JP2003306703A - Fe-Co COMPOSITE SOFT MAGNETIC SINTERED ALLOY WITH HIGH DENSITY AND HIGH MAGNETIC PERMEABILITY, AND ITS MANUFACTURING METHOD - Google Patents
Fe-Co COMPOSITE SOFT MAGNETIC SINTERED ALLOY WITH HIGH DENSITY AND HIGH MAGNETIC PERMEABILITY, AND ITS MANUFACTURING METHODInfo
- Publication number
- JP2003306703A JP2003306703A JP2002114157A JP2002114157A JP2003306703A JP 2003306703 A JP2003306703 A JP 2003306703A JP 2002114157 A JP2002114157 A JP 2002114157A JP 2002114157 A JP2002114157 A JP 2002114157A JP 2003306703 A JP2003306703 A JP 2003306703A
- Authority
- JP
- Japan
- Prior art keywords
- soft magnetic
- peak
- powder
- composite soft
- alloy
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910017061 Fe Co Inorganic materials 0.000 title claims abstract description 61
- 239000002131 composite material Substances 0.000 title claims abstract description 52
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 41
- 239000000956 alloy Substances 0.000 title claims abstract description 41
- 230000035699 permeability Effects 0.000 title claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 6
- 239000002245 particle Substances 0.000 claims abstract description 52
- 229910001004 magnetic alloy Inorganic materials 0.000 claims abstract description 40
- 239000000843 powder Substances 0.000 claims abstract description 40
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052596 spinel Inorganic materials 0.000 claims abstract description 18
- 239000011029 spinel Substances 0.000 claims abstract description 18
- 239000006247 magnetic powder Substances 0.000 claims abstract description 16
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 5
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 5
- 239000011812 mixed powder Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 abstract description 11
- 238000005245 sintering Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- 239000012535 impurity Substances 0.000 description 6
- 229910052742 iron Inorganic materials 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910017112 Fe—C Inorganic materials 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 229910052748 manganese Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229910052720 vanadium Inorganic materials 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 229910001510 metal chloride Inorganic materials 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229910000531 Co alloy Inorganic materials 0.000 description 1
- 230000004931 aggregating effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Landscapes
- Powder Metallurgy (AREA)
- Soft Magnetic Materials (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】この発明は、高密度および高透磁
性を有するＦｅ−Ｃｏ系複合軟磁性焼結合金およびその
製造方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a Fe-Co based composite soft magnetic sintered alloy having high density and high magnetic permeability and a method for producing the same.
【０００２】[0002]
【従来の技術】モータ、アクチュエータなどに用いられ
る低ロスヨーク、トランス、チョークコイルなどの磁心
にはＦｅ−Ｃｏ系軟磁性焼結材料が用いられることは知
られており、このＦｅ−Ｃｏ系軟磁性焼結材料は、質量
％でＣｏ：２５〜６０％を含有し、残部がＦｅおよび不
可避不純物からなるＦｅ−Ｃｏ系軟磁性合金粉末、また
はＣｏ：２５〜６０％、Ｖ：０．５〜５％を含有し、残
部がＦｅおよび不可避不純物からなるＦｅ−Ｃｏ系軟磁
性合金粉末を焼結して得られることが知られている。さ
らにスピネル構造を有するフェライトなど金属酸化物粉
末を焼結して得られることが知られている。前記スピネ
ル構造を有するフェライトは、一般に（ＭｅＦｅ）3Ｏ4
（但し、ＭｅはＭｎ，Ｚｎ，Ｎｉ，Ｍｇ，Ｃｕ，Ｆｅも
しくはＣｏまたはこれらの混合物）で表されることが知
られている。2. Description of the Related Art It is known that Fe--Co based soft magnetic sintered materials are used for magnetic cores such as low loss yokes, transformers and choke coils used in motors and actuators. The sintering material contains Co: 25 to 60% by mass, and the balance is Fe-Co soft magnetic alloy powder consisting of Fe and unavoidable impurities, or Co: 25 to 60%, V: 0.5 to 5 It is known that it can be obtained by sintering an Fe-Co based soft magnetic alloy powder containing 100% by weight and the balance being Fe and inevitable impurities. Further, it is known to be obtained by sintering a metal oxide powder such as ferrite having a spinel structure. The ferrite having the spinel structure is generally (MeFe) 3 O 4
(However, Me is known to be represented by Mn, Zn, Ni, Mg, Cu, Fe or Co or a mixture thereof).
【０００３】また、これらＦｅ−Ｃｏ系軟磁性合金粉末
は、飽和磁束密度が高いが、高周波特性が悪く、一方、スピ
ネル構造を有するフェライトなど金属酸化物粉末を焼結
して得られた酸化物軟磁性焼結材料は、高周波特性に優
れ、初透磁率が比較的高いが、飽和磁束密度が低い欠点が
あり、これらを改善するために、金属軟磁性粉末の表面に
スピネル構造を有するフェライト層を被覆してなる複合
軟磁性粉末を焼結して得られたＦｅ−Ｃｏ系複合軟磁性
焼結合金が提案されている（特開昭５６−３８４０２号
公報参照）。Further, these Fe--Co type soft magnetic alloy powders have high saturation magnetic flux density but poor high frequency characteristics. On the other hand, oxides obtained by sintering metal oxide powders such as ferrite having a spinel structure. The soft magnetic sintered material has excellent high-frequency characteristics and relatively high initial magnetic permeability, but has a drawback that the saturation magnetic flux density is low. In order to improve these, a ferrite layer having a spinel structure on the surface of the metal soft magnetic powder is used. A Fe-Co-based composite soft magnetic sintered alloy obtained by sintering a composite soft magnetic powder obtained by coating is proposed (see JP-A-56-38402).
【０００４】[0004]
【発明が解決しようとする課題】しかし、前記Ｆｅ−Ｃ
ｏ系軟磁性合金粉末は硬いために通常の成形条件では十
分な密度の成形体を得ることが難しく、さらに前記Ｆｅ
−Ｃｏ系軟磁性合金粉末の表面にスピネル構造を有する
フェライト層を被覆してなる複合軟磁性粉末を焼結して
得られたＦｅ−Ｃｏ系複合軟磁性焼結合金は、スピネル
構造を有するフェライト層が酸化物であるために焼結性
が悪く、したがって、十分な密度および磁気特性を有す
るＦｅ−Ｃｏ系複合軟磁性焼結合金が得られない。その
ため、Ｆｅ−Ｃｏ系軟磁性合金粉末の表面にスピネル構
造を有するフェライト層を被覆してなる複合軟磁性粉末
を成形して得られる成形体は十分な密度が得られず、ま
たこの複合軟磁性粉末の成形体を燒結して得られるＦｅ
−Ｃｏ系複合軟磁性焼結合金は十分な高密度が得られな
いために十分な透磁性が得られない、という課題があっ
た。However, the above Fe-C is used.
Since the o-type soft magnetic alloy powder is hard, it is difficult to obtain a compact having a sufficient density under ordinary molding conditions.
An Fe—Co based composite soft magnetic sintered alloy obtained by sintering a composite soft magnetic powder obtained by coating a surface of a —Co based soft magnetic alloy powder with a ferrite layer having a spinel structure is a ferrite having a spinel structure. Since the layer is an oxide, the sinterability is poor, and therefore a Fe—Co based composite soft magnetic sintered alloy having sufficient density and magnetic properties cannot be obtained. Therefore, a compact obtained by molding the composite soft magnetic powder obtained by coating the surface of the Fe-Co soft magnetic alloy powder with the ferrite layer having the spinel structure cannot obtain sufficient density, and the composite soft magnetic powder Fe obtained by sintering a powder compact
The -Co-based composite soft magnetic sintered alloy has a problem that sufficient magnetic permeability cannot be obtained because a sufficient high density cannot be obtained.
【０００５】[0005]
【課題を解決するための手段】そこで、本発明者らは、
かかる課題を解決すべく研究を行った結果、
（イ）Ｆｅ−Ｃｏ系軟磁性合金粉末の粒度分布がＤ１＝
３０〜２００μｍ（一層好ましくは８０〜１５０μｍ）
を中心とする第１ピークと、Ｄ２＝０．０５〜０．５×
Ｄ１μｍを中心とする第２ピークを有し、第１ピークは
第２ピークよりも大きな粒度分布を有するＦｅ−Ｃｏ系
軟磁性合金粉末を使用して圧粉成形すると成形体の密度
が一層向上するところから、この粒度分布を有するＦｅ
−Ｃｏ系軟磁性合金粉末の表面にスピネル構造を有する
フェライト層が被覆されている複合軟磁性粉末を圧粉成
形して得られる成形体の密度も一層向上する、（ロ）こ
の粒度分布を有するＦｅ−Ｃｏ系軟磁性合金粉末の表面
にスピネル構造を有するフェライト層が被覆されている
複合軟磁性粉末に、平均粒径：１００ｎｍ以下の二酸化
ケイ素粉末を０．０５〜１．０質量％添加し混合して得
られた混合粉末は燒結性が向上するところから密度が向
上し、したがって機械的強度が向上し、さらに磁気特
性、特に高周波における比透磁率が向上する、（ハ）前
記複合軟磁性粉末に二酸化ケイ素粉末を混合して得られ
た混合粉末を圧粉成形し焼結することにより得られたＦ
ｅ−Ｃｏ系複合軟磁性焼結合金は、Ｆｅ−Ｃｏ系軟磁性
合金粒子が平均粒径：１００ｎｍ以下の二酸化ケイ素粉
末を含むスピネル構造を有するフェライト粒界相により
被覆され隔離されて分散した組織を有する、などの研究
結果が得られたのである。Therefore, the present inventors have
As a result of research to solve such problems, (a) the particle size distribution of the Fe—Co soft magnetic alloy powder is D1 =
30-200 μm (more preferably 80-150 μm)
The first peak centered at, and D2 = 0.05 to 0.5 ×
