JPH01155602A - Permanent magnet and manufacture thereof - Google Patents
Permanent magnet and manufacture thereofInfo
- Publication number
- JPH01155602A JPH01155602A JP62314235A JP31423587A JPH01155602A JP H01155602 A JPH01155602 A JP H01155602A JP 62314235 A JP62314235 A JP 62314235A JP 31423587 A JP31423587 A JP 31423587A JP H01155602 A JPH01155602 A JP H01155602A
- Authority
- JP
- Japan
- Prior art keywords
- permanent magnet
- composition
- smtife
- phase
- compound phase
- 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
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 239000000203 mixture Substances 0.000 claims abstract description 16
- 150000001875 compounds Chemical class 0.000 claims abstract description 13
- 229910045601 alloy Inorganic materials 0.000 claims description 9
- 239000000956 alloy Substances 0.000 claims description 9
- 238000000137 annealing Methods 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 13
- 230000005291 magnetic effect Effects 0.000 abstract description 9
- 230000004907 flux Effects 0.000 abstract description 4
- 229920006395 saturated elastomer Polymers 0.000 abstract 1
- 238000007712 rapid solidification Methods 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 230000009466 transformation Effects 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910000640 Fe alloy Inorganic materials 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910000938 samarium–cobalt magnet Inorganic materials 0.000 description 2
- 102100037114 Elongin-C Human genes 0.000 description 1
- 101001011859 Homo sapiens Elongin-A Proteins 0.000 description 1
- 101001011846 Homo sapiens Elongin-B Proteins 0.000 description 1
- 101000881731 Homo sapiens Elongin-C Proteins 0.000 description 1
- 101000836005 Homo sapiens S-phase kinase-associated protein 1 Proteins 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910010340 TiFe Inorganic materials 0.000 description 1
- 230000005290 antiferromagnetic effect Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000010409 thin film Substances 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
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
この発明は、Ｆｅ −Ｓｍ系の永久磁石とその製造方法
に関するものである。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a Fe--Sm permanent magnet and a method for manufacturing the same.
（従来の技術）
ＳＩＩＩ系永久磁石は、ＳｍＣｏ５とＳｍ、Ｃｏ１１系
が代表的な磁石として知られており、小型、効率化が要
求さる電子機器の磁気回路に多用されている。(Prior Art) SmCo5, Sm, and Co11-based permanent magnets are known as typical SIII-based permanent magnets, and are widely used in magnetic circuits of electronic devices that require small size and high efficiency.
（発明が解決しようとする問題点）
しかしながらこの種の永久磁石は、高価なＧｏを多量に
含むことの他、圧粉・焼結による工程の煩雑さ故にコス
トが高く、そのため価格的に安価な磁石の開発が望まれ
、Ｓｍ −Ｆｅ系磁石の開発などが試みられているが、
現在までのところ充分な成果を挙げるまでには至ってい
ない。(Problem to be solved by the invention) However, this type of permanent magnet is expensive because it contains a large amount of expensive Go and the process of powder compaction and sintering is complicated. The development of magnets is desired, and attempts have been made to develop Sm-Fe magnets.
To date, sufficient results have not been achieved.
この発明は、上記の現状に鑑みて開発されたもので、そ
の目的とするところは、高価なＣｏを含まず、なおかつ
良好な磁気特性とくに優れた保磁力を有する永久磁石を
その有利な製造方法と共に提供することにある。This invention was developed in view of the above-mentioned current situation, and its purpose is to provide a permanent magnet that does not contain expensive Co and has good magnetic properties, especially excellent coercive force, using an advantageous manufacturing method. The aim is to provide the same.
（問題点を解決するための手段）
Ｓｍ −Ｆｅ系合金においては、従来、通常の焼結製造
法では高保磁力を有する金属間化合物は得られなかった
が、発明者らは、溶融後急速凝固するいわゆる超や、冷
性によれば、通常の方法では得られないＳｍＦｅ３やＳ
ｍｚＦｅｔ等の高保磁力を有する準安定な化合物相を生
成できることを見出した。(Means for solving the problem) Conventionally, it has not been possible to obtain an intermetallic compound with a high coercive force using a normal sintering production method for Sm-Fe alloys, but the inventors have developed a method for rapidly solidifying Sm-Fe alloys after melting. According to the so-called super or cold property, SmFe3 and S, which cannot be obtained by normal methods, are
It has been found that a metastable compound phase having a high coercive force such as mzFet can be generated.
