JP2006179576A - OXIDE FILM-COVERED Fe-Ni-Mo FLAT METAL SOFT MAGNETIC POWDER AND ITS MANUFACTURING METHOD HAVING HIGH SURFACE FINISH. - Google Patents
OXIDE FILM-COVERED Fe-Ni-Mo FLAT METAL SOFT MAGNETIC POWDER AND ITS MANUFACTURING METHOD HAVING HIGH SURFACE FINISH. Download PDFInfo
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Abstract
Description
この発明は、優れた電波吸収特性を有する電波吸収体や優れた磁気特性を有する無線通信用アンテナコアなどの高周波用磁性材料に使用される高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末およびその製造方法に関するものである。また、この発明は、前記高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末を樹脂中に配向させて分散させた高抵抗率および低保磁力を有する磁性複合シートに関するものである。 The present invention relates to an oxide film-coated Fe-Ni-Mo having a high surface roughness used for a high frequency magnetic material such as a radio wave absorber having excellent radio wave absorption characteristics and an antenna core for radio communication having excellent magnetic characteristics. The present invention relates to a flat metal soft magnetic powder and a method for producing the same. The present invention also relates to a magnetic composite sheet having a high resistivity and a low coercive force in which the oxide film-coated Fe-Ni-Mo-based flat metal soft magnetic powder having a high surface roughness is oriented and dispersed in a resin. Is.
一般に、パーマロイにＭｏを添加したＭｏパーマロイ（Ｆｅ−７９％Ｎｉ−４％Ｍｏ）やスーパーマロイ（Ｆｅ−７９％Ｎｉ−５％Ｍｏ）などのＦｅ−Ｎｉ−Ｍｏ系軟磁性粉末は知られており、これら材料はＭｏの添加により熱処理後に徐冷しても、ＦｅＮｉ３規則相の生成が抑制され、熱処理後の急冷を施さなくても結晶磁気異方性定数Ｋ１が零前後となり、結晶方位の上で等方的な多結晶体においても優れた透磁率を示すため、工業的にも広く使用されている。また、さらに透磁率を改善するためにＭｏのほかにさらにＣｕ、Ｃｒ、Ｍｎを添加した高透磁率軟磁性材料も知られている。 In general, Fe-Ni-Mo soft magnetic powders such as Mo permalloy (Fe-79% Ni-4% Mo) and supermalloy (Fe-79% Ni-5% Mo) in which Mo is added to permalloy are known. cage, even gradually cooled after the heat treatment of these materials by the addition of Mo, is suppressed generation of FeNi 3 ordered phase, the magnetocrystalline anisotropy constant K 1 without subjected to quenching after the heat treatment becomes zero before and after crystallization Polycrystalline materials that are isotropic in orientation are also widely used industrially because they exhibit excellent magnetic permeability. Further, a high magnetic permeability soft magnetic material in which Cu, Cr, or Mn is added in addition to Mo to further improve the magnetic permeability is also known.
前記Ｆｅ−Ｎｉ−Ｍｏ系軟磁性粉末は、一般に、扁平化して使用されることが多い。例えば、特許文献１には、質量％で（以下、％は質量％を示す。）、Ｆｅ−７０〜８３％Ｎｉ−２〜６％Ｍｏ−３〜６％Ｃｕ−１〜２％Ｍｎの組成を有し、平均粒径：０．１〜３０μm、平均厚さ：２μｍ以下を有する扁平金属軟磁性粉末が記載されており、この扁平金属軟磁性粉末は磁気シールド用に使用されることが記載されている。
また、特許文献２には、Ｆｅ−４０〜８０％Ｎｉ−２〜６％Ｍｏの組成を有し、厚さ：１〜５μｍ、厚さと長さの比が１：５〜２００を有する扁平フレーク状軟磁性粉末が記載されており、この扁平フレーク状軟磁性粉末は路面などの標識体に使用されることが記載されている。
さらに、特許文献３には、Ｆｅ−６０〜８０％ＮｉまたはＦｅ−６０〜８０％Ｎｉ−５％以下Ｍｏの組成を有し、フレーク厚さ：３０μｍ以下、フレーク径：５０〜２０００μｍを有する扁平金属軟磁性粉末が記載されており、この扁平金属軟磁性粉末は高周波用磁性材料として使用することが記載されている。
In general, the Fe—Ni—Mo soft magnetic powder is often used after being flattened. For example, Patent Document 1 discloses the composition of Fe-70 to 83% Ni-2 to 6% Mo-3 to 6% Cu-1 to 2% Mn in mass% (hereinafter,% represents mass%). A flat metal soft magnetic powder having an average particle diameter of 0.1 to 30 μm and an average thickness of 2 μm or less is described. The flat metal soft magnetic powder is used for a magnetic shield. Has been.
Patent Document 2 discloses a flat flake having a composition of Fe-40 to 80% Ni-2 to 6% Mo, a thickness of 1 to 5 μm, and a thickness to length ratio of 1: 5 to 200. A soft magnetic powder is described, and it is described that this flat flaky soft magnetic powder is used for a marking body such as a road surface.
Further, Patent Document 3 discloses a flat composition having a composition of Fe-60 to 80% Ni or Fe-60 to 80% Ni-5% or less, a flake thickness: 30 μm or less, and a flake diameter: 50 to 2000 μm. A metal soft magnetic powder is described, and it is described that this flat metal soft magnetic powder is used as a magnetic material for high frequency.