When a Fe-Co soft magnetic alloy powder having a second peak centered at D1 [mu] m and the first peak having a larger particle size distribution than the second peak is used for powder compaction, the density of the compact is further improved. Therefore, Fe having this particle size distribution
-The density of the molded body obtained by compacting the composite soft magnetic powder in which the ferrite layer having the spinel structure is coated on the surface of the Co-based soft magnetic alloy powder is further improved, and (b) has this particle size distribution. 0.05 to 1.0 mass% of silicon dioxide powder having an average particle diameter of 100 nm or less is added to the composite soft magnetic powder in which the surface of the Fe-Co soft magnetic alloy powder is coated with the ferrite layer having the spinel structure. The mixed powder obtained by mixing improves the sinterability and thus the density, and thus the mechanical strength, and further improves the magnetic properties, especially the relative permeability at high frequencies. F obtained by compacting and sintering a mixed powder obtained by mixing silicon dioxide powder with the powder
The e-Co-based composite soft magnetic sintered alloy is a structure in which Fe-Co-based soft magnetic alloy particles are covered with a ferrite grain boundary phase having a spinel structure containing silicon dioxide powder having an average particle diameter of 100 nm or less and are isolated and dispersed. The result of the study was obtained.
【０００６】この発明は、かかる研究結果に基づいてな
されたものであって、（１）Ｆｅ−Ｃｏ系軟磁性合金粒
子が平均粒径：１００ｎｍ以下の二酸化ケイ素粒子を含
むスピネル構造を有するフェライト粒界相により被覆さ
れて分散しており、前記Ｆｅ−Ｃｏ系軟磁性合金粒子は
粒度分布がＤ１＝３０〜２００μｍを中心とする第１ピ
ークと、Ｄ２＝０．０５〜０．５×Ｄ１μｍを中心とす
る第２ピークを有し、第１ピークは第２ピークよりも大
きな粒度分布を有する組織を有する高密度および高透磁
性を有するＦｅ−Ｃｏ系複合軟磁性焼結合金、（２）粒
度分布がＤ１＝３０〜２００μｍを中心とする第１ピー
クと、Ｄ２＝０．０５〜０．５×Ｄ１μｍを中心とする
第２ピークを有し、第１ピークは第２ピークよりも大き
な粒度分布を有するＦｅ−Ｃｏ系軟磁性合金粉末の表面
にスピネル構造を有するフェライト層が被覆されている
複合軟磁性粉末に、平均粒径：１００ｎｍ以下の二酸化
ケイ素粉末を０．０５〜１．０質量％添加して混合し、
得られた混合粉末を圧粉成形し焼結する高密度および高
透磁性を有するＦｅ−Ｃｏ系複合軟磁性焼結合金の製造
方法、に特徴を有するものである。The present invention has been made on the basis of the above research results, and (1) ferrite particles having a spinel structure, in which Fe-Co soft magnetic alloy particles include silicon dioxide particles having an average particle size of 100 nm or less. The Fe-Co based soft magnetic alloy particles are dispersed by being covered with a boundary phase, and the particle size distribution has a first peak centered at D1 = 30 to 200 μm and D2 = 0.05 to 0.5 × D1 μm. Fe-Co based composite soft magnetic sintered alloy having a high density and high magnetic permeability, having a central second peak, the first peak having a grain size distribution larger than the second peak, (2) grain size The distribution has a first peak centered at D1 = 30 to 200 μm and a second peak centered at D2 = 0.05 to 0.5 × D1 μm, the first peak having a larger particle size distribution than the second peak. With F By adding 0.05 to 1.0 mass% of silicon dioxide powder having an average particle diameter of 100 nm or less to the composite soft magnetic powder in which the ferrite layer having the spinel structure is coated on the surface of the Co based soft magnetic alloy powder. Mix and
The present invention is characterized by a method for producing a Fe-Co based composite soft magnetic sintered alloy having high density and high magnetic permeability, which is obtained by compacting and sintering the obtained mixed powder.
【０００７】この発明の高密度および高透磁性を有する
Ｆｅ−Ｃｏ系複合軟磁性焼結合金の素地に分散するＦｅ
−Ｃｏ系軟磁性合金粒子は、質量％でＣｏ：２５〜６０
％を含有し、残部がＦｅおよび不可避不純物からなるＦ
ｅ−Ｃｏ系軟磁性合金粒子、またはＣｏ：２５〜６０
％、Ｖ：０．５〜５％を含有し、残部がＦｅおよび不可
避不純物からなるＦｅ−Ｃｏ系軟磁性合金粒子であるこ
とが好ましいが、この組成に限定されるものではなく、
軟磁性を示すＦｅ−Ｃｏ系合金粒子であればいかなる成
分組成のＦｅ−Ｃｏ系軟磁性合金粒子であっても良い。
また、Ｆｅ−Ｃｏ系軟磁性合金粒子を被覆し隔離する平
均粒径：１００ｎｍ以下の二酸化ケイ素粒子を含むスピ
ネル構造を有するフェライト粒界相は、一般式（ＭｅＦ
ｅ）3Ｏ4（但し、ＭｅはＭｎ，Ｚｎ，Ｎｉ，Ｍｇ，Ｃ
ｕ，Ｆｅまたはこれらの混合物）で表されるフェライト
粒界相である。したがって、この発明の高密度および高
透磁性を有するＦｅ−Ｃｏ系複合軟磁性焼結合金を製造
するために使用する複合軟磁性粉末は、質量％でＣｏ：
２５〜６０％を含有し、残部がＦｅおよび不可避不純物
からなるＦｅ−Ｃｏ系軟磁性合金粉末、またはＣｏ：２
５〜６０％、Ｖ：０．５〜５％を含有し、残部がＦｅお
よび不可避不純物からなるＦｅ−Ｃｏ系軟磁性合金粉末
の表面にフェライト層を被覆した粉末であることが好ま
しいが、前記Ｆｅ−Ｃｏ系軟磁性合金粉末は前記成分組
成に特に限定されるものではなく、軟磁性を示すＦｅ−
Ｃｏ系合金粉末であればいかなる成分組成のＦｅ−Ｃｏ
系軟磁性合金粉末であっても良い。Fe dispersed in the base material of the Fe-Co type composite soft magnetic sintered alloy having high density and high magnetic permeability of the present invention.
-Co-based soft magnetic alloy particles have a mass% of Co: 25 to 60
%, With the balance being Fe and inevitable impurities
e-Co soft magnetic alloy particles, or Co: 25-60
%, V: 0.5 to 5%, and the balance is preferably Fe-Co based soft magnetic alloy particles containing Fe and unavoidable impurities, but is not limited to this composition.
Fe—Co based soft magnetic alloy particles having any composition may be used as long as they are soft magnetic Fe—Co based alloy particles.
Further, the ferrite grain boundary phase having a spinel structure containing silicon dioxide particles having an average particle diameter of 100 nm or less for covering and isolating Fe—Co based soft magnetic alloy particles has a general formula (MeF).
e) 3 O 4 (however, Me is Mn, Zn, Ni, Mg, C
It is a ferrite grain boundary phase represented by u, Fe or a mixture thereof. Therefore, the composite soft magnetic powder used for producing the Fe-Co based composite soft magnetic sintered alloy having high density and high magnetic permeability of the present invention is Co:
Fe-Co soft magnetic alloy powder containing 25 to 60% and the balance Fe and unavoidable impurities, or Co: 2
5 to 60%, V: 0.5 to 5%, the balance is preferably Fe-Co based soft magnetic alloy powder consisting of Fe and unavoidable impurities, the surface of which is coated with a ferrite layer. The Fe-Co based soft magnetic alloy powder is not particularly limited to the above component composition, and Fe- which exhibits soft magnetism
Fe-Co having any composition as long as it is a Co alloy powder
The soft magnetic alloy powder may be used.
【０００８】この発明の高密度および高透磁性を有する
Ｆｅ−Ｃｏ系複合軟磁性焼結合金に含まれる二酸化ケイ
素粉末の平均粒径を１００ｎｍ以下に限定した理由は、
二酸化ケイ素粉末の平均粒径が１００ｎｍを越えると焼
結性向上効果が低下すると共に比透磁率が低下するから
である。この二酸化ケイ素粉末の平均粒径の下限は製造
コストの面から１ｎｍ以上であることが一層好ましい。
また、平均粒径：１００ｎｍ以下の二酸化ケイ素粉末の
添加量を０．０５質量％以上にした理由は、平均粒径：
１００ｎｍ以下の二酸化ケイ素が０．０５質量％未満含
まれていても焼結性に大きく影響を及ぼすことはなくま
た比透磁率が低下するからであり、一方、１．０質量％
を越えて含有すると非磁性相の割合が多くなり、比透磁
率の低下をもたらすので好ましくないことによるもので
ある。二酸化ケイ素粉末の添加量の一層好ましい範囲は
０．１〜０．５質量％である。The reason why the average particle size of the silicon dioxide powder contained in the Fe--Co type composite soft magnetic sintered alloy having high density and high magnetic permeability of the present invention is limited to 100 nm or less is as follows.
