JPH10310842A - Production of terbium-containing magnet alloy - Google Patents
Production of terbium-containing magnet alloyInfo
- Publication number
- JPH10310842A JPH10310842A JP9120695A JP12069597A JPH10310842A JP H10310842 A JPH10310842 A JP H10310842A JP 9120695 A JP9120695 A JP 9120695A JP 12069597 A JP12069597 A JP 12069597A JP H10310842 A JPH10310842 A JP H10310842A
- Authority
- JP
- Japan
- Prior art keywords
- alloy
- magnet
- contg
- sputtering target
- target
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- Hard Magnetic Materials (AREA)
Abstract
Description
【0001】[0001]
【発明の属する技術分野】本発明はTbを含有する磁石合
金の製造方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a magnet alloy containing Tb.
【0002】[0002]
【従来の技術】光磁気記録膜用の磁性薄膜はスパッタリ
ング法で作製されており、スパッタリング・ターゲット
(以下、ターゲットと略す)はTb、Fe、Co、Crなどの合
金からなり、スパッターによって不均一に消耗され、バ
ッキングプレートがスパッターされる前に新品と交換さ
れている。スパッター条件の適性化を図ることにより、
より均一に消耗するように努力されているが、通常はタ
ーゲットの1/2 〜2/3 程度の量が未使用のままで交換さ
れる。また、このターゲットを作製する際にも合金のス
クラップが発生する。この使用済みターゲットや合金ス
クラップからTbなどの有用金属を回収するには、ターゲ
ットをバッキングプレートから剥がした後、ターゲッ
ト表面の酸化物を研削除去して、溶融する方法、酸に
溶解して、蓚酸などの沈澱剤を加えて蓚酸Tbとして回収
する方法などが知られている。2. Description of the Related Art Magnetic thin films for magneto-optical recording films are produced by a sputtering method, and a sputtering target (hereinafter abbreviated as a target) is made of an alloy such as Tb, Fe, Co, Cr, etc., and is non-uniform by sputtering. And was replaced with a new one before the backing plate was sputtered. By optimizing sputter conditions,
Efforts are made to wear more evenly, but usually about 1/2 to 2/3 of the target is replaced unused. Also, when this target is manufactured, alloy scrap is generated. To recover useful metals such as Tb from this used target and alloy scrap, remove the target from the backing plate, grind and remove the oxide on the target surface, melt it, dissolve in acid, and dissolve in oxalic acid. For example, a method of adding a precipitant such as the above and recovering as oxalate Tb is known.
【0003】[0003]
【発明が解決しようとする課題】しかし、の方法では
ターゲット組成と同じ組成の合金が得られるものの、組
織のコントロールが困難であり、現在広く使用されてい
るTb、Tb−Feの複合組織の合金ターゲットの原料として
使用することはできない。さらに酸素が増加する問題が
あり、使用済みターゲットを原料として作製した光磁気
記録膜は特性の低下を避けることができなかった。また
の方法では、高価な希土類成分を回収するには効果的
であるが、酸溶解や沈澱の濾過回収、さらには金属とし
て使用する場合には還元する必要があるなどの問題点が
あり、より簡便で効果的な使用済みターゲットや合金ス
クラップの活用法が望まれていた。However, in the above method, although an alloy having the same composition as the target composition can be obtained, it is difficult to control the structure, and an alloy having a composite structure of Tb and Tb-Fe which is widely used at present is used. It cannot be used as a target material. Further, there is a problem that oxygen is increased, and a magneto-optical recording film manufactured using a used target as a raw material cannot avoid deterioration in characteristics. The other method is effective for recovering expensive rare earth components, but has problems such as acid dissolution and filtration and recovery of the precipitate, and further, when used as a metal, it needs to be reduced. There has been a demand for a simple and effective method of utilizing used targets and alloy scrap.
【0004】一方、Nd系磁石においてNdの一部をTbで置
換することにより保磁力が向上することは知られてい
る。しかしTbメタルは高価であることから、工業的には
一般に使用されてはいなかった。[0004] On the other hand, it is known that coercive force is improved by replacing a part of Nd with Tb in an Nd-based magnet. However, Tb metal has not been widely used industrially because of its high cost.