これら従来のＦｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末は、いずれも通常の粉砕またはアトマイズして得られたＦｅ−Ｎｉ−Ｍｏ系粉末にエタノールや水を溶媒として添加し、さらに必要に応じて粉砕助剤を添加し、これらをアトライターやボールミルを使用して扁平化処理することにより製造されている。
このようにして製造したＦｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末は、樹脂中に扁平面が磁性複合シートの厚さ方向に対して直角方向に配向するように分散させて磁性複合シートを作製し、数１０ＭＨｚ〜数ＧＨｚにて電波吸収特性を有する電波吸収体、または数１０ｋＨｚ〜数１０ＭＨｚで磁気特性を有する無線通信用アンテナコアなどの高周波用磁性材料として使用されることも知られている。
かかる従来のＦｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末を樹脂中に扁平面が磁性複合シートの厚さ方向に対して直角方向に配向するように分散させた磁性複合シートを電波吸収体または無線通信用アンテナコアなどの高周波用磁性材料として使用し、その特性を高めようとすると、磁性複合シートに含まれるＦｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の充填密度を上げる必要があるが、Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の充填密度を上げると、隣接するＦｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末が接触し、Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末相互の絶縁を保つことが難しくなって磁性複合シートの抵抗率が１０３Ωｃｍ未満に低下し、電波吸収体および高周波用磁性材料としての特性が低下するので好ましくない。このような場合には、Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末を予め絶縁体でコーティングしておくことが好ましいことも知られている（特許文献４参照）。
The Fe—Ni—Mo-based flat metal soft magnetic powder thus produced is dispersed in the resin so that the flat surface is oriented in a direction perpendicular to the thickness direction of the magnetic composite sheet to produce a magnetic composite sheet. It is also known to be used as a radio frequency magnetic material such as a radio wave absorber having radio wave absorption characteristics at several tens of MHz to several GHz, or an antenna core for wireless communication having magnetic characteristics at several tens of kHz to several tens of MHz. .
A magnetic composite sheet in which such a conventional Fe—Ni—Mo-based flat metal soft magnetic powder is dispersed in a resin so that the flat surface is oriented in a direction perpendicular to the thickness direction of the magnetic composite sheet is used as a radio wave absorber or wireless. When it is used as a magnetic material for high frequency such as a communication antenna core and its characteristics are to be improved, it is necessary to increase the packing density of the Fe-Ni-Mo-based flat metal soft magnetic powder contained in the magnetic composite sheet. -When the packing density of the Ni-Mo-based flat metal soft magnetic powder is increased, adjacent Fe-Ni-Mo-based flat metal soft magnetic powders come into contact with each other to maintain insulation between the Fe-Ni-Mo-based flat metal soft magnetic powders. This makes it difficult to reduce the resistivity of the magnetic composite sheet to less than 10 3 Ωcm, which lowers the properties as a radio wave absorber and a magnetic material for high frequency. In such a case, it is also known that it is preferable to coat the Fe—Ni—Mo-based flat metal soft magnetic powder with an insulator in advance (see Patent Document 4).
一般に、金属軟磁性粉末の表面に予め絶縁体でコーティングする方法の一つとして、金属軟磁性粉末の表面に酸化膜を形成することが知られていることから、Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末を酸化雰囲気中で加熱することによりＦｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の表面に前記絶縁を保つために一定以上の厚さの酸化膜を形成した酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末を作製することが考えられる。この場合、前記絶縁を保つために必要な酸化膜の厚みは酸化膜の抵抗率に反比例する。しかし、Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末を酸化雰囲気中で加熱してＦｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の表面に前記絶縁を保つために必要な酸化膜を形成するには、Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末が比較的優れた耐食性を有することから、酸化雰囲気中でしかも比較的高温度の３００〜４００℃で加熱しなければならず、かかる高温で加熱すると、酸化膜として抵抗率の低いＮｉＯが形成される。このため前記絶縁を保つために必要なＮｉＯ酸化膜の厚みは大きくする必要があり、この厚みの大きなＮｉＯが形成されたＦｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末は保磁力が大幅に上昇し、かかる高保磁力を有するＦｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末を用いて作製した複合磁性シートは電波吸収体および高周波用磁性材料としての特性は大幅に低下するので好ましくない。 In general, as one method of coating the surface of the metal soft magnetic powder with an insulator in advance, it is known to form an oxide film on the surface of the metal soft magnetic powder. An oxide film coated Fe—Ni— in which an oxide film of a certain thickness or more is formed on the surface of the Fe—Ni—Mo flat metal soft magnetic powder by heating the soft magnetic powder in an oxidizing atmosphere. It is conceivable to prepare a Mo-based flat metal soft magnetic powder. In this case, the thickness of the oxide film necessary for maintaining the insulation is inversely proportional to the resistivity of the oxide film. However, in order to form an oxide film necessary for maintaining the insulation on the surface of the Fe-Ni-Mo flat metal soft magnetic powder by heating the Fe-Ni-Mo flat metal soft magnetic powder in an oxidizing atmosphere. Since the Fe—Ni—Mo-based flat metal soft magnetic powder has relatively excellent corrosion resistance, it must be heated in an oxidizing atmosphere and at a relatively high temperature of 300 to 400 ° C. When heated at such a high temperature, NiO having a low resistivity is formed as the oxide film. For this reason, it is necessary to increase the thickness of the NiO oxide film necessary for maintaining the insulation, and the coercive force of the Fe—Ni—Mo flat metal soft magnetic powder formed with NiO having a large thickness is greatly increased. A composite magnetic sheet produced using such a Fe—Ni—Mo-based flat metal soft magnetic powder having a high coercive force is not preferable because the characteristics as a radio wave absorber and a magnetic material for high frequency are greatly reduced.
