JPH0450379B2 - - Google Patents
Info
- Publication number
- JPH0450379B2 JPH0450379B2 JP60107691A JP10769185A JPH0450379B2 JP H0450379 B2 JPH0450379 B2 JP H0450379B2 JP 60107691 A JP60107691 A JP 60107691A JP 10769185 A JP10769185 A JP 10769185A JP H0450379 B2 JPH0450379 B2 JP H0450379B2
- Authority
- JP
- Japan
- Prior art keywords
- powder
- iron
- particles
- sintered
- iron powder
- 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
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 128
- 239000000843 powder Substances 0.000 claims description 84
- 239000002245 particle Substances 0.000 claims description 60
- 229910052742 iron Inorganic materials 0.000 claims description 31
- 239000002994 raw material Substances 0.000 claims description 19
- 229910052718 tin Inorganic materials 0.000 claims description 19
- 239000000696 magnetic material Substances 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 229910052698 phosphorus Inorganic materials 0.000 claims description 7
- 238000005245 sintering Methods 0.000 description 20
- 239000002184 metal Substances 0.000 description 19
- 229910052751 metal Inorganic materials 0.000 description 19
- 229910000519 Ferrosilicon Inorganic materials 0.000 description 15
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 12
- 238000000034 method Methods 0.000 description 12
- 239000011863 silicon-based powder Substances 0.000 description 12
- 229910017091 Fe-Sn Inorganic materials 0.000 description 10
- 229910017142 Fe—Sn Inorganic materials 0.000 description 10
- 229910000859 α-Fe Inorganic materials 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 229910052710 silicon Inorganic materials 0.000 description 9
- 238000009792 diffusion process Methods 0.000 description 7
- 229910017082 Fe-Si Inorganic materials 0.000 description 6
- 229910017133 Fe—Si Inorganic materials 0.000 description 6
- 230000004907 flux Effects 0.000 description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 5
- 239000011812 mixed powder Substances 0.000 description 5
- 230000035699 permeability Effects 0.000 description 5
- 230000007423 decrease Effects 0.000 description 4
- 239000011856 silicon-based particle Substances 0.000 description 4
- 229910000976 Electrical steel Inorganic materials 0.000 description 3
- 229910005382 FeSn Inorganic materials 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 238000005204 segregation Methods 0.000 description 3
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 3
- 229910001887 tin oxide Inorganic materials 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910008355 Si-Sn Inorganic materials 0.000 description 2
- 229910006453 Si—Sn Inorganic materials 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 150000003376 silicon Chemical class 0.000 description 2
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 2
- NGCDGPPKVSZGRR-UHFFFAOYSA-J 1,4,6,9-tetraoxa-5-stannaspiro[4.4]nonane-2,3,7,8-tetrone Chemical compound [Sn+4].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O NGCDGPPKVSZGRR-UHFFFAOYSA-J 0.000 description 1
- 229910006367 Si—P Inorganic materials 0.000 description 1
- 229910001128 Sn alloy Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 229910001566 austenite Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 239000011246 composite particle Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000004453 electron probe microanalysis Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- ZBJWWKFMHOAPNS-UHFFFAOYSA-N loretin Chemical compound C1=CN=C2C(O)=C(I)C=C(S(O)(=O)=O)C2=C1 ZBJWWKFMHOAPNS-UHFFFAOYSA-N 0.000 description 1
- 229950010248 loretin Drugs 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003606 tin compounds Chemical class 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
Landscapes
- Powder Metallurgy (AREA)
Description
【発明の詳細な説明】
産業上の利用分野
この発明はモーターの鉄芯などに使用される鉄
系焼結磁性材料、およびその焼結磁性材料の製造
に使用される原料粉末に関するものである。DETAILED DESCRIPTION OF THE INVENTION Field of Industrial Application This invention relates to an iron-based sintered magnetic material used for the iron core of a motor, and a raw material powder used for manufacturing the sintered magnetic material.
従来の技術
鉄系焼結材料は、積層珪素鋼板などに比較して
形状の自由度が大きいため、モーター部品などに
広く使用されるようになつている。しかしながら
鉄系焼結材料をモーター等の部品、特に鉄芯とし
て使用する場合の最大の問題は、その交流磁気特
性が積層珪素鋼板と比較して格段に劣ること、す
なわち鉄損が極めて大きいことであり、そのため
モーター等の効率が低くならざるを得ず、また発
熱の問題も避け得なかつた。このように焼結磁性
材料を用いた場合に鉄損が大きくなる理由は、一
般に焼結部品は積層物ではなく、一体物として使
用されているため、渦電液が流れ易く、そのため
渦電液損失が極端に大きくなる点にある。そこ
で、鉄系焼結磁性材料については、従来からその
電気抵抗を高めることによつて渦電流損失を低減
するための試みが種々なされている。BACKGROUND ART Iron-based sintered materials have a greater degree of freedom in shape than laminated silicon steel sheets, so they have come to be widely used in motor parts and the like. However, the biggest problem when using iron-based sintered materials for parts such as motors, especially as iron cores, is that their AC magnetic properties are significantly inferior to those of laminated silicon steel sheets, that is, the iron loss is extremely large. As a result, the efficiency of motors, etc. had to be low, and the problem of heat generation was unavoidable. The reason why iron loss is large when using sintered magnetic materials is that sintered parts are generally used as a single piece rather than as a laminate, so eddy electric liquid flows easily. This is the point where losses become extremely large. Therefore, various attempts have been made to reduce eddy current loss by increasing the electrical resistance of iron-based sintered magnetic materials.
