JPH0715121B2 - Fe-Co alloy fine powder for injection molding and Fe-Co sintered magnetic material - Google Patents
Fe-Co alloy fine powder for injection molding and Fe-Co sintered magnetic materialInfo
- Publication number
- JPH0715121B2 JPH0715121B2 JP63206720A JP20672088A JPH0715121B2 JP H0715121 B2 JPH0715121 B2 JP H0715121B2 JP 63206720 A JP63206720 A JP 63206720A JP 20672088 A JP20672088 A JP 20672088A JP H0715121 B2 JPH0715121 B2 JP H0715121B2
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- JP
- Japan
- Prior art keywords
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- powder
- fine powder
- injection molding
- 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.)
- Expired - Fee Related
Links
- 239000000843 powder Substances 0.000 title claims description 110
- 229910045601 alloy Inorganic materials 0.000 title claims description 51
- 239000000956 alloy Substances 0.000 title claims description 51
- 229910017061 Fe Co Inorganic materials 0.000 title claims description 47
- 238000001746 injection moulding Methods 0.000 title claims description 25
- 239000000696 magnetic material Substances 0.000 title claims description 8
- 239000002245 particle Substances 0.000 claims description 47
- 238000005245 sintering Methods 0.000 claims description 24
- 239000002184 metal Substances 0.000 claims description 22
- 229910052751 metal Inorganic materials 0.000 claims description 22
- 229910052698 phosphorus Inorganic materials 0.000 claims description 17
- 238000000889 atomisation Methods 0.000 claims description 13
- 239000012535 impurity Substances 0.000 claims description 10
- 239000011230 binding agent Substances 0.000 claims description 8
- 229910000531 Co alloy Inorganic materials 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 238000004898 kneading Methods 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims 2
- 239000000463 material Substances 0.000 description 44
- 229910020516 Co—V Inorganic materials 0.000 description 24
- 150000001875 compounds Chemical class 0.000 description 14
- 230000004907 flux Effects 0.000 description 12
- 238000002347 injection Methods 0.000 description 12
- 239000007924 injection Substances 0.000 description 12
- 230000000694 effects Effects 0.000 description 11
- 239000000155 melt Substances 0.000 description 11
- 239000002994 raw material Substances 0.000 description 10
- 238000005275 alloying Methods 0.000 description 9
- 229910052799 carbon Inorganic materials 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 230000007423 decrease Effects 0.000 description 8
- 238000002844 melting Methods 0.000 description 7
- 230000008018 melting Effects 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 238000000465 moulding Methods 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000001513 hot isostatic pressing Methods 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 229910001339 C alloy Inorganic materials 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910000521 B alloy Inorganic materials 0.000 description 2
- 229910001096 P alloy Inorganic materials 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000005238 degreasing Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- FPVKHBSQESCIEP-JQCXWYLXSA-N pentostatin Chemical compound C1[C@H](O)[C@@H](CO)O[C@H]1N1C(N=CNC[C@H]2O)=C2N=C1 FPVKHBSQESCIEP-JQCXWYLXSA-N 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 238000009692 water atomization Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- LFYJSSARVMHQJB-QIXNEVBVSA-N bakuchiol Chemical compound CC(C)=CCC[C@@](C)(C=C)\C=C\C1=CC=C(O)C=C1 LFYJSSARVMHQJB-QIXNEVBVSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002056 binary alloy Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Description
【発明の詳細な説明】 〈産業上の利用分野〉 本発明は、高飽和磁束密度焼結材料用の原料として、金
属粉末の射出成形に好適で焼結性に優れたアトマイズFe
-Co合金微粉とFe-Co-V合金微粉および当該合金微粉を焼
結した高密度の焼結磁性材料に関する。DETAILED DESCRIPTION OF THE INVENTION <Industrial field of application> The present invention is suitable for injection molding of metal powder as a raw material for a high saturation magnetic flux density sintered material and has excellent sinterability.
-Co alloy fine powder, Fe-Co-V alloy fine powder, and high-density sintered magnetic material obtained by sintering the alloy fine powder.
〈従来の技術〉 Fe-CO系合金は、あらゆる磁性材料の中で最高の飽和磁
束密度を有する軟質磁性材料として知られている。換言
すると、Fe-Co系合金は、同一体積で他のいかなる磁性
材料よりも高い磁気エネルギを発揮できると言える。こ
の特徴をいかし、Fe-Co系合金は、小型でも高い磁気エ
ネルギの伝達が要求されるモータや磁性ヨークなどへの
応用が期待されている。ところが、溶製Fe-Co系合金
は、冷間加工性が劣悪であるため、小型部品の工業的な
製造がほとんど不可能であると言うジレンマを持ってい
る。<Prior Art> Fe-CO alloys are known as soft magnetic materials having the highest saturation magnetic flux density among all magnetic materials. In other words, it can be said that the Fe-Co based alloy can exhibit higher magnetic energy than any other magnetic material in the same volume. Taking advantage of this feature, Fe-Co alloys are expected to be applied to motors and magnetic yokes that require high magnetic energy transmission even if they are small. However, molten Fe-Co alloys have poor cold workability, and therefore have a dilemma that industrial production of small parts is almost impossible.
粉末治金法は、このような難加工性を克服する有力な手
段と考えられており、種々の方法が提案されている。The powder metallurgy is considered to be a powerful means for overcoming such difficult workability, and various methods have been proposed.
例えば、Fe-Co系焼結材料に関しては、特開昭61-291934
号公報、特開昭62-54041号公報、特開昭62-142750号公
報があり、Ｐを含有するFe-Co系焼結材料に関しては、
特公昭57-38663号（特開昭55-85649号）公報、Ｂを含有
するFe-Co系焼結材料に関しては特開昭55-85650号公報
がある。For example, regarding a Fe-Co based sintered material, JP-A-61-291934
JP-A-62-54041 and JP-A-62-142750, the Fe-Co based sintered material containing P is
JP-B-57-38663 (JP-A-55-85649) and JP-A-55-85650 concerning Fe-Co based sintered materials containing B are disclosed.
また、Fe-Co-V系焼結材料に関しては特開昭54-75410号
公報がある。Regarding the Fe-Co-V based sintered material, there is JP-A-54-75410.
ところが、従来提案されている方法は、いずれも圧縮成
形によるものであったため、圧縮性を阻害しない程度で
なおかつ圧縮プレスの金型で成形できるようにFe-Co合
金粉、Co-V合金粉、Fe-P合金粉、Fe-B合金粉とFe粉、Co
粉を配合した、いわゆる混合粉を使用しなければならな
いという制約があった。However, the methods proposed hitherto were all based on compression molding, so that Fe-Co alloy powder, Co-V alloy powder, so that they can be molded with a mold of a compression press to the extent that they do not impair compressibility, Fe-P alloy powder, Fe-B alloy powder and Fe powder, Co
There was a constraint that a so-called mixed powder containing powder must be used.
このため、従来の技術は、この制約に起因する低焼結密
度、低磁気特性の克服を目的とするものであった。特開
昭61-291934号公報では、規則格子を形成していない急
冷Fe-Co合金の利用による圧縮性の改善と、この急冷Fe-
Co合金粉とCo粉の配合による焼結性の改善がなされ、特
開昭62-54041号公報では、熱間等方圧加圧（HIP）によ
る焼結密度向上がなされ、特開昭62-142750号公報ではF
e-Co合金粗粉とCo微粉の組合せによる圧粉密度の改善と
焼結密度の向上により磁気特性の向上を図ったものであ
る。Therefore, the conventional technique aims at overcoming low sintering density and low magnetic properties due to this restriction. Japanese Patent Laid-Open No. 61-291934 discloses improvement of compressibility by using a quenched Fe-Co alloy that does not form an ordered lattice, and this quenched Fe-
Sinterability was improved by blending Co alloy powder and Co powder, and in JP-A-62-54041, the sintering density was improved by hot isostatic pressing (HIP). 142750 gazette F
This is intended to improve the magnetic properties by improving the green compact density and the sintering density by combining the e-Co alloy coarse powder and Co fine powder.
また、特公昭57-38663号（特開昭55-85649号）公報で
は、粉砕Fe-P合金（26.5％Ｐのフェロリン）粉をＰ含有
量で0.05〜0.7％になるように配合し、特開昭55-85650
号公報では、粉砕Fe-B合金（19.9％Ｂのフェロボロン）
粉をＢ含有量で0.1〜0.4％になるように配合して焼結
し、無添加のものより焼結密度を高め磁気特性の改善を
図ったものである。Further, in Japanese Patent Publication No. 57-38663 (Japanese Patent Laid-Open No. 55-85649), pulverized Fe-P alloy (ferroline of 26.5% P) powder is blended so that the P content is 0.05 to 0.7%. Kaisho 55-85650
In the gazette, ground Fe-B alloy (19.9% B ferroboron)
The powder is blended so that the B content is 0.1 to 0.4% and sintered, and the sintered density is increased to improve the magnetic characteristics as compared with the additive-free powder.
また、特開昭54-75410号公報に開示された焼結材料は、
38％Ｖの共晶組成を中心とした35〜45wt％のＶから成る
V-Co粉砕合金粉をFe粉、Co粉に配合して液相焼結し、Fe
-Co-V系焼結材料の焼結密度を高め磁気特性の向上を図
ったものである。Further, the sintered material disclosed in JP-A-54-75410,
Consists of 35 to 45 wt% V centered on 38% V eutectic composition
V-Co crushed alloy powder is mixed with Fe powder and Co powder, and liquid phase sintering is performed.
-This is to improve the magnetic characteristics by increasing the sintering density of the Co-V type sintered material.
〈発明が解決しようとする課題〉 しかしながら、これら従来の提案は、金型によりプレス
成形するもので、原料粉末が焼結性の低い粗粒各種の単
金属粉と二元系合金粉の混粉で、それら各種の粉末は製
造法がまちまちで、その粒度と粒子形状は個々別々であ
り、射出成形用には使用できないものである。<Problems to be Solved by the Invention> However, these conventional proposals are those in which press molding is performed by a die, and raw material powder is a mixed powder of various coarse single metal powders with low sinterability and binary alloy powders. The production methods of these various powders are different, and their particle sizes and particle shapes are different from each other and cannot be used for injection molding.
現在、Fe-Co系焼結材料は、材料歩留りの改善、機械加
工費の削減を目的として溶製Fe-Co系の一部に代替しつ
つある。特に、その成形方法においては、２次元的形状
しか成形できなかったプレス成形に代って、３次元複雑
形状が容易に成形できる射出成形の発展が期待されてい
る。ところが、射出成形を利用したFe-Co系焼結材料の
製造が開始されたのはごく最近であるため、種々の技術
課題が残されており、特に、原料粉末については、多く
の改良の余地がある。Currently, Fe-Co based sintered materials are being replaced with a part of ingot Fe-Co based materials for the purpose of improving material yield and reducing machining cost. In particular, in the molding method, it is expected that the development of injection molding capable of easily molding a three-dimensional complex shape will replace the press molding that can mold only a two-dimensional shape. However, since the production of Fe-Co based sintered materials using injection molding has been started only recently, various technical problems remain, and especially for raw material powder, there is much room for improvement. There is.
一般に、射出成形用の原料粉末としては、球状であるこ
と、微粒粉であることおよび還元可能な粒子表面酸化物
であることが要求される。球状粉末の利点は、粉末同士
のすべりが良好であることである。球状粉末と不規則形
状粉末とに同一種、同一量の有機バインダを添加して比
較すると、球状粉末を使用した方が低粘度となり、射出
性に優れることが知られている。さらに、同一射出性を
低バインダ量によって達成できるため、脱脂時間の短縮
が図れる利点がある。一方、粉末の微粒化と還元可能な
粒子表面酸化物であることによって高密度が達成でき
る。これらの粉末の要求特性を達成するために、アトマ
イズ法による粉末の製造においては、アトマイズ装置の
装置パラメータの変更によって対処される。しかし、原
料粉末の化学組成の変更による改良は行なわれておら
ず、プレス成形を前提とした原料粉末（平均粒径:80μ
ｍ程度）と同様の組成が採用されていた。すなわち、プ
レス形成時の圧縮性および成形性を阻害する不純物成分
を極力低減した化学組成が常用されいた。しかし、従来
組成の射出成形用微粉末（平均粒径:20μｍ以下）の球
状化と表面酸化物に対する知見が十分ではないため、射
出性および焼結性において必ずしも十分ではないのが問
題であった。In general, raw material powders for injection molding are required to be spherical, fine powders, and reducible particle surface oxides. The advantage of the spherical powder is that the powders slide well. It is known that, when the same kind and the same amount of the organic binder are added to the spherical powder and the irregularly shaped powder for comparison, the spherical powder has a lower viscosity and is excellent in injection property. Further, since the same injection property can be achieved with a low binder amount, there is an advantage that the degreasing time can be shortened. On the other hand, high density can be achieved by the atomization of the powder and the reduction of the particle surface oxide. In order to achieve the required properties of these powders, the production of powders by the atomization method is addressed by changing the device parameters of the atomizing device. However, no improvement was made by changing the chemical composition of the raw material powder, and the raw material powder (average particle size: 80μ
The same composition as that of (about m) was adopted. That is, a chemical composition in which an impurity component that impedes compressibility and moldability during press forming is reduced as much as possible has been commonly used. However, there is not enough knowledge about spheroidization and surface oxides of fine powder for injection molding (average particle size: 20 μm or less) of the conventional composition, so that it was not always sufficient in terms of injection property and sinterability. .
本発明は、上記従来技術の問題点を解決しようとするも
のであって、金属粉末の射出成形性に好適な球形状で、
かつ還元可能な表面酸化物から成る焼結性に優れた射出
成形用のFe-Co系合金微粉とFe-Co-V系合金微粉を提供す
るとともに、当該合金微粉を射出成形し、焼結し、必要
に応じHIP処理することによる磁気特性を持つ高飽和磁
束密度を有するFe-Co系焼結材料を提供することを目的
とするものである。The present invention is intended to solve the above problems of the prior art, in a spherical shape suitable for injection moldability of metal powder,
We also provide Fe-Co-based alloy fine powder and Fe-Co-V-based alloy fine powder for injection molding that are composed of reducible surface oxides and have excellent sinterability, and the alloy fine powder is injection molded and sintered. An object of the present invention is to provide a Fe-Co based sintered material having a high saturation magnetic flux density with magnetic properties by HIP treatment if necessary.
〈課題を解決するための手段〉 本発明者らは、焼結体の磁気的性質（磁束密度;Bs、最
大透磁率；μmax、保持力;Hc）を著しく阻害することな
く、粉末形状が射出成形用として適する球状となる、焼
結性の良い、粉末化学組成の探索によって、以下の知見
を知り本発明に至った。<Means for Solving the Problems> The present inventors have confirmed that the powder shape is injected without significantly impairing the magnetic properties (magnetic flux density; Bs, maximum magnetic permeability; μmax, coercive force; Hc) of the sintered body. Through the search for a powder chemical composition which has a spherical shape suitable for molding and has good sinterability, the following knowledge was found and the present invention was achieved.
（１）C:1.00wt％以下、Si:1.00wt％以下、Mn:2.00wt％
以下で、かつMn/Siが1.00以上のFe-Co、Fe-Co-V溶湯を
アトマイズすることにより、平均粒径が20μｍ以下の射
出成形に好適な粒子形状を持ち、かつ焼結性に優れた表
面（酸化物）から成るFe-Co、Fe-Co-V微粉を製造でき
る。したがって当該合金微粉を焼結すると相対密度（真
密度に対する密度比）が92％以上で閉空孔から成る、Ｃ
が0.02wt％以下の磁気特性に優れた焼結材料を得ること
ができる。(1) C: 1.00 wt% or less, Si: 1.00 wt% or less, Mn: 2.00 wt%
By atomizing Fe-Co and Fe-Co-V melts with Mn / Si of 1.00 or more, the average particle size is 20 μm or less, which has a particle shape suitable for injection molding, and has excellent sinterability. It is possible to produce Fe-Co and Fe-Co-V fine powders having different surfaces (oxides). Therefore, when the alloy fine powder is sintered, the relative density (density ratio to the true density) is 92% or more, and it is composed of closed pores.
It is possible to obtain a sintered material having a magnetic property of 0.02 wt% or less and excellent magnetic properties.
（２）Ｂが0.02〜1.00wt％、Ｐが0.05〜1.00wt％のうち
１種または２種を上記溶湯に合金してアトマイズするこ
にとより、平均粒径が20μｍ以下の当該合金粉の見掛密
度、タップ密度の向上と、焼結密度の増加にともなった
Ｃが0.02wt％以下の磁気特性の向上が達成できる。(2) By alloying one or two of B of 0.02 to 1.00 wt% and P of 0.05 to 1.00 wt% with the molten metal and atomizing the molten alloy, the alloy powder having an average particle size of 20 μm or less is prepared. It is possible to improve the apparent density and tap density, and to improve the magnetic properties of C of 0.02 wt% or less with the increase of the sintering density.
すなわち、本発明の第１の態様は、C:1.00wt％以下、S
i:1.00wt％以下、Mn:2.00wt％以下でMn/Siが1.00以上、
Co:15〜60wt％、不純物を除き残部が実質的にFeの溶湯
をアトマイズ法で粉末化してなり、平均粒径が20μｍ以
下の球状粉であることを特徴とする射出成形用Fe-Co系
合金微粉を提供するものである。That is, the first aspect of the present invention is C: 1.00 wt% or less, S
i: 1.00 wt% or less, Mn: 2.00 wt% or less, Mn / Si is 1.00 or more,
Co: 15-60 wt%, Fe-Co system for injection molding characterized by being a spherical powder with an average particle size of 20 μm or less, which is formed by atomizing a molten metal of which balance is substantially Fe except impurities. It is intended to provide fine alloy powder.
また、本発明の第２の態様は、C:1.00wt％以下、Si:1.0
0wt％以下、Mn:2.00wt％以下でMn/Siが1.00以上、V:1.0
〜4.0wt％、Co:15〜60wt％、不純物を除き残部が実質的
にFeの溶湯をアトマイズ法で粉末化してなり、平均粒径
が20μｍ以下の球状粉であることを特徴とする射出成形
用Fe-Co系合金微粉を提供するものである。The second aspect of the present invention is C: 1.00 wt% or less, Si: 1.0
0 wt% or less, Mn: 2.00 wt% or less, Mn / Si is 1.00 or more, V: 1.0
~ 4.0wt%, Co: 15 ~ 60wt%, except the impurities, the balance is substantially Fe molten metal powdered by atomization method, which is a spherical powder with an average particle size of 20μm or less A fine powder of Fe-Co alloy for use is provided.
また、本発明の第３の態様は、C:1.00wt％以下、Si:1.0
0wt％以下、Mn:2.00wt％以下でMn/Siが1.00以上、B:0.0
2〜1.00wt％およびP:0.05〜1.00wt％のうちの１種また
は２種、Co:15〜60wt％、不純物を除き残部が実質的にF
eの溶湯をアトマイズ法で粉末化してなり、平均粒径が2
0μｍ以下の球状粉であることを特徴とする射出成形用F
e-Co系合金微粉を提供するものである。The third aspect of the present invention is C: 1.00 wt% or less, Si: 1.0
0 wt% or less, Mn: 2.00 wt% or less, Mn / Si is 1.00 or more, B: 0.0
1 to 2 of 2 to 1.00 wt% and P: 0.05 to 1.00 wt%, Co: 15 to 60 wt%, the balance being substantially F except impurities.
The molten metal of e is atomized by the atomization method and has an average particle size of 2
Injection molding F characterized by being a spherical powder of 0 μm or less
It provides fine powder of e-Co alloy.
また、本発明の第４の態様は、C:1.00wt％以下、Si:1.0
0wt％以下、Mn:2.00wt％以下でMn/Siが1.00以上、V:1.0
〜4.0wt％、B:0.02〜1.00wt％およびP:0.05〜1.00wt％
のうちの１種または２種、Co:15〜60wt％、不純物を除
き残部が実質的にFeの溶湯をアトマイズ法で粉末化して
なり、平均粒径が20μｍ以下の球状粉であることを特徴
とする射出成形用Fe-Co系合金微粉を提供するものであ
る。The fourth aspect of the present invention is C: 1.00 wt% or less, Si: 1.0
0 wt% or less, Mn: 2.00 wt% or less, Mn / Si is 1.00 or more, V: 1.0
~ 4.0wt%, B: 0.02-1.00wt% and P: 0.05-1.00wt%
One or two of them, Co: 15-60wt%, except for impurities, the balance is substantially Fe, and it is made into powder by atomization method, and it is a spherical powder with an average particle size of 20μm or less. A fine powder of Fe-Co alloy for injection molding is provided.
さらに、本発明の第５の態様は、前記本発明の第１〜第
４の態様のいずれかの射出成形用Fe-Co系合金微粉を有
機バインダーに混練して射出成形を行い、その成形品を
焼結してなる、Ｃ含有率が0.02wt％以下で、真密度に対
する密度比が92％以上であることを特徴とするFe-Co系
焼結磁性材料を提供するものである。Further, a fifth aspect of the present invention is to perform injection molding by kneading the Fe-Co based alloy fine powder for injection molding according to any one of the first to fourth aspects of the present invention with an organic binder, and performing the injection molding. The present invention provides a sintered Fe-Co magnetic material having a C content of 0.02 wt% or less and a density ratio to the true density of 92% or more.
以下に、本発明をさらに詳細に説明する。Hereinafter, the present invention will be described in more detail.
先ず、本発明の第１〜第４の態様に示す射出成形用のFe
-Co系合金微粉およびFe-Co-V系合金微粉の溶湯に具備す
べき限定理由について説明する。First, Fe for injection molding shown in the first to fourth aspects of the present invention
The reasons for limitation in the molten metal of the -Co alloy fine powder and the Fe-Co-V alloy fine powder will be described.
微粉末の球状化の程度を評価するために、タップ密
度、見掛け密度およびコンパウンド粘度との関係を
調べた。、によって、粉末の充填性よりその球状性
を知ることができる。また、は、射出性の観点から直
接要求される特性であり、コンパウンドの滑り易さより
その球状性を知ることができる。In order to evaluate the degree of spheroidization of the fine powder, the relationship with tap density, apparent density and compound viscosity was investigated. , The spherical shape can be known from the filling property of the powder. Further, is a property directly required from the viewpoint of injection property, and its spherical shape can be known from the slipperiness of the compound.
Mnの含有量を2.00wt％以下に限定する理由は以下の
通りである。The reason for limiting the Mn content to 2.00 wt% or less is as follows.
Fe-Co系およびFe-Co-V系の溶湯において、Mn量を増加す
ると、アトマイズ時の粒子表面に低融点のMnO-FeOが生
成し、凝固するまでに粒子表面層の融点の低下、表面張
力の増加、粘性の低下によってアトマイズ粒子の球状化
を促進する作用があるが、2.00wt％を超えると、その焼
結材料の飽和磁束密度がFe単味焼結材料のそれより低下
するので、Mnを2.00wt％以下に限定する。In the Fe-Co and Fe-Co-V melts, when the amount of Mn is increased, low melting point MnO-FeO is generated on the particle surface during atomization, and the melting point of the particle surface layer decreases until solidification. Although it has an action of promoting the spheroidization of atomized particles by increasing the tension and decreasing the viscosity, when it exceeds 2.00 wt%, the saturation magnetic flux density of the sintered material becomes lower than that of Fe plain sintered material, Mn is limited to 2.00 wt% or less.
Ｃの含有量を1.00wt％以下に限定する理由は以下の
通りである。The reason for limiting the C content to 1.00 wt% or less is as follows.
通常、Fe-Co、Fe-Co-V系の高飽和磁束密度焼結材料にお
いては、磁気特性の観点から、含有炭素量を極力低く抑
える必要がある。また、プレス成形を利用して製造され
るFe-Co、Fe-Co-V系焼結材料の原料粉末においては、磁
気特性の観点に加えて、プレス成形時の圧縮性の観点か
ら、溶製材以上に含有炭素の軽減が要求される。しか
し、射出成形法を利用してFe-Co、Fe-Co-V系焼結材料を
製造する場合は、いくら低炭素の原料粉末を使用して
も、加工性の観点では射出成形性を向上させることはな
く、磁気特性の観点でも、脱脂時に有機バインダに起因
する炭素によって汚染されるため、利点がないことが判
った。さらに、真空中で焼結することによって、原料粉
末に起因する炭素も、有機バインダに起因する炭素も、
同様に除去できることが判った。Usually, in a Fe-Co or Fe-Co-V based high saturation magnetic flux density sintered material, it is necessary to keep the contained carbon content as low as possible from the viewpoint of magnetic characteristics. In addition, in the raw material powder of Fe-Co and Fe-Co-V based sintered materials manufactured by press molding, in addition to the magnetic properties, in addition to the compressibility during press molding, the ingot material As mentioned above, reduction of carbon content is required. However, when manufacturing Fe-Co and Fe-Co-V based sintered materials using the injection molding method, no matter how low carbon raw material powder is used, the injection moldability is improved from the viewpoint of processability. From the viewpoint of magnetic properties as well, it was found that there is no advantage from the viewpoint of magnetic properties because carbon is contaminated by the organic binder during degreasing. Furthermore, by sintering in a vacuum, both carbon originating from the raw material powder and carbon originating from the organic binder,
It turns out that it can be removed as well.
そこで、粉末の含有する炭素を低減するのではなく、む
しろ、増加させることによって、粉末特性の改良を試み
た。その結果、炭素量の付加は、高圧媒体を利用したア
トマイズ微粉末の充填性を改良する（球状化する）こと
を実験によって見出した。Therefore, an attempt was made to improve the powder characteristics by increasing the carbon content of the powder rather than decreasing it. As a result, it was found by an experiment that addition of carbon content improves (spheroidizes) the filling property of atomized fine powder using a high-pressure medium.
これは、Fe-Co、Fe-Co-V系の溶湯へのＣの合金化により
溶湯中酸素量の低下にともない、溶湯粘度の低下および
融点低下によってアトマイズ粒子は球状化するものと考
えられる。It is considered that the atomized particles are spheroidized due to the decrease of the melt viscosity and the melting point as the oxygen content in the melt decreases due to the alloying of C into the Fe-Co and Fe-Co-V melts.
例えば、第１表に示す1000kgf/cm2の水圧のもとで噴射
した円環状の水ジエットで水アトマイズした平均粒径が
9.0〜10.0μｍのFe-50％Co微粉について、Ｃ合金量が増
加するに伴って見掛密度およびタップ密度の上昇がみら
れ、粉末が球状化したことが判る。For example, the average particle size of water atomized with a circular water jet injected under the water pressure of 1000 kgf / cm 2 shown in Table 1 is
With respect to the Fe-50% Co fine powder having a particle size of 9.0 to 10.0 μm, the apparent density and the tap density increased as the amount of C alloy increased, and it was found that the powder was spherical.
さらに、原料粉末とバインダーとの比率が等しいコンパ
ウンドについても、Fe-50％Co微粉のＣ合金量の増加に
伴って、コンパウンドの粘性温度の低下効果が見られ
る。Further, even for a compound in which the ratio of the raw material powder and the binder is equal, the effect of lowering the viscous temperature of the compound is observed as the amount of C alloy of Fe-50% Co fine powder increases.
しかし、Fe-50％Co微粉のＣ合金量が1.00wt％を超える
と、焼結材料の磁気特性上の観点から、その溶湯合金量
が限定されるSi、Mnの脱酸限よりＣ−Ｏ反応による脱酸
限が低くなり、アトマイズ粒子はCOガスを捕捉した中空
粒子が生成するようになり、見掛密度およびタップ密度
はかえて低下し、コンパウンドの粘性温度は著しく増大
する。However, if the amount of C alloy in Fe-50% Co fine powder exceeds 1.00 wt%, from the viewpoint of the magnetic properties of the sintered material, the amount of molten alloy is limited, and the amount of C-O is deoxidized from the deoxidation limit of Si and Mn. The deoxidation limit due to the reaction becomes low, and the atomized particles become hollow particles trapping CO gas, the apparent density and tap density decrease instead, and the viscous temperature of the compound increases remarkably.
また、このコンパウンドを工業的に通常採用される、焼
結最大時間である4h程度の真空焼結を施した焼結体のＣ
含有量を0.02wt％以下に低減できないため、磁気特性の
劣悪化をきたすので、Fe-CoおよびFe-Co-V系合金溶湯の
合金Ｃ量を1.00wt％以下に限定する。In addition, the C of a sintered body that has been vacuum-sintered for about 4 hours, which is the maximum sintering time, which is usually adopted industrially, is used for this compound.
Since the content cannot be reduced to 0.02 wt% or less, the magnetic properties are deteriorated. Therefore, the alloy C content of the Fe-Co and Fe-Co-V alloy melts is limited to 1.00 wt% or less.
Si:1.00wt％以下、Mn:2.00wt％以下でMn/Siが1.00
以上に限定する理由は以下の通りである。Si: 1.00 wt% or less, Mn: 2.00 wt% or less, Mn / Si is 1.00
The reason for limiting the above is as follows.
SiおよびMnは、Fe-Co系およびFe-Co-V系焼結材料の飽和
磁束密度がFe単味焼結材料のそれより高い値を示す範
囲、即ちSiが1.00wt％以下、Mnが2.00wt％以下に限定し
た。Si and Mn are in a range where the saturation magnetic flux density of the Fe-Co and Fe-Co-V based sintered materials is higher than that of the Fe-only sintered material, that is, Si is 1.00 wt% or less and Mn is 2.00%. Limited to wt% or less.
ここで例えば、第１表に示す当該溶湯を水アトマイズし
た合金微粉において、Mn/Siが1.00以上のとき、見掛密
度およびタップ密度が増大し、コンパウンドの粘性温度
が低下することから微粉末が球状化したことが判る。Here, for example, in the alloy fine powder obtained by water atomizing the molten metal shown in Table 1, when Mn / Si is 1.00 or more, the apparent density and the tap density increase, and the viscous temperature of the compound decreases, so the fine powder is It can be seen that it has become spherical.
また、Mn/Siが1.00以上のとき、焼結密度が増大し、焼
結性の良い表面状態になったことが判る。Further, it can be seen that when Mn / Si is 1.00 or more, the sintering density is increased and the surface state has good sinterability.
よってMn/Siを1.00以上に限定する。Therefore, Mn / Si is limited to 1.00 or more.
これは、溶湯のMn量を増加すると、アトマイズ時の粒子
表面に低融点のMnOが生成し、凝固するまでに粒子表面
層の融点の低下、表面張力の増加、粘性の低下によって
アトマイズ粒子が球状化するものと考えられる。またMn
Oは、工業的に通常採用される焼結温度である1400℃程
度の真空焼結であれば、コンパウンド中のＣまたは溶湯
合金ＣによってCO還元され、焼結を阻害しない。This is because when the amount of Mn in the molten metal is increased, low melting point MnO is generated on the particle surface during atomization, and the atomizing particles become spherical due to the lowering of the melting point of the particle surface layer, the increase of the surface tension, and the lowering of the viscosity until they solidify. It is thought that it will change. Also Mn
If vacuum sintering is carried out at a sintering temperature of about 1400 ° C., which is the industrially adopted sintering temperature, O is reduced by CO by the C in the compound or the molten alloy C and does not hinder the sintering.