そこで、本発明者らは、Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の表面に酸化膜を被覆した酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末を作製し、この酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末を用いて電波吸収体または高周波用磁性材料として優れた特性を有する高抵抗率および低保磁力の磁性複合シートを得るべく研究を行った。その結果、
（イ）Ｆｅ−Ｎｉ−Ｍｏ系金属軟磁性粉末を溶媒とともにアトライタやボールミルを使用し扁平化処理して得られた平均粒径：３０〜１５０μｍ、アスペクト比：５〜５００の範囲内にある通常のＦｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末を水（一層好ましくは蒸留水）中で煮沸すると、Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の表面に高抵抗率を有する酸化膜が形成され、この煮沸により形成された酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の比表面積をＳＲとし、表面に凹凸のない平滑な表面を有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の計算で求めた比表面積をＳＩとし、ＳＲをＳＩで除した比例係数をｋとすると、前記煮沸により形成された高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末は、ＳＲ／ＳＩ＝ｋ（ただし、ｋは比例係数であって、ｋ＝１０〜２００）の条件を満たす比表面積を有し、
一方、大気中などの通常の酸化性雰囲気中で加熱することにより作製した酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の比例係数ｋは８を越えることはないことから、煮沸することにより得られた酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の比例係数ｋは大気中で加熱することにより作製した通常の酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の比例係数に比べて格段に大きく、したがって、煮沸することにより得られた酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の表面粗さは、大気中などの通常の酸化雰囲気中で加熱することにより得られた通常の酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の表面粗さに比べて格段に大きい、
（ロ）この煮沸することにより得られたＦｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の表面に形成された酸化膜は組成式：ＮｉｘＦｅ３−ｘＯ４（ただし、０＜ｘ＜３）で表され、この酸化膜は従来の酸化雰囲気中で加熱することによりＦｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の表面に形成された同じ厚さのＮｉＯ酸化膜と比べて抵抗率が高いところから、一層抵抗率の高い酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末が得られ、この酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末に樹脂を混合し固化して得られた複合磁性シートの抵抗率は一層向上する、
（ハ）また、この発明の煮沸することにより表面にＮｉｘＦｅ３−ｘＯ４（ただし、０＜ｘ＜３）の酸化膜が形成されたＦｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末は、煮沸温度が１００℃前後であるから比較的低温で加熱されることから、前記絶縁を保つために必要な酸化膜の厚みをＮｉＯ酸化膜と比べて小さくすることができ、このためにその製造過程でＦｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の保磁力を上昇させることがない、
（ニ）前記煮沸することにより得られた高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末を作製するためのＦｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末は、Ｎｉ：６０〜９０％、Ｍｏ：０．０５〜１．９５％を含有し、残部：Ｆｅおよび不可避不純物からなる成分組成を有することが一層好ましい、などの知見を得たのである。
Therefore, the present inventors produced an oxide film-coated Fe-Ni-Mo-based flat metal soft magnetic powder in which an oxide film was coated on the surface of the Fe-Ni-Mo-based flat metal soft magnetic powder, and this oxide film-coated Fe Research was conducted to obtain a magnetic composite sheet having a high resistivity and a low coercive force having excellent characteristics as a radio wave absorber or a high-frequency magnetic material using a Ni-Mo flat metal soft magnetic powder. as a result,
(B) Average particle diameter obtained by flattening Fe—Ni—Mo based metal soft magnetic powder together with a solvent using an attritor or ball mill: 30 to 150 μm, aspect ratio: usually within the range of 5 to 500 When the Fe-Ni-Mo flat metal soft magnetic powder is boiled in water (more preferably distilled water), an oxide film having a high resistivity is formed on the surface of the Fe-Ni-Mo flat metal soft magnetic powder. The specific surface area of the oxide film coated Fe—Ni—Mo based flat metal soft magnetic powder formed by boiling is SR, and the oxide film coated Fe—Ni—Mo based flat metal soft powder having a smooth surface with no irregularities on the surface is used. When the specific surface area obtained by calculation of the magnetic powder is SI, and the proportionality coefficient obtained by dividing SR by SI is k, the oxide-coated Fe-Ni-Mo-based flat metal softening having a high surface roughness formed by the boiling is performed. Magnetic powder Is, SR / SI = k (however, k is a proportional coefficient, k = 10 to 200) has a satisfying specific surface area of,
On the other hand, since the proportionality coefficient k of the oxide film-coated Fe—Ni—Mo-based flat metal soft magnetic powder produced by heating in a normal oxidizing atmosphere such as the air does not exceed 8, boiling is performed. The proportionality coefficient k of the oxide film-coated Fe-Ni-Mo-based flat metal soft magnetic powder obtained by the above is proportional to the normal oxide film-coated Fe-Ni-Mo-based flat metal soft magnetic powder prepared by heating in the atmosphere. Therefore, the surface roughness of the oxide film-coated Fe-Ni-Mo flat metal soft magnetic powder obtained by boiling is to be heated in a normal oxidizing atmosphere such as in the air. It is much larger than the surface roughness of the normal oxide film-coated Fe-Ni-Mo-based flat metal soft magnetic powder obtained by
(B) The oxide film formed on the surface of the Fe—Ni—Mo-based flat metal soft magnetic powder obtained by boiling is represented by the composition formula: Ni x Fe 3-x O4 (where 0 <x <3) This oxide film has a higher resistivity than a NiO oxide film of the same thickness formed on the surface of a Fe-Ni-Mo flat metal soft magnetic powder by heating in a conventional oxidizing atmosphere. Thus, an oxide film-coated Fe—Ni—Mo-based flat metal soft magnetic powder having a higher resistivity is obtained, and this oxide film-coated Fe—Ni—Mo-based flat metal soft magnetic powder is obtained by mixing and solidifying a resin. The resistivity of the composite magnetic sheet is further improved.
(C) In addition, the Fe—Ni—Mo-based flat metal soft magnetic powder in which an oxide film of Ni x Fe 3-x O4 (where 0 <x <3) is formed on the surface by boiling of the present invention, Since the boiling temperature is around 100 ° C., the oxide film is heated at a relatively low temperature, so that the thickness of the oxide film necessary for maintaining the insulation can be made smaller than that of the NiO oxide film. And does not increase the coercive force of the Fe-Ni-Mo flat metal soft magnetic powder,
(D) Fe-Ni-Mo-based flat metal soft magnetic powder for producing an oxide film-coated Fe-Ni-Mo-based flat metal soft magnetic powder having a high surface roughness obtained by boiling is Ni : 60 to 90%, Mo: 0.05 to 1.95%, the balance: it is more preferable to have a component composition consisting of Fe and inevitable impurities.
