JPH0323606B2 - - Google Patents
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- Publication number
- JPH0323606B2 JPH0323606B2 JP60186575A JP18657585A JPH0323606B2 JP H0323606 B2 JPH0323606 B2 JP H0323606B2 JP 60186575 A JP60186575 A JP 60186575A JP 18657585 A JP18657585 A JP 18657585A JP H0323606 B2 JPH0323606 B2 JP H0323606B2
- Authority
- JP
- Japan
- Prior art keywords
- sintering
- heat treatment
- temperature
- soft magnetic
- cooling
- 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 - Lifetime
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- Powder Metallurgy (AREA)
- Soft Magnetic Materials (AREA)
Description
【発明の詳細な説明】
〔概要〕
Fe−Co焼結材料を焼結後急冷を伴なう熱処理
することによつて、保磁力、磁束密度および透磁
率等の軟質磁気特性を改良する。DETAILED DESCRIPTION OF THE INVENTION [Summary] Soft magnetic properties such as coercive force, magnetic flux density, and magnetic permeability are improved by heat-treating an Fe-Co sintered material with rapid cooling after sintering.
本発明は軟質磁性材料に関するものであり、さ
らに詳しく述べるならばFe−Co系焼結軟質磁性
材料の製造方法に関するものである。
The present invention relates to a soft magnetic material, and more specifically, to a method for producing a Fe--Co based sintered soft magnetic material.
従来軟質磁性材料として、鉄、ケイ素鋼、パー
マロイ、センダスト、パーメンジユールなどが広
く実用されている。これらの中で最も高い磁束密
度を示すものはパーメンジユールであるが、その
溶製材は冷間加工性が乏しいという欠点があつ
た。そこで、バナジウムを２％添加することによ
り冷間加工性を改善した2V−パーメンジユール
が知られているが、その加工性は未だ十分とは言
えない。粉末治金法は難加工性材料を成形加工す
る有力な一つの製造方法であるが、Fe−Co系合
金を粉末治金法で製造すると溶製材に匹敵するほ
どの軟質磁気特性が得られていなかつた。これを
解決するために種々の添加物の硬化も調べられて
いるが、軟質磁気的性質を根本的に解決するに至
つていない。
Conventionally, iron, silicon steel, permalloy, sendust, permendile, and the like have been widely used as soft magnetic materials. Among these materials, permendile exhibits the highest magnetic flux density, but its ingot material has the disadvantage of poor cold workability. Therefore, 2V-permendile is known, which has improved cold workability by adding 2% vanadium, but its workability is still not sufficient. Powder metallurgy is an effective manufacturing method for molding difficult-to-process materials, but when Fe-Co alloys are manufactured using powder metallurgy, soft magnetic properties comparable to molten materials cannot be obtained. Nakatsuta. In order to solve this problem, hardening of various additives has been investigated, but the soft magnetic properties have not been fundamentally solved.
従来、Fe−Co系軟質磁性合金を焼結する際に
その相対密度を高めることにより軟質磁気的性質
を改善することは試みられていた。だが、鉄のコ
バルトへの拡散係数がコバルトの鉄への拡散係数
より大であるために、鉄相にカーゲンドールボイ
ドが発生すること、および高温焼結時における
Fe−Co合金の焼結構造（FCC相）に起因して焼
結時の拡散が遅くなることは二つの理由によつて
焼結体の密度向上には限界があつた。さらに、添
加元素によつても焼結体の密度は根本的には改善
されておらなかつた。
Conventionally, attempts have been made to improve the soft magnetic properties of Fe--Co based soft magnetic alloys by increasing their relative density when sintering them. However, because the diffusion coefficient of iron to cobalt is larger than the diffusion coefficient of cobalt to iron, Kagendall voids occur in the iron phase and during high-temperature sintering.
There are two reasons why diffusion during sintering is slow due to the sintered structure (FCC phase) of Fe-Co alloys, which limits the ability to increase the density of sintered bodies. Furthermore, the density of the sintered body was not fundamentally improved even by the addition of elements.
本発明は実用性のある磁気的性質を有するFe
−Co系焼結軟磁性材料を提供する方法を見出す
ことを目的とする。 The present invention is based on Fe having practical magnetic properties.
- The purpose of the present invention is to find a method for providing a Co-based sintered soft magnetic material.
本発明は、Fe−Co合金を焼結した後に、750〜
900℃の温度で熱処理を行い、更に急冷処理を施
すことによつてFe−Co焼結軟質磁性材料の磁気
的性質を改良するものである。
In the present invention, after sintering Fe-Co alloy,
The magnetic properties of the Fe-Co sintered soft magnetic material are improved by heat treatment at a temperature of 900°C and further rapid cooling treatment.