しかしながら、ＳｍＦｅ５はキューリー温度が低いとい
う欠点があり、一方Ｓｍ、Ｆｅ、は飽和磁束密度が低い
だけでなく、Ｓ重量が多いために高価になるという欠点
があった。However, SmFe5 has the disadvantage of a low Curie temperature, while Sm and Fe not only have a low saturation magnetic flux density but also have a disadvantage of being expensive due to their large S weight.
この発明は、上記の欠点を改善するために、ＳｍＦｅ５
組成附近の合金系についてＳｍを他元素で置換すること
を試みた結果、Ｓｍ ４０〜７０％をＴｉで置換した場
合に高保磁力と飽和磁束密度の大きいＳｍＴｉＦｅ、相
が得られるという新規な知見に基づき完成されたもので
ある。In order to improve the above-mentioned drawbacks, this invention
As a result of trying to replace Sm with other elements in alloy systems with similar compositions, we found a new finding that when 40 to 70% of Sm was replaced with Ti, a SmTiFe phase with high coercive force and high saturation magnetic flux density could be obtained. It has been completed based on the following.
すなわち、この発明の要旨構成は次の通りである。That is, the gist of the present invention is as follows.
（１）原子％でＳｍ ： ４〜１０％、Ｔｉ：６〜１１
％、Ｆｅ ： ８１〜８６％の組成になり、内部にＳｍ
ＴｉＦｅｚ化合物Ｆｅ上なえることを特徴とする永久磁
石。(1) Sm: 4-10%, Ti: 6-11 in atomic %
%, Fe: The composition is 81-86%, with Sm inside.
A permanent magnet characterized by a TiFez compound coated with Fe.
（２）原子％でＳｍ ： ４〜１０％、Ｔｉ ： ６〜
１１％、Ｆｅ ： ８１〜８６％の組成になる合成溶湯
を、その合金組成に応じた冷却速度で冷却凝固させて、
内部にＳｍＴｔＦｅ＋＋化合物相を析出させることから
なる永久磁石の製造方法。(2) Sm: 4 to 10%, Ti: 6 to 10% in atomic %
11%, Fe: A synthetic molten metal having a composition of 81 to 86% is cooled and solidified at a cooling rate according to the alloy composition,
A method for producing a permanent magnet, which comprises precipitating an SmTtFe++ compound phase inside.
（３）原子％で５ＩＩＩ：４〜１０％、Ｔｉ ： ６〜
１１％、Ｆｅ ： ８１〜８６％の組成になる合成溶湯
を、急冷凝固させて非晶質またはＴｂＣｕ型の非平衡相
としたのち、７００〜９００℃の温度範囲で焼鈍を施し
てＳｍＴｉＦｅ＋ １化合物に相変態させることからな
る永久磁石の製造方法。(3) 5III: 4-10% in atomic %, Ti: 6-10%
A synthetic molten metal having a composition of 11% and 81% to 86% Fe is rapidly solidified to form an amorphous or TbCu type non-equilibrium phase, and then annealed in a temperature range of 700 to 900°C to form an SmTiFe+ 1 compound. A method for producing a permanent magnet, which comprises phase transformation.
（作 用）
ＳｍＦｅ、附近の組成について、ＳｍをＴｉで置換して
行（と飽和磁束密度はあまり低下せずにキューリー温度
が３００℃まで上昇する。そして原子％でＳｍ： ４〜
１０％、Ｔｉ：６〜１１％の範囲ではＳｍＴｉＦｅ＋
＋化合物相が生成し高保持力が得られるようになる。(Function) When Sm is replaced with Ti for SmFe, the Curie temperature rises to 300°C without much decrease in the saturation magnetic flux density.
10%, Ti: SmTiFe+ in the range of 6 to 11%
+ Compound phase is generated and high retention power can be obtained.
この化合物相の結晶磁気異方性定数は、発明者が測定し
た結果では５ Ｘ１０’ｅｒｇ／ｃｍ３と非常に大きい
値を呈しており、これが高保磁力に寄与しているものと
考えられる。The magnetocrystalline anisotropy constant of this compound phase has a very large value of 5 x 10'erg/cm3 as measured by the inventor, and it is thought that this contributes to the high coercive force.