この発明は、かかる知見に基づいて成されたものであって、
（１）平均粒径：３０〜１５０μｍおよびアスペクト比（平均粒径／平均厚さ）：５〜５００を有し高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末であって、
前記高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の比表面積をＳＲ、
表面に凹凸のない平滑な表面を有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の計算で求めた比表面積をＳＩとすると、
前記ＳＲとＳＩの比が、ＳＲ／ＳＩ＝ｋ（ただし、ｋは表面粗さを表現する比例係数であって、ｋ＝１０〜２００）の条件を満たす範囲内の比表面積を有する高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末、
（２）前記酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末は、質量％で（以下、％は質量％を示す）、Ｎｉ：６０〜９０％、Ｍｏ：０．０５〜１．９５％を含有し、残部：Ｆｅおよび不可避不純物からなる成分組成を有するＦｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の表面に酸化膜が形成されている粉末である前記（１）記載の高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末、
（３）前記Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の表面に形成されている酸化膜は、ＮｉｘＦｅ３−ｘＯ４（ただし、０＜ｘ＜３）である前記（１）または（２）記載の高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末、
（４）平均粒径：３０〜１５０μｍおよびアスペクト比（平均粒径／平均厚さ）：５〜５００を有するＦｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末を水中で煮沸する前記（１）、（２）または（３）記載の高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の製造方法、
（５）平均粒径：３０〜１５０μｍおよびアスペクト比（平均粒径／平均厚さ）：５〜５００を有しかつ質量％で（以下、％は質量％を示す）Ｎｉ：６０〜９０％、Ｍｏ：０．０５〜１．９５％を含有し、残部：Ｆｅおよび不可避不純物からなる成分組成を有するＦｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末を水中で煮沸する前記（１）、（２）または（３）記載の高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の製造方法、
（６）前記煮沸するための水は蒸留水である前記（４）または（５）記載の高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の製造方法、
（７）前記（１）、（２）または（３）記載の高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の扁平面が磁性複合シートの厚さ方向に対して直角方向に配向して分散している磁性複合シート、に特徴を有するものである。
This invention is made based on such knowledge,
(1) An oxide film-coated Fe—Ni—Mo-based flat metal soft magnetic powder having an average particle size of 30 to 150 μm and an aspect ratio (average particle size / average thickness) of 5 to 500 and having a high surface roughness. There,
The specific surface area of the oxide film-coated Fe—Ni—Mo based flat metal soft magnetic powder having high surface roughness is SR,
When the specific surface area obtained by calculation of the oxide film-coated Fe-Ni-Mo-based flat metal soft magnetic powder having a smooth surface without unevenness on the surface is defined as SI,
A high surface roughness having a specific surface area within a range where the ratio of SR and SI satisfies the condition of SR / SI = k (where k is a proportional coefficient expressing surface roughness, k = 10 to 200). Oxide-coated Fe-Ni-Mo-based flat metal soft magnetic powder having thickness,
(2) The oxide film-coated Fe—Ni—Mo-based flat metal soft magnetic powder is in mass% (hereinafter, “%” represents mass%), Ni: 60 to 90%, Mo: 0.05 to 1.95. The high surface roughness according to (1) above, which is a powder in which an oxide film is formed on the surface of a Fe—Ni—Mo-based flat metal soft magnetic powder having a component composition comprising:% and the balance: Fe and inevitable impurities Oxide-coated Fe-Ni-Mo-based flat metal soft magnetic powder having thickness,
(3) The oxide film formed on the surface of the Fe—Ni—Mo-based flat metal soft magnetic powder is Ni x Fe 3-x O4 (where 0 <x <3) (1) or ( 2) Oxide film-coated Fe—Ni—Mo based flat metal soft magnetic powder having a high surface roughness according to the description;
(4) The above (1), wherein the Fe—Ni—Mo flat metal soft magnetic powder having an average particle size of 30 to 150 μm and an aspect ratio (average particle size / average thickness) of 5 to 500 is boiled in water. 2) or a method for producing an oxide film-coated Fe—Ni—Mo-based flat metal soft magnetic powder having a high surface roughness according to (3),
(5) Average particle diameter: 30 to 150 μm and aspect ratio (average particle diameter / average thickness): 5 to 500 and in mass% (hereinafter,% indicates mass%) Ni: 60 to 90%, The above (1), (2), wherein Fe: Ni-Mo-based flat metal soft magnetic powder containing Mo: 0.05 to 1.95% and having the composition of the balance: Fe and inevitable impurities is boiled in water. Or a method for producing an oxide film-coated Fe—Ni—Mo-based flat metal soft magnetic powder having a high surface roughness according to (3),
(6) The method for producing an oxide film-coated Fe—Ni—Mo-based flat metal soft magnetic powder having a high surface roughness according to (4) or (5), wherein the water for boiling is distilled water,
(7) The flat surface of the oxide film-coated Fe—Ni—Mo-based flat metal soft magnetic powder having the high surface roughness described in (1), (2) or (3) is in the thickness direction of the magnetic composite sheet. The magnetic composite sheet is oriented and dispersed in a perpendicular direction.
前記（４）〜（６）記載の高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の製造方法において、Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末を煮沸する時間は１０分から１０時間の範囲内であることが好ましい。煮沸時間が１０分未満であると十分な厚さの酸化膜が形成されないので好ましくなく、一方、１０時間を越えて煮沸すると、形成される酸化膜が厚くなり過ぎ、酸化膜が厚くなり過ぎると保磁力が増加するようになるので好ましくないという理由によるものである。
この発明の高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末を高密度に樹脂を混合し固化して得られた複合磁性シートの抵抗率はその表面粗さが粗いために上昇する。その理由としては、粉末の表面に形成されている凹凸によって隣接する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末相互の接触面積が小さくなり、粉末と粉末の隙間に樹脂がまんべんなく行き渡り、得られた複合磁性シートの抵抗率を上昇させるものと考えられる。
In the method for producing an oxide film-coated Fe—Ni—Mo-based flat metal soft magnetic powder having a high surface roughness according to (4) to (6), the time for boiling the Fe—Ni—Mo-based flat metal soft magnetic powder Is preferably in the range of 10 minutes to 10 hours. If the boiling time is less than 10 minutes, an oxide film having a sufficient thickness cannot be formed. On the other hand, if the boiling time exceeds 10 hours, the formed oxide film becomes too thick and the oxide film becomes too thick. This is because the coercive force increases, which is not preferable.