本発明において、焼結とは通常の粉末混合、圧
粉および焼成を経る粉末治金法の一連の工程を指
す。この焼結法における各工程の条件には特に制
限がないが、相対密度90〜96％を得る通常の、す
なわちHIP等の特殊な方法によらない、焼結法に
よつて得られた焼結体にも本発明方法を適用する
ことができる。本発明において、焼結後とは通常
の焼結体としての密度、均一組成が得られた後を
意味している。かかる焼結体が得られた後にこれ
に再び熱的処理を加え軟質磁気的性質を改善する
ことが本発明の特徴である。通常焼結は高温加熱
後室温まで冷却することにより終了するので、室
温から所定温度まで再加熱することにより熱処理
を行なう。この場合、焼結体の供給を受けたユー
ザーが熱処理しても所期の効果が得られるのは当
然であり、熱処理の時期は問わない。また、焼結
後所定熱処理温度まで冷却した後直ちに熱処理を
行なつてもよい。本発明において熱処理で急冷を
行なうのは磁気的性質改良のために急冷が一つの
条件になつているからである。急冷としては、炉
冷より実質的に冷却速度が速い油冷、空冷、水
冷、扇冷、気体ジエツト冷却、低温浴中への浸せ
きなど各種方法あるいはこれらの混合併用方法を
採用することができる。ところで本発明における
熱処理の作用は後述のようにFe−Co規則格子を
解除するところにあるとするのが有力であるた
め、熱処理における急冷は規則格子生成温度範囲
にて行なうことが必要と考えられる。焼結Fe−
Co合金の規則格子生成温度を明確に定めること
は出来ないが、高温域を急冷することが安全であ
る。規則格子生成の危険性が低い低温域および
高々温域での急冷は必須ではない。 In the present invention, sintering refers to a series of steps in a powder metallurgy process including conventional powder mixing, powder compaction, and sintering. There are no particular restrictions on the conditions for each step in this sintering method, but sintered products obtained by a normal sintering method that achieves a relative density of 90 to 96%, that is, not using a special method such as HIP. The method of the present invention can also be applied to the body. In the present invention, "after sintering" means after the density and uniform composition of a normal sintered body have been obtained. A feature of the present invention is that after such a sintered body is obtained, it is subjected to heat treatment again to improve its soft magnetic properties. Normally, sintering is completed by heating to a high temperature and then cooling to room temperature, so heat treatment is performed by reheating from room temperature to a predetermined temperature. In this case, it is natural that the desired effect can be obtained even if the user who receives the sintered body performs heat treatment, and the timing of the heat treatment does not matter. Alternatively, the heat treatment may be performed immediately after cooling to a predetermined heat treatment temperature after sintering. The reason why quenching is performed in the heat treatment in the present invention is that quenching is one of the conditions for improving magnetic properties. For rapid cooling, various methods such as oil cooling, air cooling, water cooling, fan cooling, gas jet cooling, and immersion in a low-temperature bath, which have a substantially faster cooling rate than furnace cooling, or a combination of these methods can be employed. By the way, it is likely that the effect of the heat treatment in the present invention is to release the Fe-Co ordered lattice as described below, and therefore it is considered necessary to perform the rapid cooling in the heat treatment within the temperature range for forming an ordered lattice. . Sintered Fe−
Although it is not possible to clearly determine the temperature at which ordered lattice formation occurs in Co alloys, it is safe to rapidly cool the high temperature region. Rapid cooling in a low temperature range or a high temperature range where the risk of forming an ordered lattice is low is not essential.
本発明者等は熱的処理温度と磁性改善の関係を
調べたところが750〜900℃にて十分な効果を認め
た。このように本発明の熱処理温が750〜900℃で
十分な効果を示す理由を以下に説明する。 The present inventors investigated the relationship between thermal treatment temperature and magnetic improvement and found that a sufficient effect was observed at 750 to 900°C. The reason why the present invention exhibits sufficient effects at a heat treatment temperature of 750 to 900°C will be explained below.
Fe−50％Co合金は985〜1480℃にて常磁性のγ
相となることが知られている。従つてこの温度領
域から室温まで急冷すると、完全な急冷が行われ
た場合は全相がγ相となる。また、不完全な急冷
の場合は室温で主相であるα相（強磁性相）と残
留γ相の混相となる。いずれにしても強磁性のα
相の形成が常磁性のγ相によつて妨害されること
となり、強磁性体の製造法としては好ましくな
い。以上の理由から、985℃より高い温度領域で
の熱処理は除外される。 Fe-50%Co alloy becomes paramagnetic γ at 985-1480℃
It is known to be a phase. Therefore, when the material is rapidly cooled from this temperature range to room temperature, all phases become the γ phase if complete rapid cooling is performed. In addition, in the case of incomplete quenching, a mixed phase of the main phase α phase (ferromagnetic phase) and residual γ phase is formed at room temperature. In any case, ferromagnetic α
This is not preferred as a method for producing ferromagnetic materials because phase formation is hindered by the paramagnetic γ phase. For the above reasons, heat treatment in a temperature range higher than 985°C is excluded.
