JPH01117303A - Permanent magnet - Google Patents
Permanent magnetInfo
- Publication number
- JPH01117303A JPH01117303A JP62274799A JP27479987A JPH01117303A JP H01117303 A JPH01117303 A JP H01117303A JP 62274799 A JP62274799 A JP 62274799A JP 27479987 A JP27479987 A JP 27479987A JP H01117303 A JPH01117303 A JP H01117303A
- Authority
- JP
- Japan
- Prior art keywords
- magnet
- layer
- coercive force
- diffusing
- permanent magnet
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910052771 Terbium Inorganic materials 0.000 claims abstract description 10
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 9
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 8
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 5
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 5
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 4
- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract description 4
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 4
- 229910052691 Erbium Inorganic materials 0.000 claims abstract description 3
- 229910052689 Holmium Inorganic materials 0.000 claims abstract description 3
- 229910052765 Lutetium Inorganic materials 0.000 claims abstract description 3
- 229910052777 Praseodymium Inorganic materials 0.000 claims abstract description 3
- 229910052772 Samarium Inorganic materials 0.000 claims abstract description 3
- 229910052775 Thulium Inorganic materials 0.000 claims abstract description 3
- 229910052769 Ytterbium Inorganic materials 0.000 claims abstract description 3
- 229910052693 Europium Inorganic materials 0.000 claims description 3
- -1 Pm Inorganic materials 0.000 claims 1
- 230000002427 irreversible effect Effects 0.000 abstract description 13
- 238000000034 method Methods 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 8
- 238000010438 heat treatment Methods 0.000 abstract description 6
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 6
- 239000013077 target material Substances 0.000 abstract description 5
- 238000004544 sputter deposition Methods 0.000 abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 15
- 230000005347 demagnetization Effects 0.000 description 14
- 239000012298 atmosphere Substances 0.000 description 6
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical group [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 6
- 239000012299 nitrogen atmosphere Substances 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 5
- 229910052796 boron Inorganic materials 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 239000000956 alloy Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 3
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- 229910052773 Promethium Inorganic materials 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 1
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- VQMWBBYLQSCNPO-UHFFFAOYSA-N promethium atom Chemical compound [Pm] VQMWBBYLQSCNPO-UHFFFAOYSA-N 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0293—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Hard Magnetic Materials (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、Ｒ−Ｐｅ −Ｂ系の永久磁石に関し、更に詳
しくは高温不可逆減磁率の小さな永久磁石に関する。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to an R--Pe--B permanent magnet, and more particularly to a permanent magnet with a small high-temperature irreversible demagnetization rate.
（従来の技術）
従来、この種の永久磁石の一例としては組成比Ｎｄ＋□
、ｂＤＹ１．ａ Ｐｅｔｓ、２Ｂ？ＡＩ０．８から成る
Ｒ（希土類元素ここではＮｄ：ネオジムとＤｙ＝ジスプ
ロシウム） −Ｆｅ（鉄） −Ｂ （ホウ素）系の焼結
型磁石が知られており、該磁石は最大エネルギー積Ｂ
ＨＩ ａ Ｘが３５ＭＧＯｅと極めて高い優れた磁気特
性を有する。(Prior art) Conventionally, as an example of this type of permanent magnet, the composition ratio Nd+□
, bDY1. a Pets, 2B? A sintered magnet of the R (rare earth element, here Nd: neodymium and Dy = dysprosium) -Fe (iron) -B (boron) system consisting of AI0.8 is known, and this magnet has a maximum energy product B
It has excellent magnetic properties with extremely high HI a X of 35 MGOe.
（発明が解決しようとする問題点）
しかしながら前記Ｒ−Ｆｅ −Ｂ系磁石はキューリー点
が低く熱安定性が悪いため高温不可逆減磁率が一１５％
と極めて大きいという問題がある。(Problems to be Solved by the Invention) However, the R-Fe-B magnet has a low Curie point and poor thermal stability, so the high temperature irreversible demagnetization rate is 115%.
The problem is that it is extremely large.