The resistivity of the composite magnetic sheet obtained by solidifying the oxide film-coated Fe-Ni-Mo-based flat metal soft magnetic powder having a high surface roughness and solidifying the resin according to the present invention is rough. To rise. The reason for this is that the contact area between adjacent oxide film-coated Fe-Ni-Mo flat metal soft magnetic powders is reduced by the unevenness formed on the surface of the powder, and the resin spreads evenly between the powder and the powder, It is considered that the resistivity of the obtained composite magnetic sheet is increased.
この発明の高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末を製造するには、通常の市販のＦｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末を水中、特に蒸留水中で煮沸したのち乾燥すれば良い。
また、この発明の磁性複合シートで使用する樹脂は、塩素化ポリエチレン、シリコーン、ウレタン、酢酸ビニル、エチレン-酢酸ビニル共重合体、ＡＢＳ樹脂、塩化ビニル、ポリビニルブチラル、熱可塑性エラストマー、ＥＭ−ＰＭ−ＢＤ共重合ゴム、スチレン‐ブタジエン系ゴム、アクリロニトリル−ブタジエン系ゴムなどであり、さらにこれらをブレンドしたものまたはブレンドし変成したものであってもよい。
In order to produce the oxide film-coated Fe—Ni—Mo based flat metal soft magnetic powder having a high surface roughness according to the present invention, an ordinary commercially available Fe—Ni—Mo based flat metal soft magnetic powder is submerged in water, particularly distilled water. You can boil it and dry it.
The resin used in the magnetic composite sheet of the present invention is chlorinated polyethylene, silicone, urethane, vinyl acetate, ethylene-vinyl acetate copolymer, ABS resin, vinyl chloride, polyvinyl butyral, thermoplastic elastomer, EM-PM. -BD copolymer rubber, styrene-butadiene rubber, acrylonitrile-butadiene rubber, and the like, and those blended or blended and modified.
この発明の高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末において、成分組成、平均粒径、アスペクト比および比表面積を前述の如く限定した理由を説明する。 The reason why the component composition, average particle diameter, aspect ratio, and specific surface area of the oxide film-coated Fe—Ni—Mo-based flat metal soft magnetic powder having high surface roughness according to the present invention are limited as described above will be described.
成分組成：
この発明の高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末を構成するＦｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末に含まれるＮｉの含有量を６０〜９０％に限定した理由は、６０％より少なくても９０％より多くても磁気特性が低下するからであり、この範囲は通常知られている範囲であるが、この発明の高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末におけるＮｉの含有量は、７０〜８５％の範囲内にあることが一層好ましい。
また、Ｍｏが０．０５％未満では熱処理後の徐冷によりＦｅＮｉ３規則相の生成が過剰になり、結晶磁気異方性定数Ｋ１が負でその絶対値が大きくなり過ぎて磁気特性が低下し、一方、１．９５％よりも多く含有すると、ＦｅＮｉ３規則相の生成が不十分となり、結晶磁気異方性定数Ｋ１が負でその絶対値が小さくなり過ぎたり、正になったりして、結晶磁気異方性により扁平面内をより一層磁化容易面とする効果が不十分となり、扁平面内の透磁率が低下するのでＭｏの添加量を０．０５〜１．９５％に限定することが好ましい。この発明の高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末においてＭｏの含有量の一層好ましい範囲は０．５〜１．９５％（より一層好ましくは０．８〜１．９％）である。
Ingredient composition:
The content of Ni contained in the Fe-Ni-Mo-based flat metal soft magnetic powder constituting the oxide film-coated Fe-Ni-Mo-based flat metal soft magnetic powder having a high surface roughness of the present invention is 60 to 90%. The reason for the limitation is that the magnetic properties are deteriorated even if it is less than 60% or more than 90%, and this range is a generally known range, but the oxide film having a high surface roughness according to the present invention. The Ni content in the coated Fe—Ni—Mo-based flat metal soft magnetic powder is more preferably in the range of 70 to 85%.
Further, Mo is less than 0.05% becomes excessive generation of FeNi 3 ordered phase by slow cooling after the heat treatment, decreased magnetic properties magnetocrystalline anisotropy constant K 1 is the absolute value is too large in a negative On the other hand, if the content is more than 1.95%, the formation of the FeNi 3 ordered phase becomes insufficient, the magnetocrystalline anisotropy constant K 1 is negative, and its absolute value becomes too small or becomes positive. Thus, the effect of making the flat plane more easily magnetized due to the magnetocrystalline anisotropy becomes insufficient, and the magnetic permeability in the flat plane decreases, so the amount of Mo added is limited to 0.05 to 1.95% It is preferable to do. In the oxide film-coated Fe—Ni—Mo-based flat metal soft magnetic powder having a high surface roughness according to the present invention, the more preferable range of the Mo content is 0.5 to 1.95% (more preferably 0.8 to 1.9%).
平均粒径：
この発明の高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末において平均粒径が３０μｍよりも小さいと、扁平化処理時の歪の導入が著しくなり、十分な磁気特性が得られないので好ましくなく、一方、１５０μｍを超えると、シート等を作製する際の樹脂等との混練において、粉末が折れ曲がったり、ちぎれたりして磁気特性が低下するので好ましくない。したがって、この発明の高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の平均粒径は３０〜１５０μｍに定めた。平均粒径の一層好ましい範囲は３５〜１４０μｍである。
Average particle size:
In the oxide film-coated Fe—Ni—Mo-based flat metal soft magnetic powder having a high surface roughness according to the present invention, when the average particle size is smaller than 30 μm, the introduction of strain during the flattening treatment becomes remarkable and sufficient magnetic properties are obtained. On the other hand, if it exceeds 150 μm, the powder is bent or broken in kneading with a resin or the like when producing a sheet or the like, and the magnetic properties are lowered, which is not preferable. Therefore, the average particle diameter of the oxide film-coated Fe—Ni—Mo-based flat metal soft magnetic powder having a high surface roughness according to the present invention is set to 30 to 150 μm. A more preferable range of the average particle diameter is 35 to 140 μm.