一方、Fe−50％Co合金は730℃付近に規則−不
規則変態点を有する。従つてこの温度より低い温
度では規則化しやすく、急冷を施しても規則化を
完全に阻止することが困難となる。以上の理由か
ら730℃より低い温度領域での熱処理は除外され
る。 On the other hand, Fe-50%Co alloy has a regular-disorder transformation point around 730°C. Therefore, at temperatures lower than this temperature, ordering is likely to occur, and even if rapid cooling is performed, it is difficult to completely prevent ordering. For the above reasons, heat treatment in a temperature range lower than 730°C is excluded.
上述した理由のみでは730〜985℃における熱処
理が好ましいこととなるが730℃の近傍では規則
化が開始すること、および985℃の近傍ではγ相
が混入することを考慮し、Fe−Co合金で安全を
見て750〜900℃の範囲とした。 For the above reasons alone, heat treatment at 730 to 985°C is preferable, but considering that ordering begins near 730°C and γ phase is mixed near 985°C, it is preferable to heat treat at 730 to 985°C. For safety reasons, the temperature was set in the range of 750 to 900 degrees Celsius.
本発明のFe−Co焼結軟質磁性材料の組成は公
知のものであつてよく、Fe：Co原子比＝１：１、
残部不純物であるFe−Co合金も本発明によりす
ぐれた軟質磁性材料として改質される。 The composition of the Fe-Co sintered soft magnetic material of the present invention may be a known one, including Fe:Co atomic ratio = 1:1,
The Fe--Co alloy, which is the remaining impurity, is also modified into an excellent soft magnetic material according to the present invention.
FeCo規則格子は飽和磁束密度は高いが透磁率
は低い。一般のFe−Co磁性材料ではこのような
Fe−Co規則格子の性質が利用されている。本発
明における急冷を伴なう熱処理は、規則化を解除
し、透磁率を高めるとともに保磁力を低下させる
作用を有すると考えられる。加えて、急冷を伴な
う熱処理によつて磁束密度B4Kも高められる。
FeCo ordered lattice has high saturation magnetic flux density but low magnetic permeability. In general Fe-Co magnetic materials, such
The properties of the Fe-Co regular lattice are utilized. It is thought that the heat treatment accompanied by rapid cooling in the present invention has the effect of canceling regularization, increasing magnetic permeability, and lowering coercive force. In addition, the magnetic flux density B 4K can also be increased by heat treatment accompanied by rapid cooling.
以下、本発明の実施例を説明する。 Examples of the present invention will be described below.
実施例 １
原料粉として、−200meshの電解Fe粉、400メ
ツシユの還元Co粉およびアトマイズFe−50％Co
合金粉を用意し、この合金粉の重量％が第１図の
横軸に示す値となるように原料粉を混合し、さら
に潤滑剤として0.75質量％のステアリン酸亜鉛を
加えて混合した。これらの混合粉を392MPa
（4t／cm2）の成形圧力でφ45mm×φ35mm×７mm
（ｔ）の形状に圧粉成形した。その後、400℃にお
いて圧粉体より前述の潤滑剤を除去してから、
750−850℃において１時間、水素雰囲気にて予備
焼結し、さらに588MPa（6t／cm2）の圧力で再圧
縮成形した。焼結は、プツシヤ型水素雰囲気炉に
て1300〜1400℃にて１時間行なつた。この後、管
状雰囲気炉により、水素雰囲気にて800〜900℃で
１時間保持してから油冷で急冷した。
Example 1 Raw material powders were -200 mesh electrolytic Fe powder, 400 mesh reduced Co powder, and atomized Fe-50% Co.
An alloy powder was prepared, and raw material powder was mixed so that the weight percent of the alloy powder became the value shown on the horizontal axis in FIG. 1, and 0.75 mass percent zinc stearate was added as a lubricant and mixed. These mixed powders are heated to 392MPa
(4t/cm 2 ) molding pressure φ45mm×φ35mm×7mm
It was compacted into the shape of (t). Then, after removing the aforementioned lubricant from the green compact at 400℃,
Preliminary sintering was carried out in a hydrogen atmosphere at 750-850°C for 1 hour, followed by recompression molding at a pressure of 588 MPa (6 t/cm 2 ). Sintering was performed at 1300 to 1400° C. for 1 hour in a pusher type hydrogen atmosphere furnace. Thereafter, the mixture was kept at 800 to 900°C for 1 hour in a hydrogen atmosphere using a tubular atmosphere furnace, and then quenched with oil.