【0005】[0005]
【課題を解決するための手段】本発明者らは上記問題点
に鑑み、使用済みターゲットの有効な活用方法及びNd系
磁石特性の向上について鋭意検討を重ねた結果、本発明
を完成させた。すなわち本発明は、Tbメタルを含有する
光磁気用使用済みスパッタリング・ターゲットを、少な
くともNd、Fe、Bまたはこれらを含む合金と溶融するこ
とを特徴とするTb含有磁石合金の製造方法である。以
下、本発明を詳細に説明する。Means for Solving the Problems In view of the above problems, the present inventors have made intensive studies on how to effectively use a used target and to improve the properties of Nd-based magnets, and as a result, completed the present invention. That is, the present invention is a method for producing a Tb-containing magnet alloy, comprising melting a used sputtering target for magneto-optics containing Tb metal with at least Nd, Fe, B or an alloy containing these. Hereinafter, the present invention will be described in detail.
【0006】[0006]
【発明の実施の形態】本発明はTbを含有する使用済みタ
ーゲットをそのまま特殊な処理をすることなく磁石合金
の製造用原料として使用するものであり、より詳細に
は、バッキングプレートから剥がした使用済みターゲッ
トをNd-Fe-B系磁石合金を製造するにあたり、磁石用金
属原料と共に溶融し、Tbの添加されたNd-Fe-B系磁石合
金を製造する。また、このターゲットを作製する際に発
生するTbメタル含有合金スクラップも、使用済みターゲ
ットと同様に磁石合金の製造用原料として使用すること
ができる。BEST MODE FOR CARRYING OUT THE INVENTION The present invention is to use a used target containing Tb as a raw material for producing a magnetic alloy without special treatment as it is, and more specifically, to use the target removed from a backing plate. In producing the Nd-Fe-B-based magnet alloy, the used target is melted together with the metal material for the magnet to produce an Nd-Fe-B-based magnet alloy to which Tb is added. In addition, Tb metal-containing alloy scrap generated when manufacturing this target can also be used as a raw material for producing a magnet alloy, like the used target.
【0007】本発明に用いる使用済みターゲットまたは
合金スクラップは、Tb約30〜50wt%、Fe約40〜60wt% 、C
o約3〜10wt% が含まれているTb-Fe-Co系合金や、またT
b約40〜60wt% 、Fe約40〜60wt% 、Co約3〜10wt% 、Cr
約0.5 〜5wt% が含まれているTb-Fe-Co-Cr 系合金がよ
い。Feは磁石の主成分であり、Coは耐食性の向上に、Cr
は保磁力の向上に効果的であり、Tbメタル単独で磁石合
金に添加するよりも使用済みターゲットの方が、磁石特
性の改善効果が大きいという利点もある。また酸素の含
有量は、磁気特性を低下させないために、0.5wt%以下が
好ましい。The used target or alloy scrap used in the present invention is composed of about 30 to 50 wt% of Tb, about 40 to 60 wt% of Fe,
o Tb-Fe-Co alloy containing about 3-10wt%
b about 40-60 wt%, Fe about 40-60 wt%, Co about 3-10 wt%, Cr
A Tb-Fe-Co-Cr alloy containing about 0.5 to 5 wt% is preferable. Fe is the main component of the magnet, and Co is
Is effective in improving coercive force, and there is also an advantage that a used target has a greater effect of improving magnet properties than adding Tb metal alone to a magnetic alloy. The content of oxygen is preferably 0.5% by weight or less so as not to deteriorate the magnetic properties.
【0008】使用済みターゲットや合金スクラップと共
に溶融する磁石用金属原料は、少なくともNd、Fe、Bま
たはこれらを含む合金である。他の金属原料としては例
えばAl、Co、Dyなどが挙げられる。[0008] The magnet raw material to be melted together with the used target and alloy scrap is at least Nd, Fe, B or an alloy containing these. Examples of other metal raw materials include Al, Co, and Dy.
【0009】溶融は、従来公知の方法で行えばよいが、
量産性の点から、高周波誘導溶解炉で溶融するのが好ま
しい。また、組成調整を容易にするために、使用済みタ
ーゲットや合金スクラップは予め溶融し、均質な回収合
金としてから、磁石用金属原料と共に溶融すれば好適で
ある。The melting may be performed by a conventionally known method.
From the viewpoint of mass production, it is preferable to melt in a high frequency induction melting furnace. In addition, in order to facilitate the composition adjustment, it is preferable that the used target and the alloy scrap are melted in advance to form a homogeneous recovered alloy, and then melted together with the metal raw material for the magnet.