鉄に対する各種合金元素のうち、特にSiは電気
抵抗を高めるに最も有効な元素として知られてお
り、実際に珪素鋼板圧延板ではそのSi添加の効果
を活用している。そこで焼結磁性材料の場合にお
いても、鉄粉に金属Si粉やフエロシリコン粉を添
加・混合し、成形・焼結する方法が従来から試み
られている。しかしながら金属Si粉末粒子やフエ
ロシリコン粉末粒子は鉄粉粒子と比較して格段に
硬質であるため、これらを添加した場合圧粉密度
が低下し、そのため焼結密度が低下して、磁束密
度が低くならざるを得ないという問題がある。 Among various alloying elements for iron, Si in particular is known as the most effective element for increasing electrical resistance, and the effect of Si addition is actually utilized in rolled silicon steel sheets. Therefore, even in the case of sintered magnetic materials, attempts have been made in the past to add and mix metal Si powder or ferrosilicon powder to iron powder, form it, and sinter it. However, metal Si powder particles and ferrosilicon powder particles are much harder than iron powder particles, so when these are added, the green powder density decreases, which reduces the sintered density and increases the magnetic flux density. The problem is that it has to be lower.
上述の問題を解決するため、既に特公昭40−
12045号公報に記載されているように、Siに加え
てＰを添加し、これによつて焼結性を向上させ、
焼結密度の向上、ひいては磁気特性の向上を図る
方法が提案されている。しかしながらＰ添加の方
法では、Si量が3wt％以下と低Siの場合には７
ｇ／cm2以上の高い焼結密度を得ることが可能であ
るが、Si量が3wt％を越えれば充分な焼結密度を
得ることができず、したがつて根本的な解決とは
なつていないのが実情である。 In order to solve the above-mentioned problems, the special public
As described in Publication No. 12045, P is added in addition to Si to improve sinterability,
Methods have been proposed to improve the sintered density and, by extension, the magnetic properties. However, with the P addition method, when the Si content is low (3 wt% or less), 7
Although it is possible to obtain a high sintered density of g/ cm2 or more, if the amount of Si exceeds 3wt%, it is not possible to obtain a sufficient sintered density, and therefore it is not a fundamental solution. The reality is that there is not.
発明が解系決すべき問題点
既に述べたように鉄系焼結材料における最大の
問題はその交流磁気特性が劣ること、すなわち鉄
損値が高いことであり、これを解決するために鉄
粉に単に金属Si粉やフエロシリコン粉を混合して
成形・焼結した場合は圧粉密度・焼結密度が低下
して透磁率が低くなつてしまう問題があり、また
Siに併せてＰを添加することによつて焼結性を改
善する方法も、低Si系には有効であるが高Si系に
ついては有効ではない。Problems to be solved by the invention As already mentioned, the biggest problem with iron-based sintered materials is their poor AC magnetic properties, that is, their high iron loss. If metal Si powder or ferrosilicon powder is simply mixed and then molded and sintered, there is a problem that the compacted powder density and sintered density decrease, resulting in low magnetic permeability.
A method of improving sinterability by adding P in addition to Si is also effective for low-Si systems, but not for high-Si systems.
この発明は以上の事情に鑑みてなされたもの
で、高濃度にSiを添加したFe―Si系焼結磁性材
料においてその焼結性を充分に向上させ、これに
よつて従来よりも格段に低鉄損、高透磁率とした
鉄系焼結材料を提供すると同時に、そのような磁
気特性の優れた鉄系焼結材料を組製造するための
原料粉末を提供することを目的とするものであ
る。 This invention was made in view of the above circumstances, and it sufficiently improves the sinterability of Fe-Si based sintered magnetic materials to which Si is added at a high concentration, thereby achieving significantly lower sinterability than before. The purpose of the present invention is to provide an iron-based sintered material with high iron loss and high magnetic permeability, and at the same time to provide raw material powder for manufacturing such iron-based sintered materials with excellent magnetic properties. .
問題点を解決するための手段
上述のような目的を達成するべく、本発明者は
種々実験・検討を重ねた結果、Fe―Si系焼結材
料にSn（錫）を添加することによつて、焼結性の
改善、ひいては磁気特性の向上を図り得ることを
見出した。そしてまたその場合に原料粉末の少な
くとも一部として、鉄粉粒子表面にSnが濃化し
て存在する複合粒子を用いることが磁気特性の向
上に有効であることを見出した。さらに、Snの
ほか、Ｐをも追加添加することが磁気特性のより
一層の向上に有効であることを見出した。Means for Solving the Problems In order to achieve the above-mentioned objectives, the inventor of the present invention has conducted various experiments and studies, and found that by adding Sn (tin) to the Fe-Si based sintered material. It has been found that it is possible to improve sinterability and, in turn, improve magnetic properties. We have also found that in this case, it is effective to use composite particles in which Sn is concentrated on the surface of iron powder particles as at least part of the raw material powder to improve the magnetic properties. Furthermore, it has been found that addition of P in addition to Sn is effective in further improving magnetic properties.
この発明は上述のような知見を基礎になされた
もので、第１発明の焼結磁性材料は、Siを１〜
12wt％、Snを0.05〜7wt％含み、残部が実質的に
Feであることを特徴とするものである。 This invention was made based on the above-mentioned knowledge, and the sintered magnetic material of the first invention contains Si from 1 to 1.
Contains 12wt%, Sn 0.05-7wt%, and the remainder is substantially
It is characterized by being Fe.
また第２発明の焼結磁性材料は、Siを１〜
12wt％、Snを0.05〜7wt％、Ｐを0.05〜2wt％含
み、残部が実質的にFeであることを特徴とする
ものである。 Further, the sintered magnetic material of the second invention has Si of 1 to 1
It is characterized by containing 12wt% of Sn, 0.05 to 7wt% of Sn, 0.05 to 2wt% of P, and the balance being substantially Fe.
さらに第３発明の焼結磁性材料製造用の原料粉
末は、粉末全体としての成分組成が、Si1〜12wt
％、Sn0.05〜7wt％を含みかつ残部が実質的にFe
とされており、しかも少なくとも一部の粉末粒子
として、鉄粉粒子表面にSnが濃化して存在する
粒子を含むを特徴とするものである。 Furthermore, the raw material powder for producing the sintered magnetic material of the third invention has a component composition as a whole of Si1 to 12wt.
%, contains 0.05 to 7wt% of Sn, and the balance is substantially Fe.
Moreover, it is characterized in that at least some of the powder particles include particles in which Sn is present in a concentrated manner on the surface of the iron powder particles.
また第４発明の焼結磁性材料製造用の原料粉末
は、粉末全体としての成分組成が、Si1〜12wt
％、Sn0.05〜7wt％、P0.05〜2wt％を含みかつ残
部が実質的にFeとされており、しかも少なくと
も一部の粉末粒子として、鉄粉粒子表面にSnが
濃化して存在する粒子を含むことを特徴とするも
のである。 Further, the raw material powder for producing the sintered magnetic material of the fourth invention has a component composition as a whole of Si1 to 12wt.
%, Sn0.05-7wt%, P0.05-2wt%, and the remainder is substantially Fe, and Sn is present as concentrated on the surface of the iron powder particles as at least some of the powder particles. It is characterized by containing particles.
作 用
はじめに、Si量を１〜12％と限定した理由を説
明するため、第１図に、Fe―Si合金におけるSi
量と電気抵抗率との関係を示す。鉄損は電気抵抗
にほぼ反比例するから、交流磁気特性を向上させ
るには前述のように焼結体の電気抵抗を増す必要
があるが、第１図に示すように例えばSi1％では
電気抵抗は純鉄の場合の２倍になり、鉄損はほぼ
半減する。しかしながら純鉄の２倍程度の電気抵
抗を得筏ことは、Si添加によらなくとも、より焼
結性の良いＰなどの添加で充分に可能であるか
ら、１％未満のSi添加は意味が少ない。一方、Si
を12％を越えて添加しても、むしろ電気抵抗が低
下してしまうから、Si量は１〜12％の範囲とす
る。Function First, to explain the reason for limiting the Si content to 1 to 12%, Figure 1 shows the Si content in the Fe-Si alloy.
The relationship between quantity and electrical resistivity is shown. Iron loss is almost inversely proportional to electrical resistance, so to improve AC magnetic properties it is necessary to increase the electrical resistance of the sintered body as described above, but as shown in Figure 1, for example, with 1% Si, the electrical resistance is The iron loss is twice that of pure iron, and the iron loss is almost halved. However, it is possible to obtain a raft with electrical resistance about twice that of pure iron without adding Si, but with the addition of materials such as P, which have better sinterability, so adding less than 1% Si is meaningless. few. On the other hand, Si
If more than 12% of Si is added, the electrical resistance will actually decrease, so the amount of Si should be in the range of 1 to 12%.
次にSnの添加理由について説明する。 Next, the reason for adding Sn will be explained.
Snはα―Fe相を出現しやすくする元素である
ため、Snを添加すれば、所謂α焼結によつて焼
結が促進されて焼結密度が高まり、しかも結晶粒
が粗大化される。したがつてSnは磁気特性向上
のために元来有用な元素である。但しSnはSiほ
どには電気抵抗を増す効果はないから、Siと併せ
てSnを添加して、Fe―Si―Sn系合金として用い
ることにより、極めて有用な特性が得られるので
ある。 Sn is an element that facilitates the appearance of the α-Fe phase, so adding Sn promotes sintering through so-called α sintering, increases the sintered density, and coarsens the crystal grains. Therefore, Sn is an element originally useful for improving magnetic properties. However, since Sn is not as effective as Si in increasing electrical resistance, extremely useful properties can be obtained by adding Sn together with Si and using it as a Fe--Si--Sn alloy.
Fe―Si系焼結体を作成する場合、鉄粉とフエ
ロシリコン粉もしくは金属Si粉とを混合し、成
形・焼結するのが従来の通常の方法であるが、こ
の場合Si添加により圧粉密度は相当低下する。仮
に焼結中に焼結体の収縮が充分に起こるならば、
焼結密度は高くなるのであるが、実際には収縮の
程度は少なく、焼結密度ひいては磁束密度などの
磁気特性が劣る傾向が生じることを逸れ得ない。
すなわち、本来Siは、Snと同様にFeに合金化し
てα―Fe相を出現させやすく、しかもα―Fe相
中の拡散係数が大きいことから、焼結性を向上さ
せる可能性を有する元素ではあるが、現実にはそ
の効果を充分に発揮させることは困難であつた。 When creating a Fe-Si based sintered body, the conventional method is to mix iron powder and ferrosilicon powder or metal Si powder, and then shape and sinter it. Powder density decreases considerably. If sufficient shrinkage of the sintered body occurs during sintering,
Although the sintered density increases, the degree of shrinkage is actually small, and it cannot be ignored that the sintered density and the magnetic properties such as magnetic flux density tend to be inferior.
In other words, Si is originally an element that has the potential to improve sinterability because, like Sn, Si tends to alloy with Fe and form an α-Fe phase, and has a large diffusion coefficient in the α-Fe phase. However, in reality, it has been difficult to fully demonstrate its effects.
その最大の原因は、鉄粉粒子とフエロシリコン
もしくは金属Si粒子との接触部において、Siが鉄
粉に拡散しにくいことにある。すなわち、焼結初
期の段階では鉄粉はγ―Fe相となつており、γ
―Fe相中のSiの拡散係数はα―Fe相中の拡散係
数と比較して極めて小さく、しかも鉄粉粒子とフ
エロシリコン粉もしくは金属Si粒子との接触面積
が小さいため、Siの鉄粉粒子中への初期拡散が起
こりにくいと考えられる。 The biggest reason for this is that Si is difficult to diffuse into the iron powder at the contact area between the iron powder particles and the ferrosilicon or metal Si particles. In other words, at the initial stage of sintering, the iron powder is in the γ-Fe phase, and the γ
- The diffusion coefficient of Si in the Fe phase is extremely small compared to the diffusion coefficient in the α-Fe phase, and the contact area between iron powder particles and ferrosilicon powder or metal Si particles is small, so Si iron powder It is thought that initial diffusion into particles is unlikely to occur.
このような考察に基づき、本発明者は、焼結中
においてSiが鉄粉中に拡散を開始する前の段階で
既に鉄粉がα―Fe相になつていれば、Siを容易
に鉄粉中へ拡散させ得る筈であると考えた。その
ためには、α―Fe相は、鉄粉粒子全体にわたつ
て生成されている必要はなく、粒子表面だけでも
効果がある筈であり、したがつて焼結初期に少な
くとも鉄粉表面がα―Fe相となるようにしてお
くことが焼結性改善に有効と考えられる。 Based on these considerations, the present inventors believe that if the iron powder has already become the α-Fe phase before Si starts to diffuse into the iron powder during sintering, Si can be easily removed from the iron powder. I thought it would be possible to diffuse it inside. For this purpose, the α-Fe phase does not need to be generated over the entire iron powder particle, and should have an effect only on the particle surface. Therefore, at the beginning of sintering, at least the iron powder surface has an α-Fe phase. It is thought that keeping it in the Fe phase is effective in improving sinterability.
本発明者は、Snを用いることによつて上述の
機構による焼結性向上に成功した。すなわちSn
は、前述のようにα―Fe相を出現させ易い元素
であるに加えて、比較的容易に鉄粉粒子表面に濃
化させ得ることが大きな特徴である。鉄粉粒子表
面にSnを濃化させるためには、メツキ法を用い
ることも可能であるが、例えば鉄粉とスズ粉を混
合してSnの融点以上に加熱するという簡単な手
段によつて溶融Snがすみやかに鉄粉粒子表面を
覆い、Snの濃化部分を容易に形成することがで
きるのである。このようにSnが表面に濃化した
鉄粉をフエロシリコン粉や金属Si粉と混合して成
形・焼結すれば、焼結初期に鉄粉粒子表面がSn
の作用によりα―Fe相となり、Siの拡散が促進
される。そして一旦SiがFe中に拡散すれば、α
―Fe相がさらに拡大し、いわゆるα焼結により
高焼結密度が得られ、その結果磁気特性が大幅に
改善された焼結部品を得ることができるのであ
る。 The present inventor succeeded in improving the sinterability by the above-mentioned mechanism by using Sn. That is, Sn
In addition to being an element that tends to cause the α-Fe phase to appear as described above, its major feature is that it can be relatively easily concentrated on the surface of iron powder particles. In order to concentrate Sn on the surface of iron powder particles, it is possible to use the plating method, but for example, it is possible to melt Sn by a simple method of mixing iron powder and tin powder and heating it above the melting point of Sn. Sn quickly covers the surface of the iron powder particles, making it easy to form Sn-enriched areas. If iron powder with Sn concentrated on the surface is mixed with ferrosilicon powder or metal Si powder and then molded and sintered, the surface of the iron powder particles will become Sn in the early stage of sintering.
Due to the action of , it becomes an α-Fe phase, and the diffusion of Si is promoted. And once Si diffuses into Fe, α
-The Fe phase is further expanded and a high sintered density is obtained through so-called alpha sintering, resulting in sintered parts with significantly improved magnetic properties.
このような効果を与えるためには、Snは少な
くとも0.05wt％を必要とする。後述する実施例の
第２図に示すように、Snが0.05wt％未満ではSn
添加による充分な磁気特性改善効果が得られな
い。その理由は、Snが0.05wt％未満では焼結初
期におけるα―Fe相形成が不充分となるためと
考えられる。一方Snが7wt％を越えても第２図に
示すように逆に磁気特性が劣化する。その理由
は、Snが7wt％を越えれば鉄粉粒子表面のSnが
過剰となつて、焼結初期にα―Fe相のほかにFe
―Sn化合物相が多量に生成され、その結果かえ
つてSiの拡散が阻害されるためと思われる。した
がつて、Sn量は0.05〜7wt％の範囲内に限定し
た。 To provide such an effect, Sn needs to be at least 0.05wt%. As shown in FIG. 2 of Examples described later, when Sn is less than 0.05wt%, Sn
A sufficient effect of improving magnetic properties cannot be obtained by addition. The reason for this is thought to be that if Sn is less than 0.05 wt%, α-Fe phase formation at the initial stage of sintering becomes insufficient. On the other hand, if Sn exceeds 7wt%, the magnetic properties will deteriorate as shown in FIG. The reason for this is that if Sn exceeds 7wt%, Sn on the surface of the iron powder particles becomes excessive, and in the initial stage of sintering, Fe and Fe phases are formed.
- This seems to be because a large amount of Sn compound phase is generated, which actually inhibits the diffusion of Si. Therefore, the amount of Sn was limited within the range of 0.05 to 7 wt%.
鉄粉粒子表面にSnを濃化させる方法としては、
前述のように鉄粉とスズ粉を混合して加熱する方
法が最も簡便であるが、スズ粉の代りに酸化スズ
物を用い、その酸化スズ粉を鉄粉と混合して還元
性雰囲気で加熱しても同様の効果が得られる。こ
の場合酸化スズは金属スズ物よりも細かいものが
製造しやすいため、金属スズ粉を使用する場合よ
りも鉄粉粒子表面にSnを均一に濃化させ易い利
点がある。そのほか、塩化スズやしゆう酸スズな
ど、加熱により分解してSnを生成するスズ化合
物粉末を金属スズの代りに用いることができる。 As a method for concentrating Sn on the surface of iron powder particles,
As mentioned above, the simplest method is to mix iron powder and tin powder and heat them, but it is also possible to use tin oxide instead of tin powder, mix the tin oxide powder with iron powder, and heat it in a reducing atmosphere. The same effect can be obtained. In this case, tin oxide is easier to produce in finer pieces than metal tin products, so it has the advantage that it is easier to uniformly concentrate Sn on the surface of iron powder particles than when using metal tin powder. In addition, tin compound powder, such as tin chloride and tin oxalate, which decomposes to produce Sn when heated, can be used in place of metal tin.