以下この発明の成分組成範囲の限定理由について説明す
る。The reasons for limiting the component composition range of this invention will be explained below.
Ｓｍの含を量が４％に満たないと反強磁性相のＴｉＦｅ
ｚが生成し、一方１０％を超えるとＳｍＴｉＦｅ＋ ＋
相が得られなくなり保持磁力は（氏上する。When the amount of Sm is less than 4%, TiFe in the antiferromagnetic phase
z is generated, while when it exceeds 10%, SmTiFe+ +
The phase is no longer obtained and the holding magnetic force increases.
またＴｉ含有量が６％未満ではＳｍＴｉＦｅ、 、が生
成せず、一方１１％を超えるとＴｉＦｅｚを生成し保持
力が低下するとともに飽和磁気も低下する。Further, if the Ti content is less than 6%, SmTiFe, , etc. will not be generated, while if it exceeds 11%, TiFez will be generated, and the coercive force and saturation magnetism will also decrease.
残余のＦｅについては、８１％に満たないと飽和磁気が
低くなり、一方８６％を超えるとＴｈｚＮｉ＋を型の化
合物相が得られなくなる。Regarding the remaining Fe, if it is less than 81%, the saturation magnetism will be low, while if it exceeds 86%, a ThzNi+ type compound phase will not be obtained.
なおこの発明では、特性を維持しながら、キューリー点
の上昇と耐食性を改善するためにＣｏをＦｅに対して２
０％まで置換することができる。In addition, in this invention, in order to raise the Curie point and improve corrosion resistance while maintaining the characteristics, Co is added to Fe by 2.
It can be replaced up to 0%.
さてこの発明に従う永久磁石を製造するに当っては、通
常の溶解−鋳造一粉砕一焼結工程を利用することができ
るが、好適成分組成に溶製した合金溶湯を、急速凝固し
て合金薄帯とするいわゆる急速凝固法が有利に適合する
。Now, in manufacturing the permanent magnet according to the present invention, the usual melting-casting-grinding-sintering process can be used, but a molten alloy melted to a suitable composition is rapidly solidified to form an alloy thin film. The so-called rapid solidification method using strips is advantageously suitable.
急速凝固法としては、ガス噴射法など従来公知の方法い
ずれもが実施可能であったが、単ロール法や回転ドラム
法など、溶融金属を高速で回転するロールやドラム外表
面上に供給する方法を適用した場合にとりわけ良好な結
果が得られた。As a rapid solidification method, any conventionally known method such as a gas injection method can be implemented, but methods such as a single roll method and a rotating drum method in which molten metal is supplied onto the outer surface of a roll or drum that rotates at high speed. Particularly good results were obtained when applying
実験では、直径１６０ ｍｍの銅製ロールを用いその回
転数により冷却速度を調整したが、ロール周速が２０ｍ
／ｓ附近の場合ＳｍＴｉＦｅ＋ ｒ相が生成し高保磁力
が得られた。この点３０ｍ／ｓ以上になると非平衡相の
ＴｂＣｕ、型及び非晶質相となりや、冷ままの状態では
高保磁力は得られなくなる。しかしながら３０ｍ／ｓ以
上で急速凝固した後、焼鈍を施すことにより６００℃附
近から保磁力の増加がはじまり、８００℃で安定相のＳ
ｍＴｉＦｅｚに相変態すると最高の保磁力が得られるよ
うになった。In the experiment, a copper roll with a diameter of 160 mm was used and the cooling rate was adjusted depending on the rotation speed.
/s, SmTiFe+ r phase was generated and a high coercive force was obtained. When the speed exceeds 30 m/s, non-equilibrium TbCu, type and amorphous phases occur, and a high coercive force cannot be obtained in a cold state. However, after rapid solidification at 30 m/s or more, the coercive force begins to increase around 600°C by annealing, and at 800°C the stable phase of S
The highest coercive force can be obtained by phase transformation to mTiFez.
従ってこの発明では、焼鈍温度につき、良好な相変態が
達成できる７００〜９００″Ｃの範囲に限定したのであ
る。Therefore, in the present invention, the annealing temperature is limited to a range of 700 to 900''C at which good phase transformation can be achieved.
