ＡＶ，ＯＡ機器，自
動車電装部品等に使用される小型モーターや，複写機の
マグネットロール等の分野において従来のものにはない
高磁力のボンド磁石を提供することができる。As described above, the ferrite powder of the present invention has a characteristic that a (BH) max of 2.5 MGOe or more, which has never been achieved by the conventional bonded magnet, can be obtained. Therefore, it is possible to provide a bond magnet having a high magnetic force, which is not available in the past, in the fields of small motors used in AV, OA equipment, automobile electrical components, etc., and magnet rolls of copying machines.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 天羽 隆一 岡山県和気郡佐伯町矢田1099−３ 日本弁 柄工業株式会社内 (72)発明者 延岡 則明 岡山県和気郡佐伯町矢田1099−３ 日本弁 柄工業株式会社内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Ryuichi Ama 1099-3 Yata, Saeki-cho, Wake-gun, Okayama Nihon Benai Kogyo Co., Ltd. (72) Noriaki Nobeoka 1099-3 Yada, Saeki-cho, Wake-gun, Okayama Within Japan Bengal Industry Co., Ltd.
Claims (9)
末であって，平均粒子径が０.９〜１.５μｍ，１ton/ｃ
ｍ2 の圧力で圧縮したときの圧縮密度が３.４０ｇ／ｃ
ｍ3 以上およびＪＩＳ Ｋ−５１０１で測定した粉体Ｐ
Ｈが７〜１０であるボンド磁石用フエライト粉末。1. A magnetoplumbite-type ferrite powder having an average particle size of 0.9 to 1.5 μm and 1 ton / c.
Compressed density when compressed at a pressure of m 2 is 3.40 g / c
Powder P measured by m 3 or more and JIS K-5101
Ferrite powder for bonded magnets, wherein H is 7 to 10.
末であって，平均粒子径が０.９〜１.５μｍ，１ton/ｃ
ｍ2 の圧力で圧縮したときの圧縮密度が３.４０ｇ／ｃ
ｍ3 以上，ＪＩＳ Ｋ−５１０１で測定した粉体ＰＨが
７〜１０および本文記載のＭＦＲ測定法に従ってフエラ
イト量９３重量％で測定したメルトフローレートが７ｇ
／１０ｍｉｎ以上であるボンド磁石用フエライト粉末。2. A magnetoplumbite type ferrite powder having an average particle size of 0.9 to 1.5 μm and 1 ton / c.
Compressed density when compressed at a pressure of m 2 is 3.40 g / c
m 3 or more, the powder PH measured by JIS K-5101 is 7 to 10 and the melt flow rate measured by a ferrite amount of 93% by weight according to the MFR measurement method described in the text is 7 g.
/ 10 min or more ferrite powder for bonded magnet.
子径０.３０〜０.５０μｍのマグネトプランバイト型フ
エライトの微粉１５〜４０重量％と，平均粒子径１.０
０〜２.５０μｍのマグネトプランバイト型フエライト
の粗粉残部とを混合して得られたものである請求項１ま
たは２に記載のボンド磁石用フエライト粉末。3. The average particle size of 0.9 to 1.5 μm is 15 to 40% by weight of fine particles of magnetoplumbite type ferrite having an average particle size of 0.30 to 0.50 μm, and the average particle size is 1.0.
The ferrite powder for bonded magnets according to claim 1 or 2, which is obtained by mixing with the remainder of the coarse powder of magnetoplumbite type ferrite having a size of 0 to 2.50 µm.
２.５である請求項１，２または３に記載のボンド磁石
用フエライト粉末。4. The geometric standard deviation σg of the particle size distribution is 1.8 to
The ferrite powder for a bonded magnet according to claim 1, wherein the ferrite powder is 2.5.
４.０ｍ2/ｇである請求項１，２，３または４に記載の
ボンド磁石用フエライト粉末。5. The specific surface area measured by the BET method is 1.5 to 5.
The ferrite powder for bonded magnets according to claim 1, 2, 3 or 4, which has an amount of 4.0 m 2 / g.