これに対し、Siは、アトマイズ時に粒子表面に粘稠なSi
O2を生成して粒子を不規則状化し、SiO2は1400℃程度の
真空中ではＣによるCO還元が困難なため焼結を阻害す
る。On the other hand, Si is a viscous Si on the particle surface during atomization.
O 2 is generated to make the particles irregular, and SiO 2 hinders sintering because it is difficult to reduce CO with C in a vacuum of about 1400 ° C.
よって、アトマイズ時の粒子の球状化と焼結性の良い粒
子表面を得るために溶湯にのMn/Siを1.00以上に限定す
る。Therefore, the Mn / Si content in the molten metal is limited to 1.00 or more in order to obtain spherical particles and a surface of the particles having good sinterability during atomization.
Co:15〜60wt％に限定する理由は以下の通りであ
る。The reason for limiting Co: 15 to 60 wt% is as follows.
Coは、溶製材の場合と同様に、Feに置換することによっ
て飽和磁束密度（Bs）を向上させる効果がある。但し、
Co量が15wt％に満たない場合や、60wt％を超える場合
は、その効果が小さいため、Co量を15〜60wt％に限定し
た。Co has the effect of improving the saturation magnetic flux density (Bs) by substituting Fe, as in the case of the ingot material. However,
When the Co amount is less than 15 wt% or exceeds 60 wt%, the effect is small, so the Co amount is limited to 15 to 60 wt%.
以上の成分限定により本発明のFe-Co系合金微粉は構成
されるが、さらに以下の成分を含有せしめることにより
さらに効果を上げることができる。Although the Fe-Co based alloy fine powder of the present invention is constituted by the above component limitation, the effect can be further enhanced by further containing the following components.
V:1.0〜4.0wt％に限定する理由は以下の通りであ
る。The reason for limiting V: 1.0 to 4.0 wt% is as follows.
Ｖは、溶製材の場合と同様に、焼結材料の固有抵抗を上
昇させる効果があり、1.0wt％未満ではその効果が小さ
く、4.0wt％を超えるとHCが急増し軟磁性が劣化するた
め1.0〜4.0wt％に限定する。V has the effect of increasing the specific resistance of the sintered material, as in the case of the ingot material. If it is less than 1.0 wt%, the effect is small, and if it exceeds 4.0 wt%, HC increases rapidly and the soft magnetism deteriorates. Limited to 1.0-4.0wt%.
尚、Ｖを合金した溶湯は、タンディッシュノズルに溶湯
温度低下によるV2O3を生成析出してノズル閉塞を起こす
が、Ｃ、Si、Mnを溶湯に添加してタンディッシュノズル
を通過時の溶湯温度で平衡するＶ−Ｏ脱酸限以下に調整
することによって、このノズル閉塞を防止することが可
能である。It should be noted that the melt alloyed with V forms V 2 O 3 in the tundish nozzle due to the temperature decrease of the melt and deposits to cause nozzle clogging, but when C, Si, and Mn are added to the melt, it passes through the tundish nozzle. It is possible to prevent this nozzle blockage by adjusting the V-O deoxidation limit equal to or lower than the equilibrium at the melt temperature.
この意味からも、C;1.00wt％以下、Si;1.00wt％以下お
よびMnを2.00wt％以下で複合して溶湯に合金化すること
はアトマイズ粉製造上の経済性にも有益なものである。From this point of view, compounding C; 1.00 wt% or less, Si; 1.00 wt% or less, and Mn in 2.00 wt% or less and alloying into a molten metal is also beneficial to the economical efficiency in producing atomized powder. .
以下の成分添加により、さらに優れたFe-Co系合金微粉
とすることがきる。By adding the following components, it is possible to obtain further excellent Fe-Co alloy fine powder.
B:0.02〜1.00wt％およびP:0.05〜1.00wt％に限定す
る理由は以下の通りである。The reason for limiting to B: 0.02 to 1.00 wt% and P: 0.05 to 1.00 wt% is as follows.
ＢおよびＰは、それぞれ単独であるいは複合して溶湯に
添加合金することによって、アトマイズ粒子を球状化さ
せる効果があるが、Ｂは0.02wt％未満、Ｐは0.05wt％未
満ではその効果が小さく、ＢおよびＰともに1.00wt％を
越えると焼結材料の磁気特性とくにμmaxとHcが劣化す
るため、Ｂは0.02〜1.00wt％、Ｐは0.05〜1.00wt％に限
定する。B and P have the effect of making the atomized particles spherical by adding and alloying them individually or in combination to the molten metal, but if B is less than 0.02 wt% and P is less than 0.05 wt%, the effect is small, When both B and P exceed 1.00 wt%, the magnetic properties of the sintered material, particularly μmax and Hc, deteriorate, so B is limited to 0.02 to 1.00 wt%, and P is limited to 0.05 to 1.00 wt%.
なお、ＢおよびＰの溶湯への合金化によるアトマイズ時
の粒子の球状化効果は、Mnの場合と同様に、粒子表面に
生成するＢ酸化物、Ｐ酸化物による融点の低下、表面粘
度の低下によるものであり、焼結密度が増大するのはＢ
およびＰの合金化による拡散促進効果によるものであ
り、粒子表面の多過ぎるＢ酸化物およびＰ酸化物が焼結
を阻害すると推察できる。The effect of spheroidizing the particles during atomization by alloying B and P into the molten metal is similar to that of Mn, lowering the melting point and lowering the surface viscosity due to the B oxides and P oxides generated on the particle surface. The increase in the sintered density is due to B
This is due to the diffusion-promoting effect of alloying P and P, and it can be inferred that too much B oxide and P oxide on the particle surface hinders sintering.
平均粒径を20μｍ以下に限定する理由は以下の通り
である。The reason for limiting the average particle size to 20 μm or less is as follows.
第１表に示すように、当該合金微粉を用いた最終焼結材
料の密度および磁気特性は、当該合金微粉の平均粒径の
影響を強く受ける。平均粒径が20μｍを越えると焼結密
度比が92％以上の閉空孔から成る焼結材料を製造でき
ず、磁気特性（Bs、μmax、Hc）の著しい劣化をきたす
ので、平均粒径は20μｍ以下に限定する。As shown in Table 1, the density and magnetic properties of the final sintered material using the alloy fine powder are strongly influenced by the average particle size of the alloy fine powder. If the average particle size exceeds 20 μm, a sintered material consisting of closed pores with a sintering density ratio of 92% or more cannot be manufactured, and the magnetic properties (Bs, μmax, Hc) will deteriorate significantly, so the average particle size is 20 μm. Limited to:
本発明のFe-Co系合金微粉は基本的には以上のように構
成されるものであり、以下に、Fe-Co系焼結磁性材料に
ついて詳細に説明する。The Fe-Co based alloy fine powder of the present invention is basically configured as described above, and the Fe-Co based sintered magnetic material will be described in detail below.
次に当該Fe-Co系合金微粉およびFe-Co-V系合金微粉を焼
結した高磁束密度焼結材料に具備すべき限定理由につい
て説明する。Next, the reasons for limitation that the high magnetic flux density sintered material obtained by sintering the Fe-Co alloy fine powder and the Fe-Co-V alloy fine powder should be described.
焼結材料のＣの含有率を0.02wt％以下に限定する理
由は以下の通りである。The reason for limiting the C content of the sintered material to 0.02 wt% or less is as follows.