そこで前記Ｒ−ｒｅ −Ｂ系磁石の希土類元素成分中の
Ｎｄｍの一部をＤｙに置換し該Ｄｙ量を増加せしめるこ
とが考えられる。そして前記Ｒ−Ｐｅ −Ｂ系磁石中の
両希土類元素組成比Ｎｄ＋□、６：Ｄｙ＋、４を例えば
Ｎｄｓ １．２ ： Ｄｙｚ、 ｔｒとしたとき固有保
磁力１ｆ（ｃが増大し高温不可逆減磁率は一３％と極め
て小さくなるが、それに伴なって残留磁束密度Ｂｒが小
さくなり、その結果最大エネルギー積ＢＨＷａＸが大幅
に低下するという問題がある。Therefore, it is conceivable to replace a part of Ndm in the rare earth element component of the R-re-B magnet with Dy to increase the amount of Dy. When the composition ratio of both rare earth elements Nd+□, 6:Dy+, 4 in the R-Pe-B system magnet is, for example, Nds 1.2: Dyz, tr, the intrinsic coercive force 1f (c increases and the high temperature irreversible demagnetization rate is extremely small at -3%, but there is a problem in that the residual magnetic flux density Br is accordingly reduced, and as a result, the maximum energy product BHWaX is significantly reduced.
本発明は、最大エネルギー積ＢＨＩＩａｘの低下を伴う
ことなく高温不可逆減磁率の小さなＲ−Ｆｅ−Ｂ系の永
久磁石を提供することを目的とする。An object of the present invention is to provide an R-Fe-B permanent magnet that exhibits a small high-temperature irreversible demagnetization rate without reducing the maximum energy product BHIIax.
（問題点を解決するための手段）
本発明者等は、前記目的を達成する永久磁石について鋭
意検討した結果、Ｒ−ｒｅ−Ｂ系の永久磁石の表面部の
減磁が磁石内部よりも低い温度で生じ、該表面部の減磁
が永久磁石の高温不可逆減磁率を大きくしていることを
知見し、更にＲ−Ｆｅ −Ｂ系の永久磁石の表面付近に
磁石内部よりも固有保磁力ＩＨｃの高い層を設けること
により、最大エネルギー積ＢＨｍａｘの低下を伴うこと
なく高温不可逆減磁率が小さくなることを知見した。(Means for Solving the Problems) As a result of intensive study on permanent magnets that achieve the above object, the present inventors found that the demagnetization of the surface portion of an R-re-B permanent magnet is lower than that inside the magnet. They found that the demagnetization of the surface area increases the high-temperature irreversible demagnetization rate of the permanent magnet, and that the intrinsic coercive force IHc is greater near the surface of the R-Fe-B permanent magnet than inside the magnet. It has been found that by providing a layer with a high temperature, the high-temperature irreversible demagnetization rate can be reduced without reducing the maximum energy product BHmax.
本発明は、前記知見に基づいてなされたものであって、
Ｒ−ｒｅ −Ｂ系（ＲはＬａｓ Ｃｅ５ＰｒＳＮｄｑＰ
ＩＩ％ＳＩ、Ｅｕ、 Ｇｄ％Ｔｂ、 Ｄｙ５８０％ Ｅ
ｒｓ Ｔｍ、Ｙｌ）ｓ Ｌｕ。The present invention has been made based on the above findings, and includes:
R-re-B system (R is Las Ce5PrSNdqP
II%SI, Eu, Gd%Tb, Dy580%E
rs Tm, Yl)s Lu.
Ｙのうち少なくともＩＦＩｉ類）磁石の表面付近にＴｂ
、 ［）ｙ、 ＡＩ、 Ｇａのうち少なくとも１種類を
拡散させて磁石内部よりも固有保磁力の高い層を設けた
ことを特徴とする。Among Y, at least IFIi class) Tb near the surface of the magnet
, [)y, AI, and Ga are diffused to provide a layer having a higher intrinsic coercive force than the inside of the magnet.
本発明のＲ（希土類元素）−Ｆｅ（鉄）−Ｂ（ホウ素）
系磁石に用いるＲ（希土類元素）としてしてはＬａ （
ランタン）、Ｃ１３（セリウム）、Ｐｒ（プラセオジム
） 、Ｎｄ （ネオジム） 、Ｐａ＋ （プロメチウム
）、５Ｉｌ（サマリウム）、Ｅｕ（ユーロピウム） 、
Ｇｄ （ガドリニウム）、Ｔｂ（テルビウム）、Ｄｙ（
ジスプロシウム）、Ｈｏ（ホルミウム）、Ｅ「（エルビ
ウム） 、Ｔｍ （ツリウム） 、Ｙｂ （イッテルビ
ウム）、Ｌｕ（ルテチウム）、Ｙ（イツトリウム）があ
り、夫々単独に用いてもよいし、混合併用してもよい。R (rare earth element)-Fe (iron)-B (boron) of the present invention
The R (rare earth element) used in the system magnet is La (
Lanthanum), C13 (cerium), Pr (praseodymium), Nd (neodymium), Pa+ (promethium), 5Il (samarium), Eu (europium),
Gd (gadolinium), Tb (terbium), Dy(
Dysprosium), Ho (holmium), E (erbium), Tm (thulium), Yb (ytterbium), Lu (lutetium), and Y (yttrium), each of which may be used alone or in combination. good.
また磁石の表面付近に形成する固有保磁力ｉＨｃ材とし
てはＴｂ （テルビウム）、Ｄｙ（ジスプロシウム）、
ＡＩ （アルジニウム）、Ｇａ（ガリウム）があり、夫
々単独に用いてもよいし、混合併用してもよい。In addition, the intrinsic coercivity iHc materials formed near the surface of the magnet include Tb (terbium), Dy (dysprosium),
There are AI (aldinium) and Ga (gallium), which may be used alone or in combination.
磁石の表面付近に磁石内部よりも高い固有保磁力の層を
設けるために前記材料を拡散する方法としては例えばこ
れら材料を陰極ターゲツト材として用い真空度４〜６
Ｘ １Ｏ−６Ｔｏｒｒ中でスパッタリングを行った後、
熱処理を行う方法が挙げられる。この方法によって前記
材料は磁石の表面のみならず磁石表面より１００μも内
方の粒界および非磁性層部分まで拡散される。In order to provide a layer near the surface of the magnet with a higher intrinsic coercive force than the inside of the magnet, a method of diffusing the above-mentioned materials is, for example, using these materials as a cathode target material at a vacuum degree of 4 to 6.
After sputtering in X 1O-6 Torr,
One example is a method of performing heat treatment. By this method, the material is diffused not only to the surface of the magnet but also to the grain boundaries and non-magnetic layer portions 100 microns inward from the magnet surface.
（実施例）
次に本発明の実施例１．２．３．４および比較例につい
て説明する。(Example) Next, Examples 1, 2, 3, and 4 of the present invention and a comparative example will be described.
実施例１
まず、Ｎｄ（ネオジム）、Ｄｙ（ジスプロシウム）、Ｆ
ｅ （鉄）、Ｂ（ホウ素） 、ＡＩ （アルミニウム）
から成る組成比Ｎｄ＋ｚ、 ６Ｄｙｔ、 ｓ Ｐｅｔｓ
、 ２Ｂ？ＡＩ０．８の合金インゴットをＮ２雰囲気中
でスタンプミルにより粉砕し、更に同じＮ２雰囲気中で
ジェットミルにより微粉砕して平均粒径３．１μの粉末
を得た。Example 1 First, Nd (neodymium), Dy (dysprosium), F
e (iron), B (boron), AI (aluminum)
Composition ratio consisting of Nd+z, 6Dyt, s Pets
, 2B? An alloy ingot with an AI of 0.8 was pulverized by a stamp mill in an N2 atmosphere, and further finely pulverized by a jet mill in the same N2 atmosphere to obtain powder with an average particle size of 3.1μ.
続いて得られた粉末を１５ｋＯｅの磁場中で配向した状
態で磁界に垂直方向に１．５ｔｏｎ／ｃＪの圧力で成形
体を形成した。Subsequently, the obtained powder was oriented in a magnetic field of 15 kOe and a molded body was formed under a pressure of 1.5 ton/cJ in a direction perpendicular to the magnetic field.
更に形成された成形体をＡｒガス雰囲気中で温度１．１
００℃で１時間焼成して、長さ１（至）幅１．１（至）
厚さ０．２ ｃｍの焼結体を得た。Furthermore, the formed compact was heated at a temperature of 1.1 in an Ar gas atmosphere.
Baked at 00℃ for 1 hour, length 1 (to) width 1.1 (to)
A sintered body with a thickness of 0.2 cm was obtained.
次に得られた焼結体を陽極とし、Ｄｙ （ジスブムシウ
ム）金属を陰極ターゲツト材として、真空度５ Ｘ １
Ｏ−６Ｔｏｒｒ中で３０分間スパッタリングを行い焼結
体の表面全面に亘って厚さ０．５μのａｙの薄膜層を形
成した。Next, the resulting sintered body was used as an anode, Dy (disbumium) metal was used as a cathode target material, and the vacuum degree was 5 x 1.
Sputtering was performed in O-6 Torr for 30 minutes to form a thin film layer of 0.5 μm in thickness over the entire surface of the sintered body.
続いて薄膜層を有する焼結体をＡｒガス雰囲気中で温度
９７０℃で１時間の熱処理を行った後、更に温度６５０
℃で１時間の熱処理を施した。Subsequently, the sintered body having the thin film layer was heat treated at a temperature of 970°C for 1 hour in an Ar gas atmosphere, and then further heated at a temperature of 650°C.
Heat treatment was performed at ℃ for 1 hour.
上記工程で作成した永久磁石の残留磁石密度Ｂｒ（ｋＧ
）、固有保磁力ＩＨｃ（ｋＯｅ）、最大エネルギー１４
ＢＨｓａｘ （ＭＧＯｅ） 、不可逆減磁率（％）を
調べたところ、表に示す結果が得られた。尚表における
Ｂｒｓ ｉＨｃ ｓ ＢＨＩｌａｘの測定時の温度は２
５℃である。また不可逆減磁率の測定時の温度は１６０
℃とした。Residual magnet density Br (kG
), intrinsic coercive force IHc (kOe), maximum energy 14
When BHsax (MGOe) and irreversible demagnetization rate (%) were investigated, the results shown in the table were obtained. In addition, the temperature at the time of measurement of Brs iHc s BHIlax in the table is 2
The temperature is 5°C. The temperature at which the irreversible demagnetization rate was measured was 160°C.
℃.
実施例２
陰極ターゲツト材としてＴｂ （テルビウム）金属を用
い、焼結体の表面全体に亘って厚さ０．５μのＴｂの薄
膜層を形成した以外は実施例１と同一の方法で永久磁石
を作成した。またその特性を実施例１と同一方法で測定
したところ、表に示す結果が得られた。Example 2 A permanent magnet was produced in the same manner as in Example 1, except that Tb (terbium) metal was used as the cathode target material and a thin film layer of Tb with a thickness of 0.5 μm was formed over the entire surface of the sintered body. Created. Further, when its properties were measured using the same method as in Example 1, the results shown in the table were obtained.
実施例３
まず、Ｎｄ （ネオジム）、Ｄｙ（ジスプロシウム）、
Ｆｅ（鉄）、Ｂ（ホウ素） 、ＡＩ （アルミニウム）
から成る組成比Ｎｄ＋２．６Ｄｙ１．４ Ｐｅ７ｓ、
ＪｖＡＩｏ、 ｓの合金インゴットをＮ２雰囲気中でス
タンプミルにより粗粉砕し、更に同じＮ２雰囲気中でジ
ェットミルにより微粉砕して平均粒径３．１μの粉末を
得た。Example 3 First, Nd (neodymium), Dy (dysprosium),
Fe (iron), B (boron), AI (aluminum)
Composition ratio consisting of Nd+2.6Dy1.4 Pe7s,
An alloy ingot of JvAIo, s was coarsely pulverized with a stamp mill in an N2 atmosphere, and further finely pulverized with a jet mill in the same N2 atmosphere to obtain powder with an average particle size of 3.1μ.
続いて得られた粉末を１５ｋＯｅの磁場中で配向した状
態で磁界に垂直方向に１．５ｔｏｎ／ｃ−の圧力で成形
体を形成した。Subsequently, the obtained powder was oriented in a magnetic field of 15 kOe and a molded body was formed under a pressure of 1.5 ton/c- in a direction perpendicular to the magnetic field.
更に形成された成形体をＡｒガス雰囲気中で温度１．１
２０℃で１時間焼成して、長さ１ｃＩＩＩ幅１．１印厚
さ０．２ ｃｍの焼結体を得た。Furthermore, the formed compact was heated at a temperature of 1.1 in an Ar gas atmosphere.
Firing was performed at 20° C. for 1 hour to obtain a sintered body having a length of 1 cm, a width of 1.1 cm, and a thickness of 0.2 cm.
次に得られた焼結体を陽極とし、ＡＩ （アルミニウム
）金属を陰極ターゲツト材として、真空度５ Ｘ １０
−’Ｔｏｒｒ中で３０分間スパッタリングを行い焼結体
の表面全面に亘って厚さ０．５μのＡＩの薄膜層を形成
した。Next, the obtained sintered body was used as an anode, AI (aluminum) metal was used as a cathode target material, and the vacuum degree was 5 x 10.
-'Torr for 30 minutes to form a thin layer of AI with a thickness of 0.5 μm over the entire surface of the sintered body.
続いて薄膜層を有する焼結体をＡ「ガス雰囲気中で温度
９７０℃で１時間の熱処理を行った後、更に温度４００
℃で１時間の熱処理を施した。Subsequently, the sintered body having the thin film layer was heat-treated at a temperature of 970°C for 1 hour in a gas atmosphere, and then further heated at a temperature of 400°C.
Heat treatment was performed at ℃ for 1 hour.
上記工程で作成した永久磁石の特性を実施例１と同一方
法で測定したところ、表に示す結果が得られた。When the characteristics of the permanent magnet produced in the above steps were measured using the same method as in Example 1, the results shown in the table were obtained.
実施例４
前記実施例１の工程と同一方法で作成した磁石の表面全
面に亘ってｌＯμずつ研摩して永久磁石を作成した。ま
たその特性を実施例１と同一方法で測定したところ、表
に示す結果が得られた。Example 4 A permanent magnet was prepared by polishing the entire surface of a magnet by 10 μ by the same method as in Example 1. Further, when its properties were measured using the same method as in Example 1, the results shown in the table were obtained.
比較例
まず、Ｎｄ （ネオジム）、Ｄｙ（ジスプロシウム）、
Ｆｅ（鉄）、Ｂ（ホウ素） 、ＡＩ （アルミニウム）
から成る組成比Ｎｄ＋ｚ、 ６Ｄ）’１．４ Ｐｅ７ｓ
、 ２Ｂ？ＡＩ０．８の合金インゴットをＮ２雰囲気中
でスタンプミルにより粗粉砕し、更に同じＮ２雰囲気中
でジェットミルにより微粉砕して平均粒径３．１μの粉
末を得た。Comparative example First, Nd (neodymium), Dy (dysprosium),
Fe (iron), B (boron), AI (aluminum)
Composition ratio Nd+z, 6D)'1.4 Pe7s
, 2B? An alloy ingot with an AI of 0.8 was coarsely pulverized with a stamp mill in an N2 atmosphere, and further finely pulverized with a jet mill in the same N2 atmosphere to obtain powder with an average particle size of 3.1μ.
続いて得られた粉末を１５ｋＯｅの磁場中で配向した状
態で磁界に垂直方向に１．５ｔｏｎ／ｃ−の圧力で成形
体を形成した。Subsequently, the obtained powder was oriented in a magnetic field of 15 kOe and a molded body was formed under a pressure of 1.5 ton/c- in a direction perpendicular to the magnetic field.
更に形成された成形体をＡｒガス雰囲気中で温度１．１
００℃で１時間焼成して、長さ１（至）幅１．１（至）
厚さ０．２（至）の焼結体を得た。Furthermore, the formed compact was heated at a temperature of 1.1 in an Ar gas atmosphere.
Baked at 00℃ for 1 hour, length 1 (to) width 1.1 (to)
A sintered body with a thickness of 0.2 (up to) was obtained.
次に得られた焼結体をＡｒガス雰囲気中で温度９００℃
で１時間の熱処理を行った後、更に温度６００℃で１時
間の熱処理を施した。Next, the obtained sintered body was heated to 900°C in an Ar gas atmosphere.
After heat treatment was performed for 1 hour at a temperature of 600° C., heat treatment was further performed for 1 hour at a temperature of 600°C.
上記工程で作成した永久磁石の特性を実施例１と同一方
法で測定したところ、表に示す結果が得られた。When the characteristics of the permanent magnet produced in the above steps were measured using the same method as in Example 1, the results shown in the table were obtained.
表
更に、上記実施例１で得られた永久磁石を切断して厚み
方向の断面を露出させ、磁石内部と、磁石表面より５０
μ内側について、それぞれの粒界および非磁性層部分に
偏析する。ｙの量を分析して比較した結果、磁石内部よ
りも磁石表面から５０μ内側のほうに多量にｏｙが偏析
していた。Furthermore, the permanent magnet obtained in Example 1 was cut to expose the cross section in the thickness direction, and the inside of the magnet and the surface of the magnet were 50 mm thick.
On the inside of μ, it segregates at each grain boundary and nonmagnetic layer portion. As a result of analyzing and comparing the amount of y, it was found that a larger amount of oy was segregated 50μ inside from the magnet surface than inside the magnet.
同様にして、上記実施例２．３および比較例で・得られ
た各永久磁石についてもそれぞれの粒界およ−び非磁性
層部分に偏析するＴｂ、 ＡＩ、 ＤＹの量を分析して
比較した結果、実施例２．３で得られた各永久磁石につ
いては磁石表面から５０μ内側のほうに多量にＴｂ、
ＡＩが偏析していたが、比較例で得られた永久磁石につ
いては、磁石内部と磁石表面から５０μ内側とで偏析す
るＤｙの量に差がみられなかった。Similarly, the amounts of Tb, AI, and DY segregated in the grain boundaries and nonmagnetic layer portions of each of the permanent magnets obtained in Example 2.3 and Comparative Example were analyzed and compared. As a result, for each of the permanent magnets obtained in Example 2.3, a large amount of Tb,
Although AI was segregated, in the permanent magnet obtained in the comparative example, there was no difference in the amount of Dy segregated between the inside of the magnet and 50μ inside from the magnet surface.
表から明らかなように実施例１．２．３．４の高温不可
逆減磁率は比較例の高温不可逆減磁率に比して極めて小
さくなった。従って実施例１．２．３．４の永久磁石は
その表面付近にＤｙ１ＴｂＳＡｌのいずれか１種類が拡
散して固有保磁力の高い層が設けられていることが確認
出来、また実施例１．２．３．４の永久磁石は最大エネ
ルギー積ＢＨＩＩｌａＸの低下がなく、かつ高温不可逆
減磁率を減少させたことが確認された。As is clear from the table, the high temperature irreversible demagnetization rate of Example 1.2.3.4 was extremely small compared to the high temperature irreversible demagnetization rate of Comparative Example. Therefore, it can be confirmed that the permanent magnet of Example 1.2.3.4 has a layer with high intrinsic coercive force due to diffusion of one of Dy1TbSAl near its surface, and also Example 1.2 It was confirmed that the permanent magnet of No. 3.4 did not reduce the maximum energy product BHIIlaX and reduced the high temperature irreversible demagnetization rate.
（発明の効果）
本発明によれば、Ｒ−ｒｅ −Ｂ系（ＲはＬａｓ Ｃｅ
５Ｐｒｑ Ｎｄｓ Ｐａ、Ｓ１％ ＥＬＩＳＧｄｓ Ｔ
ｂｓ ０１％ ＨＯ％ Ｅｒｓ Ｔａ＋、Ｙｂ５Ｌｕ、
Ｙのうち少なくとも１種類）磁石の表面付近にＴｂ、
Ｄｙ、 ＡＩ、Ｇｄのうち少なくとも１種類を拡散さ
せて磁石内部よりも固有保磁力が高い層を設けるように
したので、最大エネルギー積の低下を伴うことなく高温
不可逆減磁率の小さなＲ−Ｆｅ −Ｂ系の永久磁石を提
供することが出来る。(Effect of the invention) According to the present invention, R-re-B system (R is Las Ce
5Prq Nds Pa, S1% ELISGds T
bs 01% HO% Ers Ta+, Yb5Lu,
At least one type of Y) Tb near the surface of the magnet,
By diffusing at least one of Dy, AI, and Gd to provide a layer with higher intrinsic coercive force than the inside of the magnet, R-Fe − has a small high-temperature irreversible demagnetization rate without reducing the maximum energy product. B-based permanent magnets can be provided.
Claims (1)
、Ｓｍ、Ｅｕ、Ｇｄ、Ｔｂ、Ｄｙ、Ｈｏ、Ｅｒ、Ｔｍ、
Ｙｂ、Ｌｕ、Ｙのうち少なくとも１種類）磁石の表面付
近にＴｂ、Ｄｙ、Ａｌ、Ｇａのうち少なくとも１種類を
拡散させて磁石内部よりも固有保磁力の高い層を設けた
ことを特徴とする永久磁石。R-Fe-B system (R is La, Ce, Pr, Nd, Pm
, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm,
At least one of Yb, Lu, and Y) is characterized by providing a layer having a higher intrinsic coercive force than the inside of the magnet by diffusing at least one of Tb, Dy, Al, and Ga near the surface of the magnet. permanent magnet.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62274799A JPH01117303A (en) | 1987-10-30 | 1987-10-30 | Permanent magnet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62274799A JPH01117303A (en) | 1987-10-30 | 1987-10-30 | Permanent magnet |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01117303A true JPH01117303A (en) | 1989-05-10 |
Family
ID=17546728
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62274799A Pending JPH01117303A (en) | 1987-10-30 | 1987-10-30 | Permanent magnet |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01117303A (en) |
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