グネトプランバイト型フエライトの微粉と，平均粒子径
が１.００〜２.５０μｍのマグネトプランバイト型フエ
ライトの粗粉を準備する工程，前記の微粉１５〜４０重
量％と前記の粗粉残部とを混合する工程，およびこの混
合工程の前または後においてこれらの粉体を８００〜１
１００℃でアニールする工程からなる，平均粒子径が
０.９〜１.５μｍで１ton/ｃｍ2 の圧力で圧縮したとき
の圧縮密度が３.４０ｇ／ｃｍ3以上を示すボンド磁石用
フエライト粉末の製造方法。6. A step of preparing a fine powder of magnetoplumbite-type ferrite having an average particle diameter of 0.30 to 0.50 μm and a coarse powder of magnetoplumbite-type ferrite having an average particle diameter of 1.00 to 2.50 μm. , A step of mixing 15 to 40% by weight of the fine powder with the remainder of the coarse powder, and 800 to 1 of these powders before or after the mixing step.
A ferrite magnet for a bonded magnet, which has a mean particle size of 0.9 to 1.5 μm and a compression density of 3.40 g / cm 3 or more when compressed at a pressure of 1 ton / cm 2 and comprising an annealing step at 100 ° C. Production method.
グネトプランバイト型フエライトの微粉と，平均粒子径
が１.００〜２.５０μｍのマグネトプランバイト型フエ
ライトの粗粉を準備する工程，前記の微粉１５〜４０重
量％と前記の粗粉残部とを混合する工程，この混合工程
の前または後においてこれらの粉体を８００〜１１００
℃でアニールする工程，およびアニール工程後の粉体の
ＰＨを７〜１０に調整する工程からなる，平均粒子径が
０.９〜１.５μｍで１ton/cm2の圧力で圧縮したときの
圧縮密度が３.４０ｇ／ｃｍ3 以上を示すボンド磁石用
フエライト粉末の製造方法。7. A step of preparing a fine powder of magnetoplumbite-type ferrite having an average particle diameter of 0.30 to 0.50 μm and a coarse powder of magnetoplumbite-type ferrite having an average particle diameter of 1.00 to 2.50 μm. , A step of mixing 15 to 40% by weight of the fine powder with the remainder of the coarse powder, and 800 to 1100 of these powders before or after the mixing step.
Compressing when compressed at a pressure of 1 ton / cm 2 with an average particle size of 0.9 to 1.5 μm, which consists of a step of annealing at ℃, and a step of adjusting the PH of the powder after the annealing step to 7 to 10. A method for producing a ferrite powder for a bonded magnet, which has a density of 3.40 g / cm 3 or more.
トプランバイト型フエライトの粉末９３重量％以上を樹
脂系バインダーを用いて成形してなる（ＢＨ）ｍａｘが
２.５ＭＧＯｅ以上のフエライト系ボンド磁石。8. A ferrite having a (BH) max of 2.5 MGOe or more formed by molding 93% by weight or more of a powder of magnetoplumbite type ferrite having an average particle diameter of 0.9 to 1.5 μm using a resin binder. System bond magnet.
トプランバイト型フエライトの粉末９３重量％以上を樹
脂系バインダーを用いて成形密度３.９０ｇ／ｃｍ3 以
上に成形してなる（ＢＨ）ｍａｘが２.５ＭＧＯｅ以上
のフエライト系ボンド磁石。9. A 93% by weight or more powder of magnetoplumbite-type ferrite having an average particle diameter of 0.9 to 1.5 μm is molded using a resin binder to a molding density of 3.90 g / cm 3 or more ( BH) A ferrite-based bonded magnet with a max of 2.5 MGOe or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28816395A JP3257936B2 (en) | 1995-10-11 | 1995-10-11 | Ferrite powder for bonded magnet and bonded magnet using the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28816395A JP3257936B2 (en) | 1995-10-11 | 1995-10-11 | Ferrite powder for bonded magnet and bonded magnet using the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH09106904A true JPH09106904A (en) | 1997-04-22 |
| JP3257936B2 JP3257936B2 (en) | 2002-02-18 |
Family
ID=17726628
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP28816395A Expired - Lifetime JP3257936B2 (en) | 1995-10-11 | 1995-10-11 | Ferrite powder for bonded magnet and bonded magnet using the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3257936B2 (en) |
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