不純物であるＣの存在は、磁気特性とくにμmaxとHcに
悪影響を及ぼす。Ｃ量が0.02wt％を越えるとμmaxおよ
びHcの著しい劣化をきたすので、Ｃは0.02wt％以下に限
定する。The presence of C, which is an impurity, adversely affects the magnetic properties, particularly μmax and Hc. If the amount of C exceeds 0.02 wt%, μmax and Hc are significantly deteriorated, so C is limited to 0.02 wt% or less.
相対焼結密度比を92％以上に限定する理由は以下の
通りである。The reason for limiting the relative sintered density ratio to 92% or more is as follows.
相対焼結密度比は、焼結材料の磁束密度（Bs）、最大透
磁率（μmax）および保持力（Hc）に影響を及ぼす重要
な特性値である。The relative sintered density ratio is an important characteristic value that affects the magnetic flux density (Bs), the maximum magnetic permeability (μmax) and the coercive force (Hc) of the sintered material.
相対焼結密度比は92％未満のとき、Bs、μmaxおよびHc
ともに著しい劣化をきたす。When the relative sintered density ratio is less than 92%, Bs, μmax and Hc
Both cause remarkable deterioration.
これは、第１図に示すようにHIPによる密度上昇実験に
よると、相対焼結密度比が92％未満で密度上昇しないこ
とから、この場合は開空孔から成るためである。This is because, according to the density increase experiment by HIP as shown in FIG. 1, the relative sintered density ratio is less than 92% and the density does not increase, and in this case, it is composed of open pores.
したがって、閉空孔からなる焼結材料であるためには相
対焼結密度比は92％以上に限定する。Therefore, the relative sintering density ratio is limited to 92% or more in order to use a sintered material having closed pores.
〈実施例〉 以下に、本発明を実施例に基づいて具体的に説明する。<Examples> The present invention will be specifically described below based on Examples.
第１表に、水アトマイズ法で製造した高飽和磁束密度焼
結材料用のFe-Co系、Fe-Co-V系の合金微粉と当該合金微
粉を焼結して作製した高密度の高飽和磁束密度焼結材料
の本発明例を比較例とともに示す。Table 1 shows Fe-Co and Fe-Co-V alloy fine powders for high saturation magnetic flux density sintered materials produced by the water atomizing method and high-density high saturation produced by sintering the alloy fine powders. The present invention example of the magnetic flux density sintered material will be shown together with a comparative example.
高周波誘導電気溶解炉で溶製したFe-Co系、Fe-Co-V系の
溶湯をタンディッシュ底の耐火材製の細孔ノズルから鉛
直下に流下注入し、そのまわりから1000kgf/cm2の水圧
をかけて下すぼまり形の円環状の水ジェットを噴射して
水アトマイズして第１表に示す種々の化学組成を持つFe
-Co系、Fe-Co-V系の合金微粉を作製した。マイクロトラ
ック粒度分析計により平均粒径（微粒側から累積体積が
50％となる粒径）、見掛密度およびタップ密度を測定し
た。Fe-Co and Fe-Co-V melts melted in a high-frequency induction melting furnace are vertically injected from a refractory micropore nozzle at the bottom of the tundish, and 1000 kgf / cm 2 around it. Fe with various chemical compositions shown in Table 1 by atomizing the water by jetting a water jet in the shape of a downward constriction under water pressure
-Co-based and Fe-Co-V-based alloy fine powders were prepared. The average particle size (accumulated volume from the fine particle side
The particle size of 50%), the apparent density and the tap density were measured.
次に、これらの合金微粉と46vol％のワックス系の有機
バインダーとを加圧型ニーダーにより混練してコンパウ
ンドを作製し、フローテスターにより荷重10kgのもと直
径が1mmで長さ1mmのダイにより粘度（100P［ポアズ］と
なる温度）を測定した。Next, fine particles of these alloys and 46 vol% of a wax-based organic binder are kneaded with a pressure kneader to prepare a compound, and a flow tester produces a compound having a diameter of 1 mm and a length of 1 mm under a load of 10 kg. The temperature at which 100 P [poise] is reached was measured.
次に、射出成形機を用い、射出温度150度で外径53mm、
内径41mm、高さ4.7mmのリング状に成形した。射出成形
体は、窒素中、＋7.5℃/hで600℃まで昇温後30min保持
して脱脂処理を行った。続いて、水素中、＋５℃/minの
昇温し、700℃で1h保持、950℃で1h保持の後、1350℃で
2hの保持により焼結を行った。また、950℃での保持終
了までは、露点＋30℃に保ち、その後は露点−20℃以下
に制御した。得られた焼結体は、水中法重量測定法によ
り、密度比を求めた。また、同条件で作製した試料に、
捲線を施した後、自記磁束計によって磁気特性を求め
た。結果を第１表に示す。Next, using an injection molding machine, at an injection temperature of 150 degrees, an outer diameter of 53 mm,
It was molded into a ring shape with an inner diameter of 41 mm and a height of 4.7 mm. The injection-molded body was degreased by holding it at + 7.5 ° C / h to 600 ° C in nitrogen and holding it for 30 minutes. Then, in hydrogen, increase the temperature by + 5 ℃ / min, hold at 700 ℃ for 1h, hold at 950 ℃ for 1h, and then at 1350 ℃.
Sintering was performed by holding for 2 hours. In addition, the dew point was maintained at + 30 ° C until the end of the holding at 950 ° C, and then the dew point was controlled at -20 ° C or lower. The density ratio of the obtained sintered body was determined by an underwater weighing method. In addition, for samples prepared under the same conditions,
After winding, the magnetic characteristics were determined by a self-recording magnetometer. The results are shown in Table 1.
第１表の実施例記号１〜18から明らかのように、Mn:2.0
0wt％以下、およびC;1.00wt％以下、Si;1.00wt％以下、
Mn;2.00wt％以下で、Mn/Siが1.00以上のCo;10〜60wt％
の平均粒径が20μｍ以下の本発明Fe-Co系合金微粉にお
いて、MnおよびMn/Siの増加に伴なって、またＣの増加
に伴なって見掛密度およびタップ密度が大きな値を示
し、そのコンパウンドの粘度も低い（低温ほど低粘度で
ある）値を示し、粉末が球状化し、射出成形性に優れて
いることが判る。また、焼結体Ｃ量も0.02wt％以下、相
対焼結密度比も95％を示し、その磁気特性（Bs、μma
x、Hc）の優れた焼結材料を得ることができる。 As is clear from the example symbols 1 to 18 in Table 1, Mn: 2.0
0 wt% or less, and C; 1.00 wt% or less, Si; 1.00 wt% or less,
Mn; 2.00 wt% or less, Mn / Si 1.00 or more Co; 10-60 wt%
In the Fe-Co alloy fine powder of the present invention having an average particle size of 20 μm or less, the apparent density and the tap density show large values with the increase of Mn and Mn / Si, and with the increase of C, It can be seen that the viscosity of the compound also shows a low value (the lower the temperature, the lower the viscosity), and the powder is spherical and has excellent injection moldability. Also, the amount of sintered C is 0.02 wt% or less, and the relative sintered density ratio is 95%, and its magnetic characteristics (Bs, μma
It is possible to obtain a sintered material having excellent x, Hc).
第１表の実施例記号19〜23から明らかのように、V;1.0
〜4.0wt％の本発明Fe-Co-V系合金微粉において、Ｖの溶
湯への合金化によって、溶湯ノズル閉塞防止上の観点か
らSi量、Mn量を増加させMn/Si≧1.00とすることによっ
て、球状化した射出成形性に優れたアトマイズ粉末を製
造できる。また、焼結体Ｃ量が0.01wt％で、相対焼結密
度比は95％を示し、その磁気特性（Bs、μmax、Hc）の
優れた焼結材料を得ることができる。As is clear from Example symbols 19 to 23 in Table 1, V; 1.0
In the Fe-Co-V alloy fine powder of the present invention of up to 4.0 wt%, by alloying V into a molten metal, the amounts of Si and Mn are increased from the viewpoint of preventing clogging of the molten metal nozzle so that Mn / Si ≧ 1.00. This makes it possible to produce atomized powder which is spherical and has excellent injection moldability. Further, when the amount of the sintered body C is 0.01 wt% and the relative sintered density ratio is 95%, a sintered material having excellent magnetic characteristics (Bs, μmax, Hc) can be obtained.
第１表の実施例記号24〜33から明らかのように、B;0.02
〜1.00wt％、P;0.05〜1.00wt％の本発明のFe-Co系およ
びFe-Co-V系合金微粉において、Ｂおよび／またはＰの
合金化によって見掛密度およびタップ密度が高い値を示
し、そのコンパウンドの粘度も低い値を示し、Ｂおよび
Ｐ無添加の場合（実施例記号３）より球状化し、射出成
形性も一段と向上することが判る。また、焼結体Ｃ量が
0.01wt％で、相対焼結密度比も96％と緻密化が一段と進
み、磁気特性（Bs、μmax、Hc）も一段と優れた焼結材
料が得られる。As is clear from the example symbols 24-33 in Table 1, B; 0.02
In the Fe-Co-based and Fe-Co-V-based alloy fine powders of the present invention of ˜1.00 wt%, P: 0.05-1.00 wt%, a high apparent density and a high tap density are obtained by alloying B and / or P. It can be seen that the viscosity of the compound also shows a low value, spheroidization is made more than in the case where B and P were not added (Example symbol 3), and the injection moldability was further improved. In addition, the amount of sintered body C
With 0.01 wt%, the relative sintering density ratio was 96%, and the densification was further advanced, and a sintered material with even better magnetic properties (Bs, μmax, Hc) was obtained.
第１表の実施例記号34〜43から明らかのように、平均粒
径が20μｍ以下の本発明Fe-Co系合金微粉において、平
均粒径が大きくなるにしたがって、当該合金微粉の見掛
密度およびタップ密度は高い値を示し、そのコンパウン
ドの粘度は低い値になるが相対焼結密度比が低下し、磁
気特性（Bs、μmax、Hc）も低下してくる。As is clear from the example symbols 34 to 43 in Table 1, in the Fe-Co alloy fine powder of the present invention having an average particle diameter of 20 μm or less, as the average particle diameter increases, the apparent density of the alloy fine powder and The tap density shows a high value, the viscosity of the compound becomes a low value, but the relative sintering density ratio decreases, and the magnetic properties (Bs, μmax, Hc) also decrease.
Fe-Co-V系合金微粉においても同様のことが言える。The same applies to the Fe-Co-V alloy fine powder.
平均粒径が20μｍ以下のとき、磁気特性の優れた焼結材
料を得ることができる。When the average particle size is 20 μm or less, a sintered material having excellent magnetic properties can be obtained.
第１図は、第１表の本発明実施例記号３のFe-Co系合金
微粉を用いたコンパウンドを射出成形し、1200〜1350℃
で2h水素中で焼結を行った焼結材料について1350℃で1h
Ar中で100kgf/cm2の圧力でHIP処理した際の焼結材料の
相対密度比とHIP処理後の相対密度比の関係を示す。こ
れから明かのように、焼結材料の相対密度比が92％以上
で閉空孔となり、HIP処理後の相対密度比が一段と向上
することが判る。FIG. 1 shows that the compound using the Fe-Co based alloy fine powder of Example symbol 3 of the present invention in Table 1 was injection-molded and the temperature was 1200 to 1350 ° C.
Sintered material sintered in hydrogen for 2h at 1350 ℃ for 1h
The relationship between the relative density ratio of the sintered material when HIPing at 100 kgf / cm 2 in Ar and the relative density ratio after HIPing is shown. As is clear from this, when the relative density ratio of the sintered material is 92% or more, closed pores are formed, and the relative density ratio after HIP treatment is further improved.
〈発明の効果〉 以上、詳述したように、本発明によれば、Fe-Co系およ
びFe-Co-V系の合金溶湯にC;1.00wt％以下、Si;1.00wt％
以下、Mn;2.00wt％以下でMn/Si≧1.00となるように成分
調整した溶湯をアトマイズして平均粒径が20μｍ以下の
微粉末とすることによって、球状化を図って射出成形性
と焼結性を改善したFe-Co系合金微粉を提供できるとと
もに、当該微粉末を用いることにより、相対密度比が92
％以上の焼結材料を提供することができる。<Effects of the Invention> As described above in detail, according to the present invention, C; 1.00 wt% or less, Si; 1.00 wt% in the molten Fe-Co and Fe-Co-V alloys
Below, by atomizing the molten metal whose components have been adjusted to satisfy Mn / Si ≧ 1.00 at Mn: 2.00 wt% or less to form fine powder with an average particle size of 20 μm or less, spheroidization is achieved and injection molding properties and baking are achieved. It is possible to provide Fe-Co alloy fine powder with improved binding property, and by using the fine powder, the relative density ratio is 92
% Or more of the sintered material can be provided.
また、本発明によれば、B;0.02〜1.00wt％、P;0.05〜1.
00wt％のうちの１種以上を溶湯に合金し、アトマイズし
て平均粒径が20μｍ以下の微粉末とすることによって、
一段と球状化を図って射出成形性と焼結性を改善したFe
-Co系およびFe-Co-V系合金微粉を提供できるとともに、
当該微粉を用いることにより、相対密度比が92％以上の
磁気特性に優れた焼結材料を提供することができる。Further, according to the present invention, B; 0.02 to 1.00 wt%, P; 0.05 to 1.
By alloying at least one of 00wt% with the molten metal and atomizing it into a fine powder with an average particle size of 20μm or less,
Fe with improved spheroidization for improved injection moldability and sinterability
-Co and Fe-Co-V alloy fine powder can be provided,
By using the fine powder, it is possible to provide a sintered material having a relative density ratio of 92% or more and excellent magnetic properties.
第１図は、焼結材料の相対密度比とHIP処理後の相対密
度比の関係を示すグラフである。FIG. 1 is a graph showing the relationship between the relative density ratio of the sintered material and the relative density ratio after HIP treatment.
フロントページの続き (51)Int.Cl.6 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｈ０１Ｆ 1/22 (72)発明者 渡辺 敏夫 千葉県千葉市川崎町１番地 川崎製鉄株式 会社技術研究本部内 (72)発明者 垣生 泰弘 千葉県千葉市川崎町１番地 川崎製鉄株式 会社技術研究本部内 (56)参考文献 特開 昭62−44555（ＪＰ，Ａ) 特開 昭63−53201（ＪＰ，Ａ) 特開 昭62−252919（ＪＰ，Ａ) 特開 昭59−136907（ＪＰ，Ａ) 特公 昭61−9380（ＪＰ，Ｂ２)Continuation of the front page (51) Int.Cl. 6 Identification number Reference number within the agency FI Technical indication location H01F 1/22 (72) Inventor Toshio Watanabe 1 Kawasaki-cho, Chiba-shi, Chiba Kawasaki Steel Co., Ltd. 72) Inventor Yasuhiro Kakio 1 Kawasaki-cho, Chiba-shi, Chiba Within the Technical Research Division, Kawasaki Steel Co., Ltd. (56) References JP-A-62-44555 (JP, A) JP-A-63-53201 (JP, A) Special Kai 62-252919 (JP, A) JP 59-136907 (JP, A) JP 61-9380 (JP, B2)
Claims (5)
00wt％以下でMn/Siが1.00以上、Co:15〜60wt％、不純物
を除き残部が実質的にFeの溶湯をアトマイズ法で粉末化
してなり、平均粒径が20μｍ以下の球状粉であることを
特徴とする射出成形用Fe-Co系合金微粉。1. C: 1.00 wt% or less, Si: 1.00 wt% or less, Mn: 2.
It is a spherical powder with an average particle size of 20 μm or less, which is made by atomizing a molten metal of Mn / Si of 1.00 or more at Co% of 00 wt% or less, Co: 15 to 60 wt% and the balance of Fe substantially except for impurities except for impurities by an atomization method. Fe-Co alloy fine powder for injection molding characterized by:
00wt％以下でMn/Siが1.00以上、V:1.0〜4.0wt％、Co:15
〜60wt％、不純物を除き残部が実質的にFeの溶湯をアト
マイズ法で粉末化してなり、平均粒径が20μｍ以下の球
状粉であることを特徴とする射出成形用Fe-Co系合金微
粉。2. C: 1.00 wt% or less, Si: 1.00 wt% or less, Mn: 2.
Mn / Si is 1.00 or more at 00wt% or less, V: 1.0 to 4.0wt%, Co: 15
Fe-Co alloy fine powder for injection molding, characterized in that it is a spherical powder having an average particle size of 20 μm or less, which is obtained by pulverizing a molten metal of ˜60 wt% and the balance of Fe substantially except for the impurities by an atomizing method.
00wt％以下でMn/Siが1.00以上、B:0.02〜1.00wt％およ
びP:0.05〜1.00wt％のうちの１種または２種、Co:15〜6
0wt％、不純物を除き残部が実質的にFeの溶湯をアトマ
イズ法で粉末化してなり、平均粒径が20μｍ以下の球状
粉であることを特徴とする射出成形用Fe-Co系合金微
粉。3. C: 1.00 wt% or less, Si: 1.00 wt% or less, Mn: 2.
Mn / Si is 1.00 or more at 00 wt% or less, one or two of B: 0.02 to 1.00 wt% and P: 0.05 to 1.00 wt%, Co: 15 to 6
Fe-Co alloy fine powder for injection molding, which is a spherical powder having an average particle size of 20 μm or less, which is obtained by pulverizing a molten metal of 0 wt% and the balance of Fe being substantially the rest by atomization.
00wt％以下でMn/Siが1.00以上、V:1.0〜4.0wt％、B:0.0
2〜1.00wt％およびP:0.05〜1.00wt％のうちの１種また
は２種、Co:15〜60wt％、不純物を除き残部が実質的にF
eの溶湯をアトマイズ法で粉末化してなり、平均粒径が2
0μｍ以下の球状粉であることを特徴とする射出成形用F
e-Co系合金微粉。4. C: 1.00 wt% or less, Si: 1.00 wt% or less, Mn: 2.
Mn / Si is 1.00 or more at 00 wt% or less, V: 1.0 to 4.0 wt%, B: 0.0
1 to 2 of 2 to 1.00 wt% and P: 0.05 to 1.00 wt%, Co: 15 to 60 wt%, the balance being substantially F except impurities.
The molten metal of e is atomized by the atomization method and has an average particle size of 2
Injection molding F characterized by being a spherical powder of 0 μm or less
Fine powder of e-Co alloy.
成形用Fe-Co系合金微粉を有機バインダーに混練して射
出成形を行い、その成形品を焼結してなる、Ｃ含有率が
0.02wt％以下で、真密度に対する密度比が92％以上であ
ることを特徴とするFe-Co系焼結磁性材料。5. A C content rate obtained by kneading the Fe—Co alloy fine powder for injection molding according to claim 1 with an organic binder, performing injection molding, and sintering the molded product. But
A Fe-Co based sintered magnetic material, which has a density ratio of not less than 0.02 wt% and a true density of 92% or more.
Priority Applications (8)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63206720A JPH0715121B2 (en) | 1988-08-20 | 1988-08-20 | Fe-Co alloy fine powder for injection molding and Fe-Co sintered magnetic material |
| AU38024/89A AU3802489A (en) | 1988-07-13 | 1989-07-11 | Alloy steel powders for injection molding use, their compounds and a method for making sintered parts from the same |
| CA000605506A CA1335759C (en) | 1988-07-13 | 1989-07-12 | Alloy steel powders for injection molding use, their compounds and a method for making sintered parts from the same |
| EP89307117A EP0354666B1 (en) | 1988-07-13 | 1989-07-13 | Alloy steel powders for injection molding use, their commpounds and a method for making sintered parts from the same |
| DE68924678T DE68924678T2 (en) | 1988-07-13 | 1989-07-13 | Steel alloy powder for injection molding process, its connections and a process for producing sintered parts therefrom. |
| KR1019890009962A KR930002523B1 (en) | 1988-07-13 | 1989-07-13 | Alloy steel powder |
| AU88923/91A AU637538B2 (en) | 1988-07-13 | 1991-12-06 | Alloy steel powders for injection molding use, their compounds and a method for making sintered parts from the same |
| US07/962,607 US5338508A (en) | 1988-07-13 | 1992-10-16 | Alloy steel powders for injection molding use, their compounds and a method for making sintered parts from the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63206720A JPH0715121B2 (en) | 1988-08-20 | 1988-08-20 | Fe-Co alloy fine powder for injection molding and Fe-Co sintered magnetic material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0257608A JPH0257608A (en) | 1990-02-27 |
| JPH0715121B2 true JPH0715121B2 (en) | 1995-02-22 |
Family
ID=16527990
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63206720A Expired - Fee Related JPH0715121B2 (en) | 1988-07-13 | 1988-08-20 | Fe-Co alloy fine powder for injection molding and Fe-Co sintered magnetic material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0715121B2 (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2743572B1 (en) * | 1996-01-11 | 1998-02-13 | Imphy Sa | IRON-COBALT ALLOY, METHOD FOR MANUFACTURING A STRIP OF IRON-COBALT ALLOY AND STRIP OBTAINED |
| JP4568691B2 (en) * | 2006-03-28 | 2010-10-27 | Ｊｆｅケミカル株式会社 | Magnetite-iron-cobalt composite powder for dust core, method for producing the same, and dust core using the same |
| JP5248065B2 (en) * | 2007-08-31 | 2013-07-31 | 株式会社タムラ製作所 | Core material and core using the same, choke coil using the core |
| JP5368686B2 (en) * | 2007-09-11 | 2013-12-18 | 住友電気工業株式会社 | Soft magnetic material, dust core, method for producing soft magnetic material, and method for producing dust core |
| JP4907597B2 (en) * | 2008-05-13 | 2012-03-28 | 山陽特殊製鋼株式会社 | Method for producing Fe-Co-V alloy material |
| DE102014213794A1 (en) * | 2014-07-16 | 2016-01-21 | Robert Bosch Gmbh | Soft magnetic alloy composition and method for producing such |
| JP6904034B2 (en) * | 2017-04-17 | 2021-07-14 | セイコーエプソン株式会社 | Soft magnetic powder, powder magnetic core, magnetic element and electronic equipment |
| US10607757B1 (en) | 2017-06-30 | 2020-03-31 | Tdk Corporation | Production method of soft magnetic metal powder |
| CN108284219B (en) * | 2017-08-15 | 2019-10-08 | 长沙墨科瑞网络科技有限公司 | Stainless steel mixed-powder contains the powder stainless steel clay and the Clay Consolidation technique |
| JP7087558B2 (en) | 2018-03-29 | 2022-06-21 | セイコーエプソン株式会社 | Manufacturing method of soft magnetic powder and sintered body |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59136907A (en) * | 1983-01-25 | 1984-08-06 | Seiko Epson Corp | Manufacture of resin bonded rare-earth cobalt magnet |
| JPS619380A (en) * | 1984-06-22 | 1986-01-16 | Tsutomu Miwa | Bonnet air-flowing plate |
| JPS6244555A (en) * | 1985-08-19 | 1987-02-26 | Hitachi Metals Ltd | Magnetic fe-co alloy |
| JPS62252919A (en) * | 1986-04-25 | 1987-11-04 | Seiko Epson Corp | Manufacture of sintered rare earth magnet |
| JPS6353201A (en) * | 1986-08-25 | 1988-03-07 | Daido Steel Co Ltd | Production of permanent magnet material |
-
1988
- 1988-08-20 JP JP63206720A patent/JPH0715121B2/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| JPH0257608A (en) | 1990-02-27 |
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