このようにして得られるFe―Sn粉末における、
鉄粉粒子表面のSn濃化状態は次のようなもので
ある。すなわち、Sn濃化部分におけるSnの化学
的形態は、金属スズ、またはFeと反応して生成
するFe―Sn化合物（FeSn、FeSn、FeSnなど）
の状態となつている。但し、鉄粉粒子に含有され
る元素によつては、Sn濃化部分にSn、Fe以外の
第３の元素が含有されることもある。一方Sn濃
化部分の物理的形態としては、理想的には鉄粉粒
子表面を均一に覆つたものが望ましいが、技術
上、経済上の制約により、鉄粉粒子表面の一部が
Sn濃化部分を持たない場合があり、このような
粉末も実用上は支障ない。すなわち上述したよう
なSn源の粉末と鉄粉とを混合し、加熱してFe―
Sn粉末を作成する場合、Sn源となる粉末の粒度
が粗かつたり、混合が完全でなかつたりすること
は、製造設備上の節約などで、止むを得ないこと
があり、その場合には、鉄粉粒子の表面の一部が
Sn濃化部分で覆われないこともある。 In the Fe-Sn powder obtained in this way,
The Sn concentration state on the surface of iron powder particles is as follows. In other words, the chemical form of Sn in the Sn-enriched area is metallic tin or Fe-Sn compounds (FeSn, FeSn, FeSn, etc.) produced by reacting with Fe.
It is in a state of However, depending on the element contained in the iron powder particles, a third element other than Sn and Fe may be contained in the Sn-enriched portion. On the other hand, the physical form of the Sn-enriched portion is ideally such that it uniformly covers the surface of the iron powder particle, but due to technical and economic constraints, a portion of the surface of the iron powder particle is
In some cases, the powder does not have a Sn-enriched portion, and such powder does not pose any practical problems. That is, the Sn source powder and iron powder as described above are mixed and heated to form Fe-
When creating Sn powder, it may be unavoidable that the Sn source powder has a coarse particle size or is not mixed completely due to reasons such as saving on production equipment. Part of the surface of the iron powder particles
It may not be covered by the Sn-enriched part.
上述のようにSnが表面に濃化されたFe―Sn粉
末を用いて焼結体を製造するにあたつては、最終
的に得るべき焼結体中のFe分の全量をFe―Sn粉
末で供給しても良いが、場合によつてはFe―Sn
粉末を併せて、Snが表面に濃化されていない鉄
粉を使用しても良い。すなわち、上述のように
Fe―Sn粉末を鉄粉と混合し、いわば薄めて使用
した方が、粉末の圧縮性や全体の粉末コストの観
点から有利となる場合もあり、その場合にはSn
濃化部を有する鉄粉粒子とSn濃化部を持たない
鉄粉粒子との混合粉末を焼結原料粉末として使用
することになる。また、前述のようにFe―Sn粉
末を製造するにあたつては、Sn粉末もしくはSn
を含有する粉末が鉄粉粒子表面から一部離脱して
混合状態で存在することもあり、このような場合
もその程度が少なければ支障ない。いずれにして
も、焼結原料のうちの鉄源の粉末全体として、鉄
粉粒子表面全体の20％程度以上の表面がSn濃化
部で覆われているようにすることが望ましい。 As mentioned above, when manufacturing a sintered body using Fe-Sn powder with Sn concentrated on the surface, the entire amount of Fe in the sintered body to be finally obtained is However, in some cases Fe-Sn may be supplied.
In addition to the powder, iron powder on which Sn is not concentrated on the surface may be used. That is, as mentioned above
Mixing Fe-Sn powder with iron powder and diluting it may be more advantageous in terms of powder compressibility and overall powder cost.
A mixed powder of iron powder particles having an enriched portion and iron powder particles having no Sn enriched portion will be used as the sintering raw material powder. In addition, as mentioned above, when producing Fe-Sn powder, Sn powder or Sn
In some cases, a part of the powder containing the iron powder particles separates from the surface of the iron powder particles and exists in a mixed state, and even in such a case, there is no problem as long as the extent of this is small. In any case, it is desirable that about 20% or more of the entire surface of the iron powder particles be covered with the Sn-enriched portion in the entire iron source powder of the sintering raw materials.
一方Siの添加は、前述のように鉄粉粒子表面に
Snを濃化したFe―Sn粉末（あるいはそのFe―Sn
粉末と鉄粉）に、金属Si粉やフエロシリコン粉を
所定量混合し、全体としてFe、Si、Snを含む混
合粉末として、圧粉・焼結すれば良い。 On the other hand, the addition of Si causes the surface of iron powder particles to
Fe-Sn powder enriched with Sn (or its Fe-Sn
A predetermined amount of metallic Si powder or ferrosilicon powder may be mixed with powder and iron powder), and the mixture may be pressed and sintered to form a mixed powder containing Fe, Si, and Sn as a whole.
またSi添加のための一手法としては、前述のよ
うに予め鉄粉粒子表面にSnを濃化させたFe―Sn
粒子を製造する工程において、鉄粉とスズ源の粉
末のほかに、さらに金属Si粉やフエロシリコン粉
を添加混合してから加熱処理した粉末を焼結原料
として用いても良く、この場合にはSnが溶融し
て鉄粉粒子を覆う過程でSnが金属Si粉やフエロ
シリコン粉を鉄粉粒子に付着させるバインダーと
しても作用し、その結果原料粉末中のSiの偏析を
防止し、ひいては焼結体のSiの偏析を防止する効
果が期待できる。 In addition, as a method for adding Si, as mentioned above, Fe--Sn is prepared by pre-concentrating Sn on the surface of iron powder particles.