〔磁気的性質〕 得られた焼結合金に励磁コイル
およびサーチコイルを共に42ターン巻き、最大
印加磁場4KA／ｍ（500e）にて直流自記磁束計
によりBHヒステリシス曲線を描いて磁束密度
（B4K）、保磁力（Hc）および最大透磁率（μ
ｍ）を求めた。この結果を示す第１図から明ら
かなように、焼結後の熱処理により、軟質磁性
材料として好ましい磁気的性質（高磁束密度、
低保磁力、高透磁率）を向上することができ
た。[Magnetic properties] Both the excitation coil and the search coil were wound with 42 turns around the obtained sintered alloy, and the magnetic flux density (B 4K ), coercive force (Hc) and maximum permeability (μ
m) was calculated. As is clear from Figure 1, which shows this result, the heat treatment after sintering has the desirable magnetic properties (high magnetic flux density, high magnetic flux density,
low coercive force, high magnetic permeability).
〔相対比重〕 焼結体の相対比重は90〜96％であ
つた。[Relative specific gravity] The relative specific gravity of the sintered body was 90 to 96%.
比較例 １
実施例１における熱処理後の油冷を炉冷に変え
た他は同様の方法で試験を行なつた結果を第２図
に示す。同図より熱処理の際の冷却が炉冷である
と磁気的性質が何ら改善されないことが分かる。Comparative Example 1 FIG. 2 shows the results of a test conducted in the same manner as in Example 1, except that oil cooling after heat treatment was changed to furnace cooling. From the figure, it can be seen that if the cooling during heat treatment is furnace cooling, the magnetic properties are not improved at all.
本発明によれば焼結後に熱処理を行なうだけで
実用性のある磁気的性質を有するFe−Co合金を
得ることができる。
According to the present invention, an Fe--Co alloy having practical magnetic properties can be obtained by simply performing heat treatment after sintering.
第１図および第２図は磁気的性質に及ぼす熱処
理の影響を示すグラフであつて、前者は実施例
１、後者は比較例１の結果を示す。
1 and 2 are graphs showing the influence of heat treatment on magnetic properties, with the former showing the results of Example 1 and the latter showing the results of Comparative Example 1.
Claims (1)
温度で熱処理を行い、更に急冷処理を施して磁気
特性を向上させることを特徴とするFe−Co軟質
磁性材料の製造方法。 ２ 前記Fe−Co軟質磁性材料のFe／Co原子比が
実質的に１であることを特徴とする特許請求の範
囲第１項記載の製造方法。 ３ 前記熱処理を焼結温度より低い温度で行なう
ことを特徴とする特許請求の範囲第１項または第
２項記載の方法。 ４ 前記Fe−Co軟質磁性材料のFe，Co以外は不
純物である特許請求の範囲第２項記載の方法。 ５ 前記焼結を相対密度90〜96％の焼結体を得る
焼結法により製造する特許請求の範囲第１項から
第４項までの何れか１項に記載の方法。[Claims] 1. An Fe-Co soft magnetic material characterized in that after sintering an Fe-Co alloy, heat treatment is performed at a temperature of 750 to 900°C, and further rapid cooling treatment is performed to improve magnetic properties. manufacturing method. 2. The manufacturing method according to claim 1, wherein the Fe--Co soft magnetic material has an Fe/Co atomic ratio of substantially 1. 3. The method according to claim 1 or 2, wherein the heat treatment is performed at a temperature lower than the sintering temperature. 4. The method according to claim 2, wherein components other than Fe and Co in the Fe--Co soft magnetic material are impurities. 5. The method according to any one of claims 1 to 4, wherein the sintering is performed by a sintering method that obtains a sintered body with a relative density of 90 to 96%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18657585A JPS6263617A (en) | 1985-08-27 | 1985-08-27 | Manufacture of fe-co soft magnetic material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18657585A JPS6263617A (en) | 1985-08-27 | 1985-08-27 | Manufacture of fe-co soft magnetic material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6263617A JPS6263617A (en) | 1987-03-20 |
| JPH0323606B2 true JPH0323606B2 (en) | 1991-03-29 |
Family
ID=16190937
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP18657585A Granted JPS6263617A (en) | 1985-08-27 | 1985-08-27 | Manufacture of fe-co soft magnetic material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6263617A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02125835A (en) * | 1988-11-04 | 1990-05-14 | Sumitomo Metal Mining Co Ltd | Manufacture of fe-co alloy soft magnetic material sintered body |
| CN112170834A (en) * | 2019-07-02 | 2021-01-05 | 宁波盛事达磁业有限公司 | A process and device for improving the magnetic properties of powder AlNiCo magnets |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3744248A (en) * | 1972-04-10 | 1973-07-10 | Gen Motors Corp | Catalytic convertor temperature control system |
-
1985
- 1985-08-27 JP JP18657585A patent/JPS6263617A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6263617A (en) | 1987-03-20 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |