JP2007126696A - METHOD FOR MANUFACTURING IRON POWDER HAVING SURFACE COATED WITH HIGH-Si LAYER - Google Patents

METHOD FOR MANUFACTURING IRON POWDER HAVING SURFACE COATED WITH HIGH-Si LAYER Download PDF

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JP2007126696A
JP2007126696A JP2005319248A JP2005319248A JP2007126696A JP 2007126696 A JP2007126696 A JP 2007126696A JP 2005319248 A JP2005319248 A JP 2005319248A JP 2005319248 A JP2005319248 A JP 2005319248A JP 2007126696 A JP2007126696 A JP 2007126696A
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JP4430607B2 (en
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Muneaki Watanabe
宗明 渡辺
Ryoji Nakayama
亮治 中山
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Diamet Corp
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Abstract

<P>PROBLEM TO BE SOLVED: To provide iron powder having a surface coated with high-Si layer in which a high-concentration Si diffusion layer is formed on the surface of iron powder and which is used for the production of various electromagnetic circuit components requiring high specific resistance. <P>SOLUTION: Iron powder is held at >900 to 1,250°C in a nonoxidizing atmosphere to undergo preliminary heat treatment, followed by pulverization. Then Si powder or ferrosilicon powder is added to the resultant pulverized iron powder and these are mixed. The resultant powder mixture is heated at 920 to 1,100°C in a hydrogen atmosphere to undergo heat treatment, followed by pulverization. By this method, the iron powder having a surface coated with high-Si layer can be manufactured. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

この発明は、鉄粉末の表面にＳｉの熱拡散層を有する表面高Ｓｉ層被覆鉄粉末およびその製造方法に関するものであり、この表面高Ｓｉ層被覆鉄粉末を用いて作製した軟磁性材は低鉄損を必要とする各種電磁気回路部品、例えば、モータ、アクチュエータ、ヨーク、コア、リアクトルなどの各種電磁気部品の素材として使用される。   The present invention relates to a surface high Si layer coated iron powder having a Si thermal diffusion layer on the surface of the iron powder and a method for producing the same, and a soft magnetic material produced using the surface high Si layer coated iron powder has a low It is used as a material for various electromagnetic circuit components that require iron loss, for example, various electromagnetic components such as motors, actuators, yokes, cores, and reactors.

一般に、各種電磁気回路部品に使用される軟磁性材は、鉄損が小さいことが要求されるため、電気抵抗を高くして渦電流損を低減させ、保磁力を小さくしてヒステリシス損を低減させることは知られている。さらに、近年、電磁気回路の小型化、高応答化が求められているところから、磁束密度がより高いことも重要視されている。   In general, soft magnetic materials used in various electromagnetic circuit components are required to have low iron loss. Therefore, electrical resistance is increased to reduce eddy current loss, and coercive force is reduced to reduce hysteresis loss. It is known. Furthermore, in recent years, since the miniaturization and high response of the electromagnetic circuit have been demanded, higher magnetic flux density is also regarded as important.

かかる高比抵抗を有する軟磁性材料を製造するための原料粉末の一例として鉄粉末の表面にＳｉを拡散させて鉄粉末の表面に鉄粉末に含まれるＳｉよりも高濃度のＳｉを含む高Ｓｉ濃度被覆層を形成した平均粒径：１〜２００μｍの表面高Ｓｉ層被覆鉄粉末が提供されており、この表面高Ｓｉ層被覆鉄粉末は、アトマイズ法により得られた鉄粉末を温度：５００〜９００℃、Ａｒ雰囲気中に保持する予備熱処理を施したのち、温度：８００〜９００℃、１０〜５０Ｖｏｌ％ＳｉＣｌ４＋Ａｒ雰囲気中に保持する浸珪処理を施し、さらに温度：５００〜９００℃、Ａｒ雰囲気中に保持する熱拡散処理を施すことにより製造することが知られている（特許文献１参照）。
特開平１１−８７１２３号公報 As an example of a raw material powder for producing such a soft magnetic material having a high specific resistance, Si is diffused on the surface of the iron powder, and the surface of the iron powder contains high Si containing a higher concentration of Si than Si contained in the iron powder. A surface high Si layer-coated iron powder having an average particle diameter of 1 to 200 μm formed with a concentration coating layer is provided. The surface high Si layer coated iron powder is obtained by converting the iron powder obtained by the atomization method to a temperature of 500 to After performing a pre-heat treatment to be held in an Ar atmosphere at 900 ° C., temperature: 800 to 900 ° C., a silicidation treatment to be held in an atmosphere of 10 to 50 Vol% SiCl 4 + Ar, and further to a temperature of 500 to 900 ° C., Ar It is known to manufacture by performing a thermal diffusion treatment held in an atmosphere (see Patent Document 1).
Japanese Patent Laid-Open No. 11-87123