In the process of manufacturing particles, in addition to iron powder and tin source powder, metal Si powder or ferrosilicon powder may be added and mixed and heat-treated powder may be used as the sintering raw material. In the process of Sn melting and covering the iron powder particles, Sn also acts as a binder that attaches metal Si powder and ferrosilicon powder to the iron powder particles, and as a result, it prevents the segregation of Si in the raw powder, and in turn, It can be expected to have the effect of preventing segregation of Si in the sintered body.
以上のようなFe―Si―Sn焼結体にさらにＰを
添加すれば、一層の焼結性の向上、ひいては磁気
特性の一層の向上を実現することができる。Ｐは
Snと同様にα焼結を促進する元素として知られ
ており、したがつてＰの添加によつて焼結性を一
層向上させることができるのである。ここで、Ｐ
の添加量が0.05wt％未満では、後述する実施例の
第３表に示すようにＰ添加による効果が少なく、
一方2wt％を越えれば焼結体中に非磁性の析出物
が出現して磁気特性がかえつて低下するから、Ｐ
を添加する場合の添加は0.05〜2wt％の範囲内と
する。 If P is further added to the Fe--Si--Sn sintered body as described above, it is possible to further improve the sinterability and further improve the magnetic properties. P is
Like Sn, it is known as an element that promotes α-sintering, and therefore, the addition of P can further improve sinterability. Here, P
If the addition amount of
On the other hand, if it exceeds 2wt%, non-magnetic precipitates will appear in the sintered body and the magnetic properties will deteriorate, so P
When adding, the addition should be within the range of 0.05 to 2wt%.
Ｐの添加方法としては、前述したFe―Sn粉末
に、金属Si粉やフエロシリコン粉とともにフエロ
リン粉または赤リン粉を所定量混合し、Fe、Si、
Ｐ、Snを含む混合粉末として圧粉・焼結に供す
る方法が採用できる。あるいはまた、前述のFe
―Si―Sn粉末にフエロリン粉や赤リン粉を混合
しても良い。さらには前述のFe―Sn粉末製造工
程において、フエロリン粉や赤リン粉等のリン源
の粉末を鉄粉およびスズ源の粉末（もしくはこれ
らと金属Si粉やフエロシリコン粉）に混合して加
熱し、Snをバインダーとして鉄粉粒子にリン源
の粉末粒子を付着させれば、Siの場合と同様に焼
結原料粉末中のＰの偏析防止、ひいては焼結体中
のＰの偏析防止に効果が期待できる。 To add P, a predetermined amount of ferrophosphorus powder or red phosphorus powder is mixed with the aforementioned Fe-Sn powder together with metal Si powder or ferrosilicon powder to add Fe, Si,
A method can be adopted in which a mixed powder containing P and Sn is subjected to compaction and sintering. Alternatively, the aforementioned Fe
-Si-Sn powder may be mixed with ferrophosphorus powder or red phosphorus powder. Furthermore, in the Fe-Sn powder manufacturing process mentioned above, phosphorus source powder such as ferrophosphorus powder and red phosphorus powder is mixed with iron powder and tin source powder (or these and metal Si powder or ferrosilicon powder) and heated. However, if phosphorus source powder particles are attached to iron powder particles using Sn as a binder, it will be effective in preventing the segregation of P in the sintering raw material powder, and eventually in the sintered body, as in the case of Si. can be expected.
なお、以上のような焼結材料およびその原料粉
末には、若干の不可避的不純物が含まれることは
止むを得ない。これら不純物の量はできる限り低
く抑えることが焼結材料の磁気特性上好ましい
が、工業的な制約を考慮すれば、Ｃ：0.001〜
0.02％、Mn：0.005〜0.4％、Ｓ：0.0005〜0.02％、
Ｏ：0.01〜0.3％、Ｎ：0.0003〜0.01％程度の範囲
内が望ましい。 Incidentally, it is unavoidable that the above-mentioned sintered material and its raw material powder contain some unavoidable impurities. It is preferable to keep the amount of these impurities as low as possible in terms of the magnetic properties of the sintered material, but considering industrial constraints, C: 0.001~
0.02%, Mn: 0.005-0.4%, S: 0.0005-0.02%,
It is desirable that O: 0.01 to 0.3% and N: about 0.0003 to 0.01%.
以上述べたようなFe、SiおよびSnを含有する
焼結原料粉末またはFe、Si、ＰおよびSnを含有
する原料粉末は、次のように成形・焼結されて磁
性材料となる。なお原料粉末中には前述のように
表面にSnを濃化していない鉄粉をも含むことが
ある。但し前述したように、粉末中の鉄粉粒子の
全表面の少なくとも20％程度以上は、Sn濃化部
分を形成していることが好ましい。 The sintered raw material powder containing Fe, Si, and Sn or the raw material powder containing Fe, Si, P, and Sn as described above is shaped and sintered to become a magnetic material as follows. Note that the raw material powder may also contain iron powder whose surface is not enriched with Sn, as described above. However, as described above, it is preferable that at least about 20% or more of the entire surface of the iron powder particles in the powder form a Sn-enriched portion.
先ずこのような原料粉末に潤滑剤としてステア
リン酸亜鉛などを0.5〜1.0wt％程度添加し、金型
中で成形圧力３〜10t／cm2程度の成形を行なう。
成形された圧粉体を、焼結炉に送り、還元性雰囲
気、不活性ガス雰囲気または真空中で、温度1000
〜1350℃で0.5〜５時間焼結する。得られた焼結
体は、必要に応じてサイジングにより整形した
り、切削加工を加えたりして、焼結部品とすれば
良い。 First, about 0.5 to 1.0 wt % of zinc stearate or the like is added as a lubricant to such raw material powder, and molding is performed in a mold at a molding pressure of about 3 to 10 t/cm 2 .
The formed green compact is sent to a sintering furnace and heated to a temperature of 1000 in a reducing atmosphere, inert gas atmosphere, or vacuum.