アスペクト比：
この発明の高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末においてアスペクト比が５より小さいと、粉末の反磁界が大きくなり、扁平面内の透磁率が低下するので好ましくなく、一方、アスペクト比が５００よりも大きくなると、扁平化処理時の歪の導入が著しくなり、十分な磁気特性が得られなくなるので好ましくない。したがって、この発明の高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末のアスペクト比は５〜５００に定めた。
比表面積：
この発明の高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の比表面積ＳＲ、表面に凹凸のない平滑な表面を有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の比表面積をＳＩとすると、ＳＲ＝ｋ・ＳＩ（ただし、ｋは表面粗さを表現する比例係数であって、ｋ＝１０〜２００）の条件を満たす範囲内の比表面積を有する。すなわち、比例係数ｋはｋ＝ＳＲ／ＳＩで定義される係数であるが、比例係数ｋが大きくなるほど表面粗さが大きくなる。しかし、比例係数ｋが１０未満の酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末では従来と比べて十分な高抵抗率を有する複合磁性シートを作製することができないので好ましくなく、一方、比例係数ｋが２００を越える酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末を作製するには相当時間の煮沸を行わなければならず、現実的でないからである。
この発明の高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の比表面積を、ＳＲ＝ｋ・ＳＩで表現したのは、粉末の比表面積は一般に同じ表面粗さを有する粉末であっても、粒径が小さくなるほど大きな比表面積値を示すためであり、粒径の大小にかかわらず正確な比表面積を得るためには、粉末の比表面積をＳＲ＝ｋ・ＳＩという式で定義することが必要であり、この定義を用いれば粉末の粒径の大小に関係なく正確な比表面積を得られるからである。
aspect ratio:
If the aspect ratio of the oxide-coated Fe-Ni-Mo flat metal soft magnetic powder having a high surface roughness according to the present invention is less than 5, the demagnetizing field of the powder increases and the magnetic permeability in the flat plane decreases. On the other hand, if the aspect ratio is greater than 500, the introduction of strain during the flattening process becomes significant, and sufficient magnetic properties cannot be obtained. Therefore, the aspect ratio of the oxide film-coated Fe—Ni—Mo-based flat metal soft magnetic powder having a high surface roughness according to the present invention is set to 5 to 500.
Specific surface area:
Specific surface area SR of oxide-coated Fe-Ni-Mo-based flat metal soft magnetic powder having a high surface roughness of the present invention, and oxide-coated Fe-Ni-Mo-based flat metal soft having a smooth surface with no irregularities on the surface Assuming that the specific surface area of the magnetic powder is SI, the magnetic powder has a specific surface area within a range that satisfies the condition of SR = k · SI (where k is a proportional coefficient expressing surface roughness, k = 10 to 200). That is, the proportional coefficient k is a coefficient defined by k = SR / SI, but the surface roughness increases as the proportional coefficient k increases. However, an oxide film-coated Fe-Ni-Mo-based flat metal soft magnetic powder having a proportionality coefficient k of less than 10 is not preferable because a composite magnetic sheet having a sufficiently high resistivity cannot be produced compared to the conventional one, This is because, in order to produce an oxide film-coated Fe—Ni—Mo-based flat metal soft magnetic powder having a proportionality coefficient k exceeding 200, boiling must be performed for a considerable time, which is not practical.
The specific surface area of the oxide-coated Fe-Ni-Mo-based flat metal soft magnetic powder having a high surface roughness according to the present invention is expressed by SR = k · SI. The specific surface area of the powder generally has the same surface roughness. This is because the specific surface area of the powder is SR = k · SI in order to obtain an accurate specific surface area regardless of the particle size. This is because an accurate specific surface area can be obtained regardless of the particle size of the powder.
この発明の高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末は、アンテナ、インダクタ用として高抵抗率を有する高周波磁性材料を提供することができ、さらに高抵抗率を有する電波吸収体を提供することができ、電気および電子産業において優れた効果をもたらすものである。 The oxide film-coated Fe-Ni-Mo-based flat metal soft magnetic powder having a high surface roughness according to the present invention can provide a high-frequency magnetic material having a high resistivity for an antenna and an inductor, and further has a high resistivity. It is possible to provide a radio wave absorber having an excellent effect in the electrical and electronic industries.
実施例
合金原料を高周波溶解してＮｉ：７９質量％、Ｍｏ：１質量％を含有し、残部がＦｅおよび不可避不純物からなる成分組成の溶湯を作製し、これら溶湯を水アトマイズしてＦｅ−Ｎｉ−Ｍｏ系金属軟磁性アトマイズ粉末を作製し、そのＦｅ−Ｎｉ−Ｍｏ系金属軟磁性アトマイズ粉末を分級処理したのち、通常のアトライターにて扁平化処理し、得られた扁平粉末を風力分級機により分級することにより平均粒径ｄ：８２．９μｍ、平均厚さｔ：１．９６μｍ、アスペクト比（ｄ／ｔ）：４２．３を有するＦｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の原料粉末を作製した。
このようにして得られたＦｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の原料粉末を蒸留水中で表１に示される時間煮沸することにより本発明酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末（以下、本発明酸化膜被覆扁平軟磁性粉末という）１〜９および比較酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末（以下、比較酸化膜被覆扁平軟磁性粉末という）１を作製した。
さらに比較のために前記Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の原料粉末を大気中、温度：３７５℃で１時間あるいは６分間加熱することにより従来酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末（以下、従来酸化膜被覆扁平軟磁性粉末という）１〜２を作製した。
これら本発明酸化膜被覆扁平軟磁性粉末１〜９、比較酸化膜被覆扁平軟磁性粉末１および従来酸化膜被覆扁平軟磁性粉末１〜２についてその表面に形成されている酸化膜の成分組成およびその厚さを測定し、その結果を表１に示した。
Example An alloy raw material was melted at high frequency to prepare molten metal having a composition of Ni: 79% by mass and Mo: 1% by mass, the balance being Fe and inevitable impurities, and the molten metal was atomized with water to obtain Fe-Ni. -Mo-based metal soft magnetic atomized powder was prepared, and the Fe-Ni-Mo-based metal soft magnetic atomized powder was classified and then flattened with a normal attritor. The raw material powder of the Fe—Ni—Mo flat metal soft magnetic powder having an average particle diameter d: 82.9 μm, an average thickness t: 1.96 μm, and an aspect ratio (d / t): 42.3 Was made.