しかし、前記従来の表面高Ｓｉ層被覆鉄粉末の製造方法は、ＳｉＣｌ４ガスを使用するために得られた表面高Ｓｉ層被覆鉄粉末には塩素が含まれており、この塩素を含んだ表面高Ｓｉ層被覆鉄粉末は腐食し易く、また、ＳｉＣｌ４ガス自体の取扱いが難しく、さらに前記従来の表面高Ｓｉ層被覆鉄粉末の製造方法により得られた表面高Ｓｉ層被覆鉄粉末の保磁力を十分に下げることができないなど軟磁性材料を製造するための原料粉末として満足な特性が得られなかった。 However, in the conventional method for producing a surface high Si layer-coated iron powder, the surface high Si layer-coated iron powder obtained by using SiCl 4 gas contains chlorine, and this surface containing chlorine The high Si layer-coated iron powder is easily corroded, and it is difficult to handle the SiCl 4 gas itself. Further, the coercive force of the surface high Si layer-coated iron powder obtained by the conventional method for producing a surface high Si layer-coated iron powder is as follows. As a raw material powder for producing a soft magnetic material, for example, it was not possible to sufficiently lower the temperature, satisfactory characteristics could not be obtained.

そこで、本発明者らは、ＳｉＣｌ４ガスなどの取扱いの難しい気体を使用することなく軟磁性材料を製造するための原料粉末として一層磁気特性に優れた表面高Ｓｉ層被覆鉄粉末を製造すべく研究を行った。
その結果、鉄粉末の予備熱処理を真空、水素、アルゴン等の非酸化雰囲気中で従来よりも高温の温度：９００越え〜１２５０℃で行ったのち粉砕すると、鉄粉末の結晶粒径が成長して結晶粒径の大きな鉄粉砕粉末が得られ、この結晶粒径の大きな鉄粉砕粉末にＳｉ粉末またはフェロシリコン粉末を添加し混合して得られた混合粉末を水素雰囲気中、温度：９２０〜１１００℃で加熱したのち粉砕すると、軟磁性材料を製造するための原料粉末として一層磁気特性に優れた表面高Ｓｉ層被覆鉄粉末が得られる、という研究結果が得られたのである。
この発明は、これら研究結果に基づいてなされたものであって、
（１）鉄粉末を非酸化雰囲気中で温度：９００越え〜１２５０℃に保持することにより予備熱処理したのち粉砕することにより鉄粉砕粉末を作製し、この鉄粉砕粉末にＳｉ粉末またはフェロシリコン粉末を添加し混合したのち水素雰囲気中、温度：９２０〜１１００℃で加熱する熱処理を施し、次いで粉砕する表面高Ｓｉ層被覆鉄粉末の製造方法、に特徴を有するものである。 Therefore, the inventors of the present invention are to manufacture a surface high Si layer-coated iron powder having a further excellent magnetic property as a raw material powder for producing a soft magnetic material without using a difficult gas such as SiCl 4 gas. I did research.
As a result, when the pre-heat treatment of the iron powder is performed in a non-oxidizing atmosphere such as vacuum, hydrogen, argon, etc. at a temperature higher than the conventional temperature: over 900 to 1250 ° C., the grain size of the iron powder grows. An iron pulverized powder having a large crystal grain size is obtained, and a mixed powder obtained by adding and mixing Si powder or ferrosilicon powder to the iron pulverized powder having a large crystal grain size is heated in a hydrogen atmosphere at a temperature of 920 to 1100 ° C. The result of the study was that the surface high Si layer-coated iron powder, which was further excellent in magnetic properties, was obtained as a raw material powder for producing a soft magnetic material when heated and ground.
This invention was made based on these research results,
(1) The iron powder is preheated by holding the iron powder in a non-oxidizing atmosphere at a temperature of over 900 to 1250 ° C. and then pulverized to produce an iron pulverized powder. The iron pulverized powder is mixed with Si powder or ferrosilicon powder. It is characterized by a method for producing a surface-high Si layer-coated iron powder that is added and mixed, then subjected to heat treatment at a temperature of 920 to 1100 ° C. in a hydrogen atmosphere, and then pulverized.

この発明の表面高Ｓｉ層被覆鉄粉末の製造方法で行う予備熱処理を９００越え〜１２５０℃で行うのは、鉄粉末を９００℃以下で予備熱処理を行っても予備熱処理中に結晶粒の十分な成長が成されず、結晶粒の微細な予備熱処理した粉末を使用して作製した表面高Ｓｉ層被覆鉄粉末は保磁力を下げることができないので好ましくなく、一方、１２５０℃を越える温度で予備熱処理すると、焼結が進みすぎてその後の粉砕が困難になり、粉砕できたとしても困難な粉砕により歪残留量が多くなって結晶粒が再び微細化し、得られた表面高Ｓｉ層被覆鉄粉末の磁気特性が所望の値にならなくなるので好ましくない、という理由によるものである。   The preliminary heat treatment performed in the method for producing the surface high Si layer-coated iron powder of the present invention is performed at a temperature exceeding 900 to 1250 ° C., even if the iron powder is subjected to the preliminary heat treatment at 900 ° C. or less, sufficient crystal grains are obtained during the preliminary heat treatment. The surface high Si layer coated iron powder produced by using the preheat-treated powder with no crystal growth and fine grain is not preferable because the coercive force cannot be lowered, while preheat treatment at a temperature exceeding 1250 ° C. Then, the sintering progressed too much and subsequent pulverization became difficult. Even if pulverization was possible, the residual amount of strain increased due to difficult pulverization, and the crystal grains were refined again. This is because the magnetic characteristics are not desirable because they are not desired.

また、この発明の表面高Ｓｉ層被覆鉄粉末の製造方法で行う熱処理を水素雰囲気中で９２０〜１１００℃で行う理由は、非酸化雰囲気中の内でも水素雰囲気で熱処理することにより最も短時間で効率よく鉄粉砕粉末の表面に高濃度のＳｉ拡散層を形成することができるからであり、その温度が９２０℃未満では通常の遅い拡散速度しか得られないので好ましくなく、一方、１１００℃を越えた温度で熱処理すると、鉄粉砕粉末の焼結が進行し過ぎて粉砕が困難になり、粉砕することができたとしても鉄粉末の表面に高Ｓｉ濃度被覆層を有する表面高Ｓｉ層被覆鉄粉末が得られなくなるので好ましくないことによるものである。   The reason why the heat treatment performed in the method for producing the surface high Si layer-coated iron powder of the present invention is performed at 920 to 1100 ° C. in a hydrogen atmosphere is the shortest in the non-oxidizing atmosphere by performing the heat treatment in the hydrogen atmosphere. This is because a high-concentration Si diffusion layer can be efficiently formed on the surface of the iron pulverized powder. If the temperature is less than 920 ° C., it is not preferable because only a normal slow diffusion rate can be obtained, while exceeding 1100 ° C. When the heat treatment is performed at a high temperature, sintering of the iron pulverized powder proceeds excessively, making pulverization difficult, and even if pulverized, the surface has a high Si concentration coating layer on the surface of the iron powder. This is because it is not preferable since the above cannot be obtained.

この発明の表面高Ｓｉ層被覆鉄粉末の製造方法で使用する鉄粉末は、純鉄粉末が好ましいが、純度：９８．５質量％以上あれば十分であり、炭素鋼粉末なども使用することが出来る。そして前記鉄粉末の粒径は特に限定されるものではないが、平均粒径:５０〜１５０μｍの範囲内にあることが好ましい。したがって、この発明は、
（２）前記鉄粉末は、純度：９８．５質量％以上の鉄粉末である前記（１）記載の表面高Ｓｉ層被覆鉄粉末の製造方法、に特長を有するものである。
この発明の表面高Ｓｉ層被覆鉄粉末の製造方法で使用する鉄粉末に添加し混合するＳｉ粉末またはフェロシリコン（Ｓｉ：５０％以上含有のフェロシリコン）粉末は粒径：１０μｍ以下の微細粉末であることが好ましい。その理由は、Ｓｉ粉末またはフェロシリコン粉末の粒径が１０μｍを越えるようになると、原料粉末の鉄粉末に比べて大きく、混合時に鉄粉末の周囲に不均一に分散しなくなるので高Ｓｉ層被覆層が鉄粉末の表面に均一な厚さで被覆しなくなるので好ましくないからである。したがって、この発明は、
（３）前記Ｓｉ粉末またはフェロシリコン粉末は、粒径：１０μｍ以下の微細粉末である前記（１）記載の表面高Ｓｉ層被覆鉄粉末の製造方法、に特長を有するものである。 The iron powder used in the method for producing the surface high Si layer-coated iron powder of the present invention is preferably pure iron powder, but it is sufficient if the purity is 98.5% by mass or more, and carbon steel powder or the like may be used. I can do it. The particle size of the iron powder is not particularly limited, but it is preferable that the average particle size is in the range of 50 to 150 μm. Therefore, the present invention
(2) The iron powder has a feature in the method for producing a surface high Si layer-coated iron powder according to (1), which is an iron powder having a purity of 98.5% by mass or more.
The Si powder or ferrosilicon (Si: ferrosilicon containing 50% or more) powder added to and mixed with the iron powder used in the method for producing the surface high Si layer-coated iron powder of the present invention is a fine powder having a particle size of 10 μm or less. Preferably there is. The reason is that when the particle size of the Si powder or ferrosilicon powder exceeds 10 μm, it is larger than the iron powder of the raw material powder and does not disperse unevenly around the iron powder during mixing. Is not preferable because the surface of the iron powder is not coated with a uniform thickness. Therefore, the present invention
(3) The Si powder or ferrosilicon powder has a feature in the method for producing a surface high Si layer-coated iron powder according to (1), which is a fine powder having a particle size of 10 μm or less.