This is because if the average particle diameter of the silicon dioxide powder exceeds 100 nm, the effect of improving sinterability is reduced and the relative permeability is reduced. The lower limit of the average particle size of the silicon dioxide powder is more preferably 1 nm or more from the viewpoint of manufacturing cost.
Further, the reason why the addition amount of the silicon dioxide powder having an average particle diameter of 100 nm or less is 0.05% by mass or more is that the average particle diameter:
This is because if the content of silicon dioxide of 100 nm or less is less than 0.05% by mass, the sinterability is not significantly affected and the relative magnetic permeability is decreased, while 1.0% by mass is used.
This is because if the content exceeds the above range, the proportion of the non-magnetic phase increases and the relative magnetic permeability decreases, which is not preferable. A more preferable range of the amount of silicon dioxide powder added is 0.1 to 0.5% by mass.
【０００９】[0009]
【発明の実施の形態】表１に示される成分組成を有する
Ｆｅ−Ｃｏ系軟磁性合金原料を高周波溶解して溶湯を作
製し、これら溶湯を水アトマイズしてＦｅ−Ｃｏ系軟磁
性合金アトマイズ粉末を作製し、そのアトマイズ粉末を
分級処理してＦｅ−Ｃｏ系軟磁性合金アトマイズ原料粉
末を作製した。このアトマイズ原料粉末をさらに風力分
級機により分級し、表１に示されるＤ１＝３０〜２００
μｍを中心とする第１ピークと、Ｄ２＝０．０５〜０．
５×Ｄ１μｍを中心とする第２ピークを有するＦｅ−Ｃ
ｏ系軟磁性合金粉末を作製した。このＦｅ−Ｃｏ系軟磁
性合金粉末の粒度分布はマイクロトラック装置により測
定した。BEST MODE FOR CARRYING OUT THE INVENTION Fe-Co based soft magnetic alloy raw materials having the composition shown in Table 1 are melted by high frequency to prepare molten metal, and these molten metal are atomized with water to form Fe-Co based soft magnetic alloy atomized powder. Was prepared, and the atomized powder was classified to prepare Fe—Co based soft magnetic alloy atomized raw material powder. This atomized raw material powder was further classified by an air classifier, and D1 = 30 to 200 shown in Table 1
the first peak centered at .mu.m and D2 = 0.05-0.
Fe-C having a second peak centered at 5 × D1 μm
An o-based soft magnetic alloy powder was produced. The particle size distribution of this Fe-Co based soft magnetic alloy powder was measured by a Microtrack device.
【００１０】このようにして得られたＦｅ−Ｃｏ系軟磁
性合金粉末をイオン交換水に浸漬してよく撹拌したの
ち、窒素により十分に脱酸素を行なった。この窒素によ
り十分に脱酸素を行なったイオン交換水に、金属塩化物
（ＭＣｌ2,ただしＭ＝Ｆｅ、Ｚｎ、Ｍｎ）を溶かし、酸化
物膜組成が得られるよう調製された金属塩化物水溶液を
静かに注ぎ、その後ＮａＯＨ水溶液によりｐＨを７.０に
調整した。この混合液を７０℃一定に保ち、０.５〜３
時間に渡り空気を吹き込みながら緩やかに撹拌し、Ｆｅ
−Ｃｏ系軟磁性合金粉末の表面に表１に示される厚さの
（Ｍｎ17Ｚｎ16Ｆｅ67）3Ｏ4フェライト膜を成膜した。
その後、このフェライト膜を成膜したＦｅ−Ｃｏ系軟磁
性合金粉末を濾過、水洗、乾燥することにより表１に示
される複合軟磁性粉末Ａ〜ｄを得た。The Fe--Co type soft magnetic alloy powder thus obtained was immersed in ion-exchanged water, stirred well, and then sufficiently deoxidized with nitrogen. A metal chloride aqueous solution prepared by dissolving a metal chloride (MCl 2 , where M = Fe, Zn, Mn) in ion-exchanged water that has been sufficiently deoxygenated with nitrogen to obtain an oxide film composition is prepared. Pour gently and then adjust pH to 7.0 with aqueous NaOH solution. Keep this mixture at 70 ℃ constant, 0.5-3
Stir gently while blowing air over time
-Co-based thickness shown in the surface of the soft magnetic alloy powder in Table 1 (Mn 17 Zn 16 Fe 67) 3 O 4 ferrite film was formed.