【0010】[0010]
【実施例】次に、本発明の実施例について説明する。 実施例1 光磁気記録膜用の磁性薄膜をスパッタリング法で作製し
た際の、Tbを含有する使用済みターゲットを、スパッタ
リング装置のバッキングプレートを加熱して剥がし、付
着しているボンディング剤を研磨して除去した。この使
用済みターゲット10枚を高周波誘導溶解炉で溶融して、
均質な回収合金Aを得た。この組成はTb41wt%、Fe 52wt
%、Co 7wt% であり、酸素は 0.30wt%であった。また
これとは別に、光磁気用ターゲットの製造時に発生し
た、Tbを含有する合金スクラップ6kgを、使用済みター
ゲット5枚と共に高周波誘導溶解炉で溶融して、均質な
回収合金Bを得た。この組成はTb 46wt%、Fe 45wt%、Co
7wt% 、Cr2wt% であり、酸素は 0.28wt%であった。
回収合金Aと、Nd、フェロボロン、電解鉄、アルミニウ
ムを所定量配合して表1に記載の組成とし、高周波誘導
溶解炉で溶融して磁石合金を製造した。これに公知の磁
石製造方法に従い、粉砕、成形、焼結、時効を行って焼
結磁石合金を製造し、その磁気特性を測定した。測定結
果を表1に記す。Next, an embodiment of the present invention will be described. Example 1 When a magnetic thin film for a magneto-optical recording film was prepared by a sputtering method, a used target containing Tb was peeled off by heating a backing plate of a sputtering apparatus, and the attached bonding agent was polished. Removed. These ten used targets are melted in a high-frequency induction melting furnace,
A homogeneous recovered alloy A was obtained. This composition is Tb41wt%, Fe52wt
%, Co 7 wt%, and oxygen 0.30 wt%. Separately, 6 kg of alloy scrap containing Tb generated during the production of the magneto-optical target was melted together with the five used targets in a high-frequency induction melting furnace to obtain a homogeneous recovered alloy B. This composition is Tb 46wt%, Fe 45wt%, Co
The content was 7 wt%, Cr 2 wt%, and oxygen was 0.28 wt%.
The recovered alloy A, Nd, ferroboron, electrolytic iron, and aluminum were blended in predetermined amounts to obtain the composition shown in Table 1, and were melted in a high frequency induction melting furnace to produce a magnet alloy. According to a known magnet manufacturing method, the magnet was subjected to pulverization, molding, sintering and aging to produce a sintered magnet alloy, and its magnetic properties were measured. Table 1 shows the measurement results.
【0011】[0011]
【表1】 [Table 1]
【0012】実施例2 回収合金Bを使用し、表1に記載の組成とした以外は実
施例1と同じ条件で、磁石合金を作製し、磁気特性を測
定した。測定結果を表1に併記する。Example 2 A magnet alloy was prepared and the magnetic properties were measured under the same conditions as in Example 1 except that the recovered alloy B was used and the composition shown in Table 1 was used. Table 1 also shows the measurement results.
【0013】実施例3 回収合金Aを使用し、表1に記載の組成とした以外は実
施例1と同じ条件で、磁石合金を作製し、磁気特性を測
定した。測定結果を表1に併記する。Example 3 A magnet alloy was prepared and the magnetic properties were measured under the same conditions as in Example 1 except that the recovered alloy A was used and the composition shown in Table 1 was used. Table 1 also shows the measurement results.
【0014】実施例4 回収合金Bを使用し、表1に記載の組成とした以外は実
施例1と同じ条件で、磁石合金を作製し、磁気特性を測
定した。測定結果を表1に併記する。Example 4 A magnet alloy was prepared and the magnetic properties were measured under the same conditions as in Example 1 except that the recovered alloy B was used and the compositions shown in Table 1 were used. Table 1 also shows the measurement results.
【0015】比較例1 回収合金を使用せず、表1に記載の組成とした以外は実
施例1と同じ条件で、磁石合金を作製し、磁気特性を測
定した。結果を表1に併記する。Comparative Example 1 A magnet alloy was prepared and the magnetic properties were measured under the same conditions as in Example 1 except that the recovered alloy was not used and the compositions shown in Table 1 were used. The results are also shown in Table 1.
【0016】比較例2 回収合金を使用せず、かつTbメタルを2wt%使用して実
施例1と同じ組成とした以外は、実施例1と同じ条件で
磁石合金を作製し、磁気特性を測定した。結果を表1に
併記する。Comparative Example 2 A magnet alloy was manufactured under the same conditions as in Example 1 except that the recovered alloy was not used and the composition was the same as that of Example 1 except that 2 wt% of Tb metal was used, and the magnetic properties were measured. did. The results are also shown in Table 1.
【0017】[0017]
【発明の効果】本発明によれば、磁気特性、特に保磁力
に優れたNd-Fe-B系焼結磁石が得られる。また、高価な
Tbメタルを使用した場合と同等の優れた磁気特性を得る
ことができ、工業的価値は非常に大きい。According to the present invention, an Nd-Fe-B sintered magnet having excellent magnetic properties, particularly excellent coercive force, can be obtained. Also expensive
The same excellent magnetic properties as when using Tb metal can be obtained, and the industrial value is very large.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 徳井 均臣 東京都千代田区大手町2丁目6番1号 信 越化学工業株式会社本社内 (72)発明者 山本 健治 福井県武生市北府2丁目1番5号 信越化 学工業株式会社磁性材料研究所内 ──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Hitomi Tokui 2-6-1 Otemachi, Chiyoda-ku, Tokyo Shin-Etsu Chemical Co., Ltd. (72) Inventor Kenji Yamamoto 2-1-1 Kitafu, Takefu-shi, Fukui Prefecture No. 5 Shin-Etsu Kagaku Kogyo Co., Ltd. Magnetic Materials Research Laboratory
Claims (5)
パッタリング・ターゲットを、少なくともNd、Fe、Bま
たはこれらを含む合金と溶融することを特徴とするTb含
有磁石合金の製造方法。1. A method for producing a Tb-containing magnet alloy, comprising melting a used sputtering target for magneto-optics containing Tb metal with at least Nd, Fe, B or an alloy containing them.
ップを、少なくともNd、Fe、Bまたはこれらを含む合金
と溶融することを特徴とするTb含有磁石合金の製造方
法。2. A method for producing a Tb-containing magnet alloy, comprising melting a scrap of magneto-optical alloy containing Tb metal with at least Nd, Fe, B or an alloy containing these.
び/または合金スクラップがTb-Fe-Co系合金である請求
項1または2に記載のTb含有磁石合金の製造方法。3. The method for producing a Tb-containing magnet alloy according to claim 1, wherein the used sputtering target and / or alloy scrap is a Tb—Fe—Co alloy.
び/または合金スクラップがTb-Fe-Co-Cr 系合金である
請求項1または2に記載のTb含有磁石合金の製造方法。4. The method for producing a Tb-containing magnet alloy according to claim 1, wherein the used sputtering target and / or alloy scrap is a Tb-Fe-Co-Cr alloy.
項1乃至4のいずれか一項に記載のTb含有磁石合金の製
造方法。5. The method for producing a Tb-containing magnet alloy according to claim 1, wherein the melting is performed in a high-frequency induction melting furnace.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP9120695A JPH10310842A (en) | 1997-05-12 | 1997-05-12 | Production of terbium-containing magnet alloy |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP9120695A JPH10310842A (en) | 1997-05-12 | 1997-05-12 | Production of terbium-containing magnet alloy |
Publications (1)
Publication Number | Publication Date |
---|---|
JPH10310842A true JPH10310842A (en) | 1998-11-24 |
Family
ID=14792694
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP9120695A Pending JPH10310842A (en) | 1997-05-12 | 1997-05-12 | Production of terbium-containing magnet alloy |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPH10310842A (en) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1076853C (en) * | 1999-01-06 | 2001-12-26 | 宁波韵升强磁材料有限公司 | Method for making Nd-Fe-B series permanent magnet by using leftover bits and pieces of material |
WO2010071048A1 (en) * | 2008-12-17 | 2010-06-24 | Tanakaホールディングス株式会社 | Method for recovering metal from target and target manufacturing method |
JP2011214104A (en) * | 2010-03-31 | 2011-10-27 | Tanaka Kikinzoku Kogyo Kk | Method for recovering metal from target and method for manufacturing target |
-
1997
- 1997-05-12 JP JP9120695A patent/JPH10310842A/en active Pending
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1076853C (en) * | 1999-01-06 | 2001-12-26 | 宁波韵升强磁材料有限公司 | Method for making Nd-Fe-B series permanent magnet by using leftover bits and pieces of material |
WO2010071048A1 (en) * | 2008-12-17 | 2010-06-24 | Tanakaホールディングス株式会社 | Method for recovering metal from target and target manufacturing method |
US8287804B2 (en) | 2008-12-17 | 2012-10-16 | Tanaka Holdings Co., Ltd | Method for recovering metal from target and method for manufacturing target |
JP2011214104A (en) * | 2010-03-31 | 2011-10-27 | Tanaka Kikinzoku Kogyo Kk | Method for recovering metal from target and method for manufacturing target |
US8366800B2 (en) | 2010-03-31 | 2013-02-05 | Tanaka Kikinzoku Kogyo K.K. | Method for recovering metal from target and method for manufacturing target |
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