Sinter at ~1350°C for 0.5-5 hours. The obtained sintered body may be shaped by sizing or subjected to cutting as necessary to form a sintered part.
実施例
実施例 １
粒度80メツシ以下のアトマイズ純鉄粉、250メ
ツシユ以下の金属Si粉、および250メツシユ以下
のスズ粉を、全体の成分組成がSi6.5wt％、Sn0
〜10wt％、残部Feとなるように混合し、水素ガ
ス中において1000℃で１時間加熱した。加熱後の
ケーキ状に固まつた混合粉末を粉砕し、80メツシ
ユ以下の粉末とした。その粉末粒子中の組成分布
を調べるため、粉末を樹脂に埋込んで研磨し、断
面をFPMAによつて観察した。その結果、Snを
0.1wt％以上含む粉末は、金属Si粒子と、表面に
Snが濃化した鉄粉粒子とからなり、金属Si粒子
の一部は鉄粉粒子表面に付着ないし冶金結合して
いることがわかつた。ExamplesExample 1 Atomized pure iron powder with a particle size of 80 mesh or less, metal Si powder with a particle size of 250 mesh or less, and tin powder with a particle size of 250 mesh or less with a total composition of Si6.5wt%, Sn0
The mixture was mixed so that the remaining content was ~10 wt% Fe, and the mixture was heated at 1000°C for 1 hour in hydrogen gas. After heating, the mixed powder that solidified into a cake was pulverized to a powder of 80 mesh or less. In order to investigate the composition distribution in the powder particles, the powder was embedded in resin and polished, and the cross section was observed using FPMA. As a result, Sn
Powders containing 0.1wt% or more contain metal Si particles and
It was found that the particles were composed of iron powder particles enriched with Sn, and some of the metal Si particles were attached or metallurgically bonded to the surface of the iron powder particles.
このような粉末を原料粉末とし、これにステア
リン酸亜鉛1wt％を添加し、7t／cm2で成形して、
外径38mm、内径25mm、高さ6.5mmのリング状圧粉
体を作成した。次いで圧粉体を水素ガス中にて
1260℃で120分焼結し、焼結体試料を得た。 This powder was used as a raw material powder, 1wt% of zinc stearate was added to it, and it was molded at 7t/ cm2 .
A ring-shaped powder compact with an outer diameter of 38 mm, an inner diameter of 25 mm, and a height of 6.5 mm was created. Next, the green compact is placed in hydrogen gas.
A sintered sample was obtained by sintering at 1260°C for 120 minutes.
これら焼結体の密度および磁気特性をSn含有
量と対応して第２図に示す。磁気特性としては、
磁界250eにおける磁束密度(B)、保磁力（Hc）、最
大透磁率（μmax）、磁束密度10kGで周波数50Hz
における鉄損（W10／50）を測定した。なお第２
図中にＰ＝1wt％と示している測定点は、比較の
ため、アトマイズ純鉄粉に金属Si粉を6.5wt％、−
250メツシユのフエロリン粉（17.5wt％Ｐ）をＰ
量にして1wt％混合し、同一条件で成形・焼結し
たFe―Si―Ｐ焼結体についての測定結果を示す
ものである。 The density and magnetic properties of these sintered bodies are shown in FIG. 2 in correspondence with the Sn content. As for magnetic properties,
Magnetic flux density (B), coercive force (Hc), maximum permeability (μmax) at magnetic field 250e, frequency 50Hz at magnetic flux density 10kG
The iron loss (W 10 / 50 ) was measured. Furthermore, the second
For comparison, the measurement points shown as P = 1wt% in the figure are 6.5wt% of metal Si powder in atomized pure iron powder, -
250 mesh powder of ferroline powder (17.5wt%P)
This figure shows the measurement results for a Fe--Si--P sintered body that was mixed in an amount of 1 wt% and molded and sintered under the same conditions.
第２図から明らかなように、Snを0.05〜7wt％
含有するFe―Si―Sn焼結体は、Fe−Si焼結体
（第２図におけるSn＝Owt％のもの）あるいはSn
を含有しないFe―Si―Ｐ焼結体（第２図におけ
るＰ＝1wt％のもの）にくらべて、焼結密度が大
きいため、磁束密度が高く、透磁率が大きく、さ
らに鉄損が小さいという、良好な磁気特性を示し
ている。Sn量が0.05wt％未満で磁気特性向上効
果が小さいのは、焼結初期の鉄粉粒子表面のα―
Fe相が不足するためと推察され、またSn量が
7wt％を越えるとかえつて磁気特性が劣化するの
は、焼結初期にFeとSnとの金属間化合物がSiの
拡散を妨げるためと推察される。 As is clear from Figure 2, Sn content is 0.05 to 7wt%.
The Fe-Si-Sn sintered body containing Fe-Si sintered body (Sn=Owt% in Figure 2) or Sn
Compared to Fe-Si-P sintered bodies that do not contain P (P = 1wt% in Figure 2), the sintered density is higher, so the magnetic flux density is higher, the magnetic permeability is higher, and the iron loss is lower. , exhibiting good magnetic properties. The reason why the magnetic property improvement effect is small when the Sn content is less than 0.05wt% is because the α-
This is presumed to be due to the lack of Fe phase, and the amount of Sn
The reason why the magnetic properties deteriorate when the content exceeds 7 wt% is presumed to be because the intermetallic compound of Fe and Sn prevents the diffusion of Si in the early stage of sintering.