この発明の表面高Ｓｉ層被覆鉄粉末にバインダーとしての有機絶縁材料や無機絶縁材料、あるいは有機絶縁材料と無機絶縁材料との混合材料を混合して比抵抗および強度のさらに向上した軟磁性材を作製することができる。この場合、有機絶縁材料では、エポキシ樹脂、フッ素樹脂、フェノール樹脂、ウレタン樹脂、シリコーン樹脂、ポリエステル樹脂、フェノキシ樹脂、ユリア樹脂、イソシアネート樹脂、アクリル樹脂、ポリイミド樹脂、ＰＰＳ樹脂，等を用いることができる。また無機絶縁材料では、リン酸鉄などのリン酸塩、各種ガラス状絶縁物、珪酸ソーダを主成分とする水ガラス、絶縁性酸化物、等を用いることができる。そして、表面高Ｓｉ層被覆鉄粉末に添加するバインダー量は０．２〜３質量％の範囲内にあることが好ましい。この添加量は一般に知られている範囲内である。
この発明の表面高Ｓｉ層被覆鉄粉末に前記バインダーを添加し混合した混合粉末を圧粉成形し、得られた圧粉成形体を温度：５００〜９００℃で燒結することにより軟磁性材を作製することができる。この焼結温度は一般に知られている温度である。
この発明の表面高Ｓｉ層被覆鉄粉末を用いて作製した軟磁性材は高密度、高強度、高比抵抗、高磁束密度および低保磁力を有し、この軟磁性材は、高磁束密度で高周波低鉄損の特徴を有する事からこの特徴を生かした各種電磁気回路部品の材料として使用できる。前記電磁気回路部品は、磁心、電動機コア，発電機コア、ソレノイドコア、イグニッションコア、リアクトル、トランス、チョークコイルコアまたは磁気センサコアなどがある。そして、この発明の酸化膜被覆Ｆｅ−Ｓｉ系鉄基軟磁性粉末を用いた軟磁性材からなる電磁気回路部品を組み込んだ電気機器には、電動機、発電機、ソレノイド、インジェクタ、電磁駆動弁、インバータ、コンバータ、変圧器、継電器、磁気センサシステム等があり、電気機器の高効率高性能化や小型軽量化を行うことができる。 A soft magnetic material having further improved specific resistance and strength by mixing an organic insulating material or inorganic insulating material as a binder or a mixed material of an organic insulating material and an inorganic insulating material with the surface high Si layer-coated iron powder of the present invention. Can be produced. In this case, as the organic insulating material, epoxy resin, fluorine resin, phenol resin, urethane resin, silicone resin, polyester resin, phenoxy resin, urea resin, isocyanate resin, acrylic resin, polyimide resin, PPS resin, or the like can be used. . As the inorganic insulating material, phosphates such as iron phosphate, various glassy insulators, water glass mainly composed of sodium silicate, insulating oxides, and the like can be used. And it is preferable that the amount of binders added to surface high Si layer coating iron powder exists in the range of 0.2-3 mass%. The amount added is within a generally known range.
The mixed powder obtained by adding and mixing the binder to the surface high Si layer-coated iron powder of this invention is compacted, and the resulting compacted body is sintered at a temperature of 500 to 900 ° C. to produce a soft magnetic material. can do. This sintering temperature is a generally known temperature.
The soft magnetic material produced using the surface high Si layer coated iron powder of the present invention has high density, high strength, high specific resistance, high magnetic flux density and low coercive force, and this soft magnetic material has high magnetic flux density. Since it has the characteristics of high-frequency and low iron loss, it can be used as a material for various electromagnetic circuit components utilizing this characteristic. Examples of the electromagnetic circuit component include a magnetic core, a motor core, a generator core, a solenoid core, an ignition core, a reactor, a transformer, a choke coil core, and a magnetic sensor core. In addition, an electric device incorporating an electromagnetic circuit component made of a soft magnetic material using the oxide film-coated Fe-Si iron-based soft magnetic powder of the present invention includes an electric motor, a generator, a solenoid, an injector, an electromagnetically driven valve, an inverter There are converters, transformers, relays, magnetic sensor systems, etc., which can improve the efficiency, performance, size and weight of electrical equipment.

この発明の表面高Ｓｉ層被覆鉄粉末を使用して軟磁性材を製造すると、高比抵抗を有することから低渦電流損失を有し、さらに保磁力が低いことから低ヒステリシス損失を有する軟磁性材を低コスト安定して作製することができ、電気・電子産業上優れた効果をもたらすものである。   When a soft magnetic material is manufactured using the surface high Si layer coated iron powder of this invention, it has a low specific eddy current loss due to its high specific resistance, and also has a low hysteresis loss due to its low coercive force. The material can be produced stably at a low cost, and has an excellent effect in the electric and electronic industries.

原料粉末としてアトマイズして得られた平均粒径：８０μｍを有する純鉄粉末およびアトマイズして得られた平均粒径：８０μｍを有する炭素鋼粉末（成分組成、質量％で、Ｃ：０．０１％、Ｓｉ：０．１％、Ｍｎ：０．３５％、Ｐ：０．０１％、Ｓ：０．０２％を含有し、残部がＦｅおよび不可避不純物）を用意し、さらに平均粒径：５μｍを有するＳｉ粉末、平均粒径：５μｍを有しＳｉ：７５％を含有する市販のフェロシリコン粉末を用意した。
実施例１
まず、純鉄粉末を真空、水素、アルゴン雰囲気中、表１に示される条件で予備熱処理したのち粉砕して純鉄粉砕粉末を作製し、これら純鉄粉砕粉末に純Ｓｉ粉末を、純鉄粉砕粉末：純Ｓｉ粉末＝９７質量％：３％質量となるように配合し、混合して混合粉末を作製し、得られた混合粉末を表１に示される条件で熱処理したのち粉砕する本発明法１〜８および比較法１〜５を実施することにより純鉄粉末の表面に高濃度Ｓｉ拡散層が形成された粒径：１５０以下の表面高Ｓｉ層被覆鉄粉末を作製した。 Pure iron powder having an average particle size of 80 μm obtained by atomization as a raw material powder and carbon steel powder having an average particle size of 80 μm obtained by atomization (component composition, mass%, C: 0.01% Si: 0.1%, Mn: 0.35%, P: 0.01%, S: 0.02%, the balance being Fe and inevitable impurities), and an average particle size of 5 μm A commercially available ferrosilicon powder having an Si powder having an average particle size of 5 μm and containing Si: 75% was prepared.
Example 1
First, pure iron powder is preheated in a vacuum, hydrogen, and argon atmosphere under the conditions shown in Table 1, and then pulverized to produce pure iron pulverized powder. Pure iron powder is then pulverized with pure Si powder. Powder: Pure Si powder = 97% by mass: 3% by mass, mixed to prepare a mixed powder, and the obtained mixed powder is heat-treated under the conditions shown in Table 1 and then pulverized. By carrying out 1 to 8 and Comparative Methods 1 to 5, the surface high Si layer-coated iron powder having a particle size of 150 or less with a high-concentration Si diffusion layer formed on the surface of the pure iron powder was produced.

本発明法１〜８および比較法１〜５で得られた表面高Ｓｉ層被覆鉄粉末にシランカップリング処理を施したのちバインダーとしてシリコーン樹脂：１．５質量％を添加し混合したのち金型に入れ、プレス成形して縦：５５ｍｍ、横：１０ｍｍ、厚さ：５ｍｍの寸法を有する板状圧粉体および外径：３５ｍｍ、内径：２５ｍｍ、高さ：５ｍｍの寸法を有するリング形状圧粉体を成形し、得られた圧粉体を真空雰囲気中、温度：８００℃、３０分保持の条件で焼成を行い、板状およびリング状焼成体からなる軟磁性材を作製し、この板状焼成体からなる軟磁性材の比抵抗を測定してその結果を表２に示し、さらにリング状焼成体からなる軟磁性材に巻き線を施し、磁束密度、保磁力、並びに磁束密度１Ｔ、周波数１ｋＨｚの時の鉄損および磁束密度０．１Ｔ、周波数１０ｋＨｚの時の鉄損などの磁気特性を測定し、それらの結果を表２に示した。
従来例１
先に用意した純鉄粉末を真空、水素、Ａｒ雰囲気中、温度:８００℃、０．５時間保持の予備熱処理をおこなったのち、温度:８００℃、１５Ｖｏｌ．％ＳｉＣｌ４＋Ａｒ雰囲気中、０．５時間保持の浸珪処理を施し、さらにＡｒ雰囲気中、温度:８００℃、０．５時間保持することにより従来法１を実施することにより純鉄粉末の表面に高濃度Ｓｉ拡散層が形成された表面高Ｓｉ層被覆鉄粉末を作製した。 After applying silane coupling treatment to the surface high Si layer-coated iron powder obtained by the present invention methods 1-8 and comparative methods 1-5, a silicone resin: 1.5% by mass is added as a binder, and then mixed. And pressed into a plate-shaped green compact having a length of 55 mm, a width of 10 mm, and a thickness of 5 mm, and a ring-shaped powder having an outer diameter of 35 mm, an inner diameter of 25 mm, and a height of 5 mm. The body was molded, and the obtained green compact was fired in a vacuum atmosphere at a temperature of 800 ° C. and held for 30 minutes to produce a soft magnetic material composed of a plate-like and ring-like fired body. The specific resistance of the soft magnetic material made of the fired body was measured and the results are shown in Table 2. Further, the soft magnetic material made of the ring-like fired body was wound, and the magnetic flux density, coercive force, magnetic flux density 1T, frequency Iron loss and magnetic flux density at 1 kHz 0.1 T, the magnetic properties such as iron loss at a frequency 10kHz were measured. The results are shown in Table 2.
Conventional Example 1
The pre-prepared pure iron powder was preliminarily heat-treated in a vacuum, hydrogen and Ar atmosphere at a temperature of 800 ° C. for 0.5 hours, and then the temperature was 800 ° C. and 15 Vol. The surface of the pure iron powder is obtained by performing the conventional method 1 by performing a siliconizing treatment for 0.5 hours in an atmosphere of% SiCl 4 + Ar, and further maintaining in an Ar atmosphere at a temperature of 800 ° C. for 0.5 hours. The surface high Si layer coating iron powder in which the high concentration Si diffusion layer was formed was prepared.

得られた表面高Ｓｉ層被覆鉄粉末にシランカップリング処理を施したのちバインダーとしてシリコーン樹脂：１．５質量％を添加し混合したのち金型に入れ、プレス成形して縦：５５ｍｍ、横：１０ｍｍ、厚さ：５ｍｍの寸法を有する板状圧粉体および外径：３５ｍｍ、内径：２５ｍｍ、高さ：５ｍｍの寸法を有するリング形状圧粉体を成形し、得られた圧粉体を窒素雰囲気中、温度：５００℃、３０分保持の条件で焼成を行い、板状およびリング状焼成体からなる軟磁性材を作製し、この板状焼成体からなる軟磁性材の比抵抗を測定してその結果を表２に示し、さらにリング状焼成体からなる軟磁性材に巻き線を施し、磁束密度、保磁力、並びに磁束密度１Ｔ、周波数１ｋＨｚの時の鉄損および磁束密度０．１Ｔ、周波数１ｋＨｚの時の鉄損などの磁気特性を測定し、それらの結果を表２に示した。   The obtained surface high Si layer-coated iron powder is subjected to a silane coupling treatment, and then added and mixed with a silicone resin: 1.5% by mass as a binder, and then put into a mold, press-molded, and length: 55 mm, width: A plate-shaped green compact having dimensions of 10 mm, thickness: 5 mm, and a ring-shaped green compact having dimensions of outer diameter: 35 mm, inner diameter: 25 mm, height: 5 mm, and forming the green compact into nitrogen Firing is performed in an atmosphere at a temperature of 500 ° C. for 30 minutes to produce a soft magnetic material made of a plate-like and ring-like fired body, and the specific resistance of the soft magnetic material made of the plate-like fired body is measured. The results are shown in Table 2, and a soft magnetic material made of a ring-shaped fired body is wound, and magnetic flux density, coercive force, magnetic flux density 1T, iron loss and magnetic flux density 0.1T at a frequency of 1 kHz, Iron at a frequency of 1 kHz The magnetic characteristics such as measured, The results are shown in Table 2.

Figure 2007126696
Figure 2007126696

Figure 2007126696
Figure 2007126696

表１〜２に示される結果から、実施例１の本発明法１〜８で作製した表面高Ｓｉ層被覆鉄粉末を用いた軟磁性材は、従来例１の従来法１で作製した表面高Ｓｉ層被覆鉄粉末を用いた軟磁性材と比べて、密度については大差は無いが、実施例１の本発明法１〜８で作製した表面高Ｓｉ層被覆鉄粉末を用いた軟磁性材は、従来例１の従来法１で作製した表面高Ｓｉ層被覆鉄粉末を用いた軟磁性材に比べて、磁束密度が高く、保磁力が小さく、さらに比抵抗が高く、そのため鉄損、特に１ｋＨｚ以上の高周波域での鉄損が小さくなるなどの特性を有することが分かる。しかし、この発明の条件から外れた条件の比較法１〜５で作製した表面高Ｓｉ層被覆鉄粉末を用いた軟磁性材は一部好ましくない特性があることが分かる。
実施例２
次に、先に用意した炭素鋼粉末を真空、水素、アルゴン雰囲気中、表３に示される条件で予備熱処理したのち粉砕して炭素鋼粉砕粉末を作製し、これら炭素鋼粉砕粉末に先に用意したフェロシリコン粉末を、炭素鋼粉砕粉末：フェロシリコン粉末＝９８質量％：２％質量となるように配合し、混合して混合粉末を作製し、得られた混合粉末を表３に示される条件で熱処理したのち粉砕する本発明法９〜１６および比較法６〜１０を実施することにより炭素鋼粉末の表面に高濃度Ｓｉ拡散層が形成された表面高Ｓｉ層被覆鉄粉末を作製した。 From the results shown in Tables 1 and 2, the soft magnetic material using the surface-high Si layer-coated iron powder produced in the inventive methods 1 to 8 of Example 1 is the surface height produced in the conventional method 1 of Conventional Example 1. Compared with the soft magnetic material using the Si layer-coated iron powder, there is no significant difference in density, but the soft magnetic material using the surface high Si layer-coated iron powder produced by the inventive methods 1 to 8 of Example 1 is Compared with the soft magnetic material using the surface high Si layer-coated iron powder produced by the conventional method 1 of the conventional example 1, the magnetic flux density is high, the coercive force is small, and the specific resistance is high, so that the iron loss, particularly 1 kHz. It turns out that it has the characteristic that the iron loss in the above high frequency region becomes small. However, it can be seen that the soft magnetic material using the surface high Si layer-coated iron powder produced by Comparative Methods 1 to 5 under conditions deviating from the conditions of the present invention has some undesirable characteristics.
Example 2
Next, the prepared carbon steel powder is preheated in a vacuum, hydrogen, argon atmosphere under the conditions shown in Table 3 and then pulverized to produce a pulverized carbon steel powder. The obtained ferrosilicon powder was blended so that the pulverized carbon steel powder: ferrosilicon powder = 98% by mass: 2% by mass and mixed to prepare a mixed powder. The obtained mixed powder was subjected to the conditions shown in Table 3. By carrying out the present invention methods 9 to 16 and comparative methods 6 to 10 which were heat-treated and then ground, a high-Si surface-coated iron powder having a high-concentration Si diffusion layer formed on the surface of the carbon steel powder was produced.

本発明法９〜１６および比較法６〜１０で得られた表面高Ｓｉ層被覆鉄粉末にシランカップリング処理を施したのちバインダーとしてシリコーン樹脂：１．５質量％を添加し混合したのち金型に入れ、プレス成形して縦：５５ｍｍ、横：１０ｍｍ、厚さ：５ｍｍの寸法を有する板状圧粉体および外径：３５ｍｍ、内径：２５ｍｍ、高さ：５ｍｍの寸法を有するリング形状圧粉体を成形し、得られた圧粉体を窒素雰囲気中、温度：５００℃、３０分保持の条件で焼成を行い、板状およびリング状焼成体からなる軟磁性材を作製し、この板状焼成体からなる軟磁性材の比抵抗を測定してその結果を表４に示し、さらにリング状焼成体からなる軟磁性材に巻き線を施し、磁束密度、保磁力、並びに磁束密度１Ｔ、周波数１ｋＨｚの時の鉄損および磁束密度０．１Ｔ、周波数１０ｋＨｚの時の鉄損などの磁気特性を測定し、それらの結果を表４に示した。
従来例２
先に用意した炭素鋼粉末をＡｒ雰囲気中、温度:８００℃、０．５時間保持の予備熱処理をおこなったのち、温度:８００℃、１５Ｖｏｌ．％ＳｉＣｌ４＋Ａｒ雰囲気中、０．５時間保持の浸珪処理を施し、さらにＡｒ雰囲気中、温度:８００℃、０．５時間保持することにより従来法２を実施することにより炭素鋼粉末の表面に高濃度Ｓｉ拡散層が形成された表面高Ｓｉ層被覆鉄粉末を作製した。 After applying silane coupling treatment to the surface high Si layer-coated iron powder obtained by the present invention methods 9 to 16 and comparative methods 6 to 10, a silicone resin: 1.5% by mass is added as a binder, and then mixed. And pressed into a plate-shaped green compact having a length of 55 mm, a width of 10 mm, and a thickness of 5 mm, and a ring-shaped powder having an outer diameter of 35 mm, an inner diameter of 25 mm, and a height of 5 mm. The body was molded, and the obtained green compact was fired in a nitrogen atmosphere at a temperature of 500 ° C. for 30 minutes to produce a soft magnetic material comprising a plate-like and ring-like fired body. The specific resistance of the soft magnetic material made of the fired body was measured and the results are shown in Table 4. Further, the soft magnetic material made of the ring-like fired body was wound, and the magnetic flux density, coercive force, magnetic flux density 1T, frequency Iron loss and magnetism at 1 kHz Density 0.1 T, the magnetic properties such as iron loss at a frequency 10kHz were measured. The results are shown in Table 4.
Conventional example 2
The previously prepared carbon steel powder was pre-heated in an Ar atmosphere at a temperature of 800 ° C. and held for 0.5 hours, and then the temperature was 800 ° C. and 15 Vol. The surface of the carbon steel powder is obtained by performing the conventional method 2 by performing a siliconization treatment for 0.5 hours in a% SiCl 4 + Ar atmosphere, and further maintaining the temperature in the Ar atmosphere at 800 ° C. for 0.5 hours. The surface high Si layer coating iron powder in which the high concentration Si diffusion layer was formed was prepared.

得られた表面高Ｓｉ層被覆鉄粉末にバインダーとしてエポキシ樹脂：１質量％を添加し混合したのち金型に入れ、プレス成形して縦：５５ｍｍ、横：１０ｍｍ、厚さ：５ｍｍの寸法を有する板状圧粉体および外径：３５ｍｍ、内径：２５ｍｍ、高さ：５ｍｍの寸法を有するリング形状圧粉体を成形し、得られた圧粉体を窒素雰囲気中、温度：５００℃、３０分保持の条件で焼成を行い、板状およびリング状焼成体からなる軟磁性材を作製し、この板状焼成体からなる軟磁性材の比抵抗を測定してその結果を表４に示し、さらにリング状焼成体からなる軟磁性材に巻き線を施し、磁束密度、保磁力、並びに磁束密度１Ｔ、周波数１０ｋＨｚの時の鉄損および磁束密度０．１Ｔ、周波数１０ｋＨｚの時の鉄損などの磁気特性を測定し、それらの結果を表４に示した。   Epoxy resin as a binder is added to the obtained surface high Si layer-coated iron powder, mixed in 1% by mass, put into a mold, and press-molded to have dimensions of 55 mm in length, 10 mm in width, and 5 mm in thickness. A plate-shaped green compact and a ring-shaped green compact having dimensions of an outer diameter of 35 mm, an inner diameter of 25 mm, and a height of 5 mm were formed, and the obtained green compact was placed in a nitrogen atmosphere at a temperature of 500 ° C. for 30 minutes. Firing is performed under the holding conditions to produce a soft magnetic material made of a plate-like and ring-like fired body, the specific resistance of the soft magnetic material made of this plate-like fired body is measured, and the results are shown in Table 4, Winding is applied to a soft magnetic material made of a ring-shaped fired body, and magnetic flux density, coercive force, and magnetic loss such as iron loss at a magnetic flux density of 1T and a magnetic flux density of 0.1T and a magnetic flux density of 0.1T and a frequency of 10 kHz. Measure the properties and It is shown in Table 4.

Figure 2007126696
Figure 2007126696

Figure 2007126696
Figure 2007126696

表３〜４に示される結果から、実施例２の本発明法９〜１６で作製した表面高Ｓｉ層被覆鉄粉末を用いた軟磁性材は、従来例２の従来法２で作製した表面高Ｓｉ層被覆鉄粉末を用いた軟磁性材と比べて、密度については大差は無いが、実施例２の本発明法９〜１６で作製した表面高Ｓｉ層被覆鉄粉末を用いた軟磁性材は、従来例２の従来法２で作製した表面高Ｓｉ層被覆鉄粉末を用いた軟磁性材に比べて、磁束密度が高く、保磁力が小さく、さらに比抵抗が高く、そのため鉄損、特に１ｋＨｚ以上の高周波域での鉄損がが小さくなるなどの特性を有することが分かる。しかし、この発明の条件から外れた条件の比較法６〜１０で作製した表面高Ｓｉ層被覆鉄粉末を用いた軟磁性材は一部好ましくない特性があることが分かる。
From the results shown in Tables 3 to 4, the soft magnetic material using the surface high Si layer-coated iron powder produced by the inventive methods 9 to 16 of Example 2 is the surface height produced by the conventional method 2 of Conventional Example 2. Compared with the soft magnetic material using the Si layer-coated iron powder, the density is not much different, but the soft magnetic material using the surface high Si layer-coated iron powder produced by the inventive methods 9 to 16 of Example 2 is Compared with the soft magnetic material using the surface high Si layer-coated iron powder prepared by the conventional method 2 of the conventional example 2, the magnetic flux density is high, the coercive force is small, and the specific resistance is high, so that the iron loss, particularly 1 kHz. It turns out that it has the characteristic that the iron loss in the above high frequency region becomes small. However, it can be seen that the soft magnetic material using the surface high Si layer-coated iron powder produced by Comparative Methods 6 to 10 under conditions other than the conditions of the present invention has some undesirable characteristics.

Claims (8)

鉄粉末を非酸化雰囲気中で温度：９００越え〜１２５０℃に保持することにより予備熱処理したのち粉砕することにより鉄粉砕粉末を作製し、この鉄粉砕粉末にＳｉ粉末またはフェロシリコン粉末を添加し混合したのち水素雰囲気中、温度：９２０〜１１００℃で加熱し、次いで粉砕することを特徴とする表面高Ｓｉ層被覆鉄粉末の製造方法。 The iron powder is preheated by holding the iron powder in a non-oxidizing atmosphere at a temperature exceeding 900 to 1250 ° C. and then pulverized to produce an iron pulverized powder. The iron pulverized powder is mixed with Si powder or ferrosilicon powder. After that, a method for producing a surface high Si layer-coated iron powder characterized by heating in a hydrogen atmosphere at a temperature of 920 to 1100 ° C. and then pulverizing. 前記鉄粉末は、純度：９８．５質量％以上の鉄粉末であることを特徴とする請求項１記載の表面高Ｓｉ層被覆鉄粉末の製造方法。 The method for producing a surface high Si layer-coated iron powder according to claim 1, wherein the iron powder is an iron powder having a purity of 98.5% by mass or more. 前記Ｓｉ粉末またはフェロシリコン粉末は、粒径：１０μｍ以下の微細粉末であることを特徴とする請求項１記載の表面高Ｓｉ層被覆鉄粉末の製造方法。 2. The method for producing a surface high Si layer-coated iron powder according to claim 1, wherein the Si powder or ferrosilicon powder is a fine powder having a particle size of 10 [mu] m or less. 請求項１、２または３記載の方法で作製した表面高Ｓｉ層被覆鉄粉末にバインダーを０．２〜３質量％添加したのち圧粉成形し、この圧粉成形体を５００〜９００℃で焼成することを特徴とする複合軟磁性材の製造方法。 The surface high Si layer-coated iron powder produced by the method according to claim 1, 2 or 3 is added with 0.2 to 3 mass% of binder and then compacted, and the compact is fired at 500 to 900 ° C. A method for producing a composite soft magnetic material, comprising: 請求項４記載のバインダーは、エポキシ樹脂、フッ素樹脂、シリコーン樹脂、ポリイミド樹脂、ポリエステル樹脂、ポリアミド樹脂、フェノール樹脂などの有機樹脂、リン酸塩、ガラス状絶縁物、珪酸ソーダを主成分とする水ガラス、または絶縁性酸化物であることを特徴とする複合軟磁性材の製造方法。 The binder according to claim 4 is an epoxy resin, a fluororesin, a silicone resin, a polyimide resin, a polyester resin, a polyamide resin, an organic resin such as a phenol resin, a phosphate, a glassy insulator, or water mainly composed of sodium silicate. A method for producing a composite soft magnetic material, characterized by being made of glass or an insulating oxide. 請求項４または５記載の方法で作製した複合軟磁性材からなる電磁気回路部品。 An electromagnetic circuit component comprising a composite soft magnetic material produced by the method according to claim 4. 請求項６記載の電磁気回路部品は、磁心、電動機コア，発電機コア，ソレノイドコア，イグニッションコア，トランスコア，チョークコイルコアまたは磁気センサコアであることを特徴とする電磁気回路部品。 The electromagnetic circuit component according to claim 6, wherein the electromagnetic circuit component is a magnetic core, a motor core, a generator core, a solenoid core, an ignition core, a transformer core, a choke coil core, or a magnetic sensor core. 請求項７記載の前記電磁気回路部品を組み込んだ電気機器。 An electric device incorporating the electromagnetic circuit component according to claim 7.
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