Thereafter, the Fe-Co based soft magnetic alloy powder on which this ferrite film was formed was filtered, washed with water, and dried to obtain composite soft magnetic powders A to d shown in Table 1.
【００１１】得られた複合軟磁性粉末Ａ〜ｄに、表２に
示す平均粒径のＳｉＯ2粉末を表２に示す割合となるよ
うに混ぜ、６ｔｏｎ／ｃｍ2の成形圧をかけることによ
り外径：３５ｍｍ、内径：２５ｍｍ、高さ：５ｍｍのリ
ング状圧粉体を成形し、得られたリング状圧粉体を不活
性ガス雰囲気中、１０００℃の温度で焼結することによ
りリング状焼結体からなる本発明Ｆｅ−Ｃｏ系複合軟磁
性焼結合金１〜１２、比較Ｆｅ−Ｃｏ系複合軟磁性焼結
合金１〜７および従来Ｆｅ−Ｃｏ系複合軟磁性焼結合金
を作製した。このようにして得られたリング状焼結体の
組織をＳＥＭで観察した結果、本発明Ｆｅ−Ｃｏ系複合
軟磁性焼結合金１〜１２および比較Ｆｅ−Ｃｏ系複合軟
磁性焼結合金１〜７にはいずれもＳｉＯ2粉末がフェラ
イト粒界相中に分散している組織を有していた。さらに
これら本発明Ｆｅ−Ｃｏ系複合軟磁性焼結合金１〜１
２、比較Ｆｅ−Ｃｏ系複合軟磁性焼結合金１〜７および
従来Ｆｅ−Ｃｏ系複合軟磁性焼結合金についてＳＥＭで
被測定粒子群の濃淡画像を入力し、それに粒子分離画像
処理を施し、この画像よりＦｅ−Ｃｏ系軟磁性合金粒子
の円相当径法にて求めた面積を基に各粒子の直径を求
め、求めた直径を集計することにより粒度分布を求めた
ところ、本発明Ｆｅ−Ｃｏ系複合軟磁性焼結合金１〜１
２、比較Ｆｅ−Ｃｏ系複合軟磁性焼結合金１〜７および
従来Ｆｅ−Ｃｏ系複合軟磁性焼結合金の各組織における
Ｆｅ−Ｃｏ系軟磁性合金粒子は前記アトマイズ粉末の粒
度分布とほぼ同じ粒度分布を示していた。その後、さら
にＦｅ−Ｃｏ系複合軟磁性焼結合金１〜１２、比較Ｆｅ
−Ｃｏ系複合軟磁性焼結合金１〜７および従来Ｆｅ−Ｃ
ｏ系複合軟磁性焼結合金の相対密度を測定し、その結果
を表３〜４に示した。さらに、本発明Ｆｅ−Ｃｏ系複合
軟磁性焼結合金１〜１２、比較Ｆｅ−Ｃｏ系複合軟磁性
焼結合金１〜７および従来Ｆｅ−Ｃｏ系複合軟磁性焼結
合金について表３〜４に示される周波数の高周波におけ
る比透磁率をインピーダンスアナライザで測定し、その
結果を表３〜４に示した。The obtained composite soft magnetic powders A to d were mixed with SiO 2 powder having an average particle size shown in Table 2 at a ratio shown in Table 2, and a molding pressure of 6 ton / cm 2 was applied to remove them. A ring-shaped green compact having a diameter of 35 mm, an inner diameter of 25 mm, and a height of 5 mm is molded, and the obtained ring-shaped green compact is sintered at a temperature of 1000 ° C. in an inert gas atmosphere to form a ring-shaped powder. Fe-Co based composite soft magnetic sintered alloys 1 to 12 of the present invention, comparative Fe-Co based composite soft magnetic sintered alloys 1 to 7 and conventional Fe-Co based composite soft magnetic sintered alloys were prepared. As a result of observing the structure of the ring-shaped sintered body thus obtained by SEM, the present invention Fe-Co-based composite soft magnetic sintered alloys 1 to 12 and comparative Fe-Co-based composite soft magnetic sintered alloys 1 to 1 All of the samples 7 had a structure in which SiO 2 powder was dispersed in the ferrite grain boundary phase. Further, these Fe—Co based composite soft magnetic sintered alloys 1 to 1 of the present invention
2, the comparative Fe-Co composite soft magnetic sintered alloys 1 to 7 and the conventional Fe-Co composite soft magnetic sintered alloys are input with the SEM a grayscale image of the particle group to be measured and subjected to particle separation image processing, From this image, the diameter of each particle was calculated based on the area of the Fe-Co soft magnetic alloy particles calculated by the circle equivalent diameter method, and the particle diameter distribution was calculated by aggregating the calculated diameters. Co-based composite soft magnetic sintered alloy 1-1
2. Comparative Fe—Co based composite soft magnetic sintered alloys 1 to 7 and Fe—Co based soft magnetic alloy particles in each structure of conventional Fe—Co based composite soft magnetic sintered alloys have almost the same particle size distribution as the atomized powder. It showed a particle size distribution. After that, Fe-Co composite soft magnetic sintered alloys 1 to 12 and comparative Fe were further added.