実施例 ２
粒度80メツシユ以下のアトマイズ純鉄粉、250
メツシユ以下のフエロシリコン粉（77wt％Si）、
250メツシユ以下の金属スズ粉、および250メツシ
ユ以下のフエロリン粉（17.5wt％Ｐ）を、粉末全
体としての成分組成がSi6.5wt％、Sn1wt％、PO
〜2.5wt％となるように混合し、その混合粉末を
実施例１と同じ条件で加熱、解砕して原料粉末を
得た。EPMA観察によれば、これらの粉末は、
フエロシリコン粒子と、（Ｐを添加したものは）
フエロリン粒子と、表面にSnが濃化した鉄粉粒
子とからなり、フエロシリコン粒子およびフエロ
ン粒子の一部は鉄粉粒子に付着ないし冶金結合し
ていることがわかつた。Example 2 Atomized pure iron powder with particle size of 80 mesh or less, 250
Ferrosilicon powder (77wt%Si) below mesh size,
Metal tin powder of 250 mesh or less and ferroline powder (17.5wt%P) of 250 mesh or less are combined into powders whose composition as a whole is Si6.5wt%, Sn1wt%, PO
The mixed powder was heated and crushed under the same conditions as in Example 1 to obtain a raw material powder. According to EPMA observations, these powders
Ferrosilicon particles and (those with P added)
It was found that it consists of ferroline particles and iron powder particles with Sn concentrated on the surface, and that some of the ferrosilicon particles and ferron particles are attached to or metallurgically bonded to the iron powder particles.
成形・焼結および磁気特性測定を実施例１に準
拠した方法で行ない、第３図の結果を得た。第３
図から、0.05〜2wt％の範囲内のＰの添加により、
一層磁気特性が向上することが明らかである。 Molding, sintering and measurement of magnetic properties were carried out in accordance with the method of Example 1, and the results shown in FIG. 3 were obtained. Third
From the figure, it can be seen that by adding P within the range of 0.05 to 2 wt%,
It is clear that the magnetic properties are further improved.
発明の効果
前述の実施例からも明らかなように、この発明
の焼結磁性材料は、高い磁束密度、低い保磁力、
高い透磁率と、低い鉄損とを同時に実現し得たも
のであり、またこの発明の焼結磁性材料製造用原
料粉末によれば、そのように優れた磁気特性を有
する焼結磁性材料を容易に得ることができ、した
がつてこの発明をモーターの鉄心等の磁性部品に
適用すればその効率向上など、多大な利益を得る
ことができる。Effects of the Invention As is clear from the above examples, the sintered magnetic material of the present invention has high magnetic flux density, low coercive force,
The raw material powder for producing sintered magnetic materials of the present invention can achieve high magnetic permeability and low core loss at the same time, and it is possible to easily produce sintered magnetic materials with such excellent magnetic properties. Therefore, if this invention is applied to magnetic parts such as the iron core of a motor, great benefits such as improved efficiency can be obtained.
第１図はFe―Si合金におけるSi量と電気抵抗
率との関係を示すグラフ、第２図は実施例１にお
ける添加Sn量と焼結体の密度および各種磁気特
性との関係を示すグラフ、第３図は実施例２にお
ける添加Ｐ量と焼結体の密度および各種磁気特性
との関係を示すグラフである。
FIG. 1 is a graph showing the relationship between the amount of Si and electrical resistivity in the Fe-Si alloy, FIG. 2 is a graph showing the relationship between the amount of added Sn, the density of the sintered body, and various magnetic properties in Example 1, FIG. 3 is a graph showing the relationship between the amount of added P, the density of the sintered body, and various magnetic properties in Example 2.
Claims (1)
部が実質的にFeであることを特徴とする焼結磁
性材料。 ２ Siを１〜12wt％、Snを0.05〜7wt％、Ｐを
0.05〜2wt％含み、残部が実質的にFeであること
を特徴とする焼結磁性材料。 ３ 粉末全体としての成分組成が、Si1〜12wt
％、Sn0.05〜7wt％を含みかつ残部が実質的にFe
とされており、しかも少なくとも一部の粉末粒子
として、鉄粉粒子表面にSnが濃化して存在する
粒子を含むことを特徴とする、焼結磁性材料製造
用の原料粉末。 ４ 粉末全体としての成分組成が、Si1〜12wt
％、Sn0.05〜7wt％、P0.05〜2wt％を含みかつ残
部が実質的にFeとされており、しかも少なくと
も一部の粉末粒子として、鉄粉粒子表面にSnが
濃化して存在する粒子を含むことを特徴とする、
焼結磁性材料製造用の原料粉末。[Claims] 1. A sintered magnetic material comprising 1 to 12 wt% of Si, 0.05 to 7 wt% of Sn, and the balance being substantially Fe. 2 Si 1-12wt%, Sn 0.05-7wt%, P
A sintered magnetic material containing 0.05 to 2 wt%, with the remainder being substantially Fe. 3 The composition of the powder as a whole is Si1~12wt.
%, contains 0.05 to 7wt% of Sn, and the balance is substantially Fe.
A raw material powder for producing a sintered magnetic material, characterized in that at least some of the powder particles include particles in which Sn is present in concentrated form on the surface of iron powder particles. 4 The composition of the powder as a whole is Si1~12wt
%, Sn0.05-7wt%, P0.05-2wt%, and the remainder is substantially Fe, and Sn is present as concentrated on the surface of the iron powder particles as at least some of the powder particles. characterized by containing particles,
Raw material powder for manufacturing sintered magnetic materials.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60107691A JPS61266553A (en) | 1985-05-20 | 1985-05-20 | Sintered magnetic material and powdery starting material for manufacture sintered magnetic material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60107691A JPS61266553A (en) | 1985-05-20 | 1985-05-20 | Sintered magnetic material and powdery starting material for manufacture sintered magnetic material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61266553A JPS61266553A (en) | 1986-11-26 |
| JPH0450379B2 true JPH0450379B2 (en) | 1992-08-14 |
Family
ID=14465515
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60107691A Granted JPS61266553A (en) | 1985-05-20 | 1985-05-20 | Sintered magnetic material and powdery starting material for manufacture sintered magnetic material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61266553A (en) |
-
1985
- 1985-05-20 JP JP60107691A patent/JPS61266553A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS61266553A (en) | 1986-11-26 |
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