The raw material powder of the Fe—Ni—Mo-based flat metal soft magnetic powder thus obtained is boiled in distilled water for the time shown in Table 1 so that the oxide film-coated Fe—Ni—Mo-based flat metal soft magnetic powder of the present invention is obtained. Preparation of powders (hereinafter referred to as oxide-coated flat soft magnetic powders according to the present invention) 1 to 9 and comparative oxide-coated Fe-Ni-Mo-based flat metal soft magnetic powders (hereinafter referred to as comparative oxide-coated flat soft magnetic powders) 1 did.
Further, for comparison, the raw material powder of the Fe—Ni—Mo based flat metal soft magnetic powder is heated in the atmosphere at a temperature of 375 ° C. for 1 hour or 6 minutes, thereby forming a conventional oxide-coated Fe—Ni—Mo based flat metal. Soft magnetic powders (hereinafter referred to as conventional oxide film-coated flat soft magnetic powders) 1 and 2 were produced.
These oxide film-coated flat soft magnetic powders 1 to 9 of the present invention, comparative oxide film-coated flat soft magnetic powder 1 and conventional oxide film-coated flat soft magnetic powders 1 and 2, and component compositions of oxide films formed on the surfaces thereof and The thickness was measured and the results are shown in Table 1.
これら本発明酸化膜被覆扁平軟磁性粉末１〜９、比較酸化膜被覆扁平軟磁性粉末１および従来酸化膜被覆扁平軟磁性粉末１〜２について粉体抵抗率および保磁力を測定し、その結果を表１に示した。
その後、さらに本発明酸化膜被覆扁平軟磁性粉末１〜９、比較酸化膜被覆扁平軟磁性粉末１および従来酸化膜被覆扁平軟磁性粉末１〜２についてＪＩＳ Ｚ ８８３０で規定される気体吸着法により比表面積ＳＲを測定し、その結果を表１に示した。
さらに、平均粒径ｄ：８２．９μｍ、平均厚さｔ：１．９６μｍ、アスペクト比（ｄ／ｔ）：４２．３を有する表面に凹凸のない平滑な表面を有する仮想のＦｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の比表面積ＳＩを計算で求めると、ＳＩ＝０．１２３９８ｍ２／ｇとなるから、ＳＲ／ＳＩ＝ｋからｋの値を計算により求め、その結果を表１に示した。
The powder resistivity and coercivity of these oxide film-coated flat soft magnetic powders 1 to 9, comparative oxide film-coated flat soft magnetic powder 1 and conventional oxide film-coated flat soft magnetic powders 1 and 2 were measured, and the results were obtained. It is shown in Table 1.
Thereafter, the oxide film-coated flat soft magnetic powders 1 to 9, the comparative oxide film-coated flat soft magnetic powder 1 and the conventional oxide film-coated flat soft magnetic powders 1 to 2 of the present invention were compared by the gas adsorption method defined in JIS Z 8830. The surface area SR was measured, and the results are shown in Table 1.
Furthermore, the virtual Fe-Ni-Mo which has a smooth surface without unevenness on the surface having an average particle diameter d: 82.9 μm, an average thickness t: 1.96 μm, and an aspect ratio (d / t): 42.3 When the specific surface area SI of the system flat metal soft magnetic powder was calculated, SI = 0.12398 m2 / g. Therefore, the value of k was calculated from SR / SI = k, and the results are shown in Table 1.
この本発明酸化膜被覆扁平軟磁性粉末１〜９、比較酸化膜被覆扁平軟磁性粉末１および従来酸化膜被覆扁平軟磁性粉末１〜２に塩素化ポリエチレン：１５質量％を混合し混練したのち、ロール成形することにより酸化膜被覆扁平金属軟磁性粉末の扁平面がシート面に平行に配列した厚み：０．５ｍｍを有する本発明磁性複合シート１〜９、比較磁性複合シート１および従来磁性複合シート１〜２を作製し、これら磁性複合シートの抵抗率および保磁力を測定し、その結果を表２に示した。 The present oxide film-coated flat soft magnetic powders 1 to 9, comparative oxide film-coated flat soft magnetic powder 1 and conventional oxide film-coated flat soft magnetic powders 1 to 2 were mixed and kneaded with 15% by mass of chlorinated polyethylene, The present invention magnetic composite sheets 1 to 9, the comparative magnetic composite sheet 1 and the conventional magnetic composite sheet having a thickness of 0.5 mm in which the flat surfaces of the oxide film-coated flat metal soft magnetic powder are arranged in parallel to the sheet surface by roll forming 1-2 were prepared, and the resistivity and coercive force of these magnetic composite sheets were measured. The results are shown in Table 2.
表１〜２に示される結果から、Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末を蒸留水中で煮沸して得られた比例係数ｋが１０〜２００の範囲内にある本発明酸化膜被覆扁平軟磁性粉末１〜９はいずれも従来酸化膜被覆扁平軟磁性粉末２よりも高抵抗率を有しかつ高比表面積および高比例係数ｋを有する。また、本発明酸化膜被覆扁平軟磁性粉末１〜９はいずれも従来酸化膜被覆扁平軟磁性粉末１と抵抗率が同程度であるが、保磁力が低いことが分かる。
本発明酸化膜被覆扁平軟磁性粉末１〜９で作製した本発明磁性複合シート１〜９は、従来酸化膜被覆扁平軟磁性粉末２で作製した従来磁性複合シート２に比べて高抵抗率を有する。また、本発明酸化膜被覆扁平軟磁性粉末１〜９で作製した本発明磁性複合シート１〜９は、いずれも従来酸化膜被覆扁平軟磁性粉末１で作製した従来磁性複合シート１に比べて抵抗率が同程度であるが、保磁力が低いことが分かる。
しかし、この発明の条件から外れた比例係数ｋを有する比較酸化物被覆扁平軟磁性粉末１で作製した比較磁性複合シート１は保磁力が低いが抵抗率も１０３Ωｃｍ未満と低いことが分かる。
From the results shown in Tables 1 and 2, the present invention oxide-coated flat soft having a proportionality coefficient k within the range of 10 to 200 obtained by boiling Fe-Ni-Mo-based flat metal soft magnetic powder in distilled water. Each of the magnetic powders 1 to 9 has a higher resistivity than the conventional oxide film-coated flat soft magnetic powder 2 and has a high specific surface area and a high proportionality coefficient k. Further, it can be seen that the oxide film-coated flat soft magnetic powders 1 to 9 of the present invention all have the same resistivity as the conventional oxide film-coated flat soft magnetic powder 1 but have a low coercive force.
The magnetic composite sheets 1 to 9 of the present invention prepared with the oxide film-coated flat soft magnetic powders 1 to 9 of the present invention have higher resistivity than the conventional magnetic composite sheet 2 of the conventional oxide film-coated flat soft magnetic powder 2. . Also, the magnetic composite sheets 1 to 9 of the present invention prepared with the oxide film-coated flat soft magnetic powders 1 to 9 of the present invention are more resistant than the conventional magnetic composite sheet 1 of the conventional oxide film-coated flat soft magnetic powder 1. It can be seen that the rate is similar, but the coercivity is low.
However, it can be seen that the comparative magnetic composite sheet 1 made of the comparative oxide-coated flat soft magnetic powder 1 having a proportionality coefficient k outside the conditions of the present invention has a low coercive force but a low resistivity of less than 10 3 Ωcm.
Claims (7)
前記高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の比表面積をＳＲ、
表面に凹凸のない平滑な表面を有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末の計算で求めた比表面積をＳＩとすると、
前記ＳＲとＳＩとが、ＳＲ＝ｋ・ＳＩ（ただし、ｋは表面粗さを表現する比例係数であって、ｋ＝１０〜２００）の関係を満たす範囲内の比表面積を有することを特徴とする高表面粗さを有する酸化膜被覆Ｆｅ−Ｎｉ−Ｍｏ系扁平金属軟磁性粉末。 An oxide film-coated Fe—Ni—Mo-based flat metal soft magnetic powder having an average particle size of 30 to 150 μm and an aspect ratio (average particle size / average thickness) of 5 to 500, and having a high surface roughness,
The specific surface area of the oxide film-coated Fe—Ni—Mo based flat metal soft magnetic powder having high surface roughness is SR,
When the specific surface area obtained by calculation of the oxide film-coated Fe-Ni-Mo-based flat metal soft magnetic powder having a smooth surface without unevenness on the surface is defined as SI,
The SR and SI have a specific surface area within a range satisfying a relationship of SR = k · SI (where k is a proportional coefficient expressing surface roughness, k = 10 to 200). Oxide-coated Fe-Ni-Mo-based flat metal soft magnetic powder having high surface roughness.
The flat surface of the oxide film-coated Fe-Ni-Mo-based flat metal soft magnetic powder having a high surface roughness according to claim 1, 2, or 3 is oriented in a direction perpendicular to the thickness direction of the magnetic composite sheet. A magnetic composite sheet characterized by being dispersed.
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| JP2004369372A JP2006179576A (en) | 2004-12-21 | 2004-12-21 | OXIDE FILM-COVERED Fe-Ni-Mo FLAT METAL SOFT MAGNETIC POWDER AND ITS MANUFACTURING METHOD HAVING HIGH SURFACE FINISH. |
| PCT/JP2005/023359 WO2006068136A1 (en) | 2004-12-21 | 2005-12-20 | OXIDE FILM COATED Fe-Ni-Mo BASED FLAT METAL SOFT MAGNETIC POWDER HAVING HIGH SURFACE ROUGHNESS AND METHOD FOR PRODUCTION THEREOF |
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| JP2004369372A JP2006179576A (en) | 2004-12-21 | 2004-12-21 | OXIDE FILM-COVERED Fe-Ni-Mo FLAT METAL SOFT MAGNETIC POWDER AND ITS MANUFACTURING METHOD HAVING HIGH SURFACE FINISH. |
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| JPS5638402A (en) * | 1979-09-05 | 1981-04-13 | Tdk Corp | High density sintered magnetic body and its manufacture |
| WO2002008129A1 (en) * | 2000-07-26 | 2002-01-31 | Heraeus Tenevo Ag | Method for the vitrification of a porous soot body |
| KR20040015826A (en) * | 2001-08-09 | 2004-02-19 | 자이단호진 리코가쿠신코카이 | Composite magnetic material prepared by compression forming of ferrite-coated metal particles and method for preparation thereof |
| JP2003086415A (en) * | 2001-09-12 | 2003-03-20 | Aisin Seiki Co Ltd | Soft magnetic particle for motor of electromagnetic actuator, manufacturing method therefor, soft magnetic molded body for motor or electromagnetic actuator, and manufacturing method therefor |
| JP3795432B2 (en) * | 2002-06-28 | 2006-07-12 | Ｔｄｋ株式会社 | Method for manufacturing electromagnetic wave absorbing sheet |
| JP2003332114A (en) * | 2002-05-09 | 2003-11-21 | Mitsubishi Materials Corp | Bonded soft magnetic body with excellent mechanical strength and cavitation damage resistance at room temperature and high temperature and its fabricating method |
| JP4449077B2 (en) * | 2003-08-05 | 2010-04-14 | 三菱マテリアル株式会社 | Fe-Ni-Mo-based flat metal soft magnetic powder and magnetic composite material including the soft magnetic powder |
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| CN105436498A (en) * | 2015-11-18 | 2016-03-30 | 山东大学 | Porous nickel-carbon nano-composite microsphere electromagnetic wave absorbing material and preparation method and application thereof |
| CN105436498B (en) * | 2015-11-18 | 2017-12-01 | 山东大学 | A kind of porous nickel carbon composite nano-microsphere electromagnetic wave absorbent material and preparation method and application |
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