-Co-based composite soft magnetic sintered alloys 1 to 7 and conventional Fe-C
The relative density of the o-based composite soft magnetic sintered alloy was measured, and the results are shown in Tables 3 and 4. Further, Tables 3 and 4 show the Fe—Co based composite soft magnetic sintered alloys 1 to 12 of the present invention, the comparative Fe—Co based composite soft magnetic sintered alloys 1 to 7 and the conventional Fe—Co based composite soft magnetic sintered alloys. The relative magnetic permeability at a high frequency of the indicated frequency was measured with an impedance analyzer, and the results are shown in Tables 3-4.
【００１２】[0012]
【表１】 [Table 1]
【００１３】[0013]
【表２】 [Table 2]
【００１４】[0014]
【表３】 [Table 3]
【００１５】[0015]
【表４】 [Table 4]
【００１６】表１〜４に示される結果から、Ｆｅ−Ｃｏ
系複合軟磁性合金粉末の表面にスピネル構造を有するフ
ェライト層が被覆されている複合軟磁性粉末にＳｉＯ2
粉末を０．０５〜１．０質量％添加し混合し圧粉成形し
焼結して得られた本発明Ｆｅ−Ｃｏ系複合軟磁性焼結合
金１〜１２は、従来Ｆｅ−Ｃｏ系複合軟磁性焼結合金に
比べて高密度を有すると共に高周波における比透磁率が
優れていることが分かる。しかし、この発明の範囲から
外れた条件で作製した比較Ｆｅ−Ｃｏ系複合軟磁性焼結
合金１〜７は密度または比透磁率の内の少なくともいず
れかが劣るので好ましくないことが分かる。From the results shown in Tables 1 to 4, Fe--Co
SiO 2 in the composite soft magnetic powder ferrite layer is coated with a spinel structure in the surface of the system complex soft magnetic alloy powder
Fe-Co-based composite soft magnetic sintered alloys 1 to 12 of the present invention obtained by adding and mixing powder in an amount of 0.05 to 1.0% by mass, compacting and compacting the powder are conventional Fe-Co-based composite soft alloys. It can be seen that the magnetic sintered alloy has high density and high relative permeability at high frequencies as compared with the magnetic sintered alloy. However, it is understood that the comparative Fe—Co based composite soft magnetic sintered alloys 1 to 7 produced under the conditions outside the scope of the present invention are inferior in at least one of the density and the relative magnetic permeability, which is not preferable.
【００１７】[0017]
【発明の効果】この発明は、高密度で機械的強度が優
れ、さらに高周波の比透磁率の高いＦｅ−Ｃｏ系複合軟
磁性焼結合金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。INDUSTRIAL APPLICABILITY The present invention can provide a Fe-Co based composite soft magnetic sintered alloy having a high density, excellent mechanical strength, and high relative permeability at high frequencies, and is excellent in the electrical and electronic industries. It has an effect.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｃ２２Ｃ 38/00 ３０４ Ｃ２２Ｃ 38/00 ３０４ 38/10 38/10 Ｈ０１Ｆ 1/22 Ｈ０１Ｆ 1/22 (72)発明者 中山 亮治 埼玉県さいたま市北袋町１−297 三菱マ テリアル株式会社総合研究所内 (72)発明者 森本 耕一郎 新潟県新潟市小金町３−１ 三菱マテリア ル株式会社新潟製作所内 Ｆターム(参考） 4K018 AA25 AB01 AC01 BA16 BC12 BC33 CA00 DA00 5E041 AA05 AA19 BC01 BC08 BD01 CA02 HB03 HB05 HB17 NN05 NN06 ─────────────────────────────────────────────────── ─── Continuation of front page (51) Int.Cl. 7 Identification code FI theme code (reference) C22C 38/00 304 C22C 38/00 304 38/10 38/10 H01F 1/22 H01F 1/22 (72) Inventor Ryoji Nakayama 1-297 Kitabukuro-cho, Saitama City, Saitama Prefecture Mitsubishi Materials Corp. Research Laboratory (72) Inventor Koichiro Morimoto 3-1 Koganecho, Niigata City, Niigata Prefecture Mitsubishi Material Co., Ltd. F-term in Niigata Plant (reference) 4K018 AA25 AB01 AC01 BA16 BC12 BC33 CA00 DA00 5E041 AA05 AA19 BC01 BC08 BD01 CA02 HB03 HB05 HB17 NN05 NN06
Claims (2)
１００ｎｍ以下の二酸化ケイ素粒子を含むスピネル構造
を有するフェライト粒界相により被覆されて分散してお
り、前記Ｆｅ−Ｃｏ系軟磁性合金粒子は粒度分布がＤ１
＝３０〜２００μｍを中心とする第１ピークと、Ｄ２＝
０．０５〜０．５×Ｄ１μｍを中心とする第２ピークを
有し、第１ピークは第２ピークよりも大きな粒度分布を
有する組織を有することを特徴とする高密度および高透
磁性を有するＦｅ−Ｃｏ系複合軟磁性焼結合金。1. Fe-Co soft magnetic alloy particles have an average particle diameter:
The Fe-Co based soft magnetic alloy particles are coated with and dispersed by a ferrite grain boundary phase having a spinel structure containing silicon dioxide particles of 100 nm or less, and the particle size distribution is D1.
= The first peak centered at 30 to 200 μm, and D2 =
High density and high magnetic permeability characterized by having a second peak centered at 0.05 to 0.5 × D1 μm, the first peak having a structure with a larger particle size distribution than the second peak. Fe-Co based composite soft magnetic sintered alloy.
とする第１ピークと、Ｄ２＝０．０５〜０．５×Ｄ１μ
ｍを中心とする第２ピークを有し、第１ピークは第２ピ
ークよりも大きな粒度分布を有するＦｅ−Ｃｏ系軟磁性
合金粉末の表面にスピネル構造を有するフェライト層が
被覆されている複合軟磁性粉末に、平均粒径：１００ｎ
ｍ以下の二酸化ケイ素粉末を０．０５〜１．０質量％添
加して混合し、得られた混合粉末を圧粉成形し焼結する
ことを特徴とする高密度および高透磁性を有するＦｅ−
Ｃｏ系複合軟磁性焼結合金の製造方法。2. A first peak having a particle size distribution centered at D1 = 30 to 200 μm and D2 = 0.05 to 0.5 × D1 μ.
The composite soft magnetic powder has a second peak centered at m, and the first peak has a particle size distribution larger than that of the second peak, and the ferrite layer having a spinel structure is coated on the surface of the Fe-Co soft magnetic alloy powder. Magnetic powder, average particle size: 100n
Fe- having high density and high magnetic permeability, characterized in that 0.05 to 1.0% by mass of silicon dioxide powder of m or less is added and mixed, and the obtained mixed powder is compacted and sintered.
A method for producing a Co-based composite soft magnetic sintered alloy.
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|---|---|---|---|
| JP2002114157A JP2003306703A (en) | 2002-04-17 | 2002-04-17 | Fe-Co COMPOSITE SOFT MAGNETIC SINTERED ALLOY WITH HIGH DENSITY AND HIGH MAGNETIC PERMEABILITY, AND ITS MANUFACTURING METHOD |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002114157A JP2003306703A (en) | 2002-04-17 | 2002-04-17 | Fe-Co COMPOSITE SOFT MAGNETIC SINTERED ALLOY WITH HIGH DENSITY AND HIGH MAGNETIC PERMEABILITY, AND ITS MANUFACTURING METHOD |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009054615A (en) * | 2007-08-23 | 2009-03-12 | Alps Electric Co Ltd | Powder magnetic core, and manufacturing method thereof |
| JP2015190017A (en) * | 2014-03-28 | 2015-11-02 | 三菱マテリアル株式会社 | Softly magnetic thin film forming sputtering target |
| US20230130266A1 (en) * | 2021-10-21 | 2023-04-27 | Tdk Corporation | Soft magnetic alloy powder, dust core, and magnetic device |
-
2002
- 2002-04-17 JP JP2002114157A patent/JP2003306703A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009054615A (en) * | 2007-08-23 | 2009-03-12 | Alps Electric Co Ltd | Powder magnetic core, and manufacturing method thereof |
| JP2015190017A (en) * | 2014-03-28 | 2015-11-02 | 三菱マテリアル株式会社 | Softly magnetic thin film forming sputtering target |
| US20230130266A1 (en) * | 2021-10-21 | 2023-04-27 | Tdk Corporation | Soft magnetic alloy powder, dust core, and magnetic device |
| US12062474B2 (en) * | 2021-10-21 | 2024-08-13 | Tdk Corporation | Soft magnetic alloy powder comprising Fe, Co and Si, dust core, and magnetic device |
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