以上のように凝固速度をコントロールすることにより直
接ＳｍＴｉＦｅ、相を生成することもできるが、周速３
０ｍ／ｓ以上の急速凝固により非平衡相としたのち、７
００〜９００℃の焼鈍によってＳｍＴｉＦｅｚ相を生成
させる方がより制御が容易である。Although it is possible to directly generate the SmTiFe phase by controlling the solidification rate as described above,
After forming a non-equilibrium phase by rapid solidification at 0 m/s or more, 7
It is easier to control the SmTiFez phase by annealing at 00 to 900°C.
（実施例）
実施例１
表１に示す組成になる合金溶湯をアルゴン雰囲気中で高
周波溶解したのち、０．５ ｋｇ／ｃｍ”のアルゴンを
溶湯に加圧して内径：０．５ｍｍの石英ノズルから、５
〜４２ｍ／ｓの種々の周速で回転する直径：１６０胴の
銅製の回転ロール上に噴射し、急速に冷却凝固させて薄
帯を得た。(Example) Example 1 After high-frequency melting of a molten alloy having the composition shown in Table 1 in an argon atmosphere, 0.5 kg/cm'' of argon was applied to the molten metal and the melt was melted through a quartz nozzle with an inner diameter of 0.5 mm. , 5
The mixture was sprayed onto a copper rotating roll with a diameter of 160 mm rotating at various circumferential speeds of ~42 m/s, and rapidly cooled and solidified to obtain a ribbon.
かくして得られた各薄帯につき、振動形磁力計により、
最大印加磁場１８ｋＯｅの範囲で磁気特性を測定した。For each ribbon obtained in this way, a vibrating magnetometer was used to measure the
The magnetic properties were measured in the range of a maximum applied magnetic field of 18 kOe.
得られた結果を表１に併記する。なお表１に示した特性
値は、各合金組成の溶湯をロール周速を変えて作製した
薄帯について得られた最高の値である。The obtained results are also listed in Table 1. The characteristic values shown in Table 1 are the highest values obtained for ribbons made from molten metal of each alloy composition at different roll speeds.
同表より表らかなように、この発明に従い得られた合金
薄帯（Ｎα３〜６）はいずれも、高い保磁力が得られ、
またＸ線デイフラクト法により回折した結果、ＳｍＴｉ
Ｆｅ＋＋相が同定された。As is obvious from the same table, all the alloy ribbons (Nα3 to 6) obtained according to the present invention have high coercive force,
Furthermore, as a result of diffraction using the X-ray diffract method, SmTi
A Fe++ phase was identified.
大旌拠主
表１の発明合金Ｎα３を実施例１と同様の方法にて、周
速３０ｍ／ｓで薄帯を作製した。ついで得られた薄帯を
５００〜９００℃の温度で５時間焼鈍したのちの保持力
について調べた結果を表２に示す。A ribbon was produced from the invention alloy Nα3 shown in Table 1 in the same manner as in Example 1 at a circumferential speed of 30 m/s. Table 2 shows the results of examining the holding power after annealing the obtained ribbon at a temperature of 500 to 900° C. for 5 hours.
表２
加熱温度（至）５００ ６００ ７００ ８００
９００ｉＨｃ（ｋｏｅ） ０．２５１．０２．９
５．０ ２．２薄帯作製ままの状態ではＴｂＣｕ７型の
非平衡相であったが、７００〜９００℃の焼鈍を施した
のちは、平衡相であるＳｍＴｉＦｅ、 ｒ相が同定され
た。とくに８００℃の焼鈍においてとりわけ高いｉＨｃ
が得られた。Table 2 Heating temperature (to) 500 600 700 800
900iHc(koe) 0.251.02.9
5.0 2.2 In the as-prepared state of the ribbon, it was a non-equilibrium phase of TbCu7 type, but after annealing at 700 to 900°C, an equilibrium phase, SmTiFe, r phase was identified. Particularly high iHc during annealing at 800°C
was gotten.
以上実施例では、薄帯形状で測定した特性値を示したが
、結晶磁気異方性は非常に大きく、また薄帯の粉砕は極
めて容易であるので、最適粒度に粉砕し結晶粒の配向度
をそろえて焼結することによって強力な磁石を製造する
こともできる。In the examples above, the characteristic values measured in the shape of a ribbon were shown, but since the magnetocrystalline anisotropy is very large and the ribbon is extremely easy to crush, it is necessary to crush the ribbon to the optimum particle size and improve the orientation of the crystal grains. Strong magnets can also be manufactured by sintering them.
（発明の効果）
この発明磁石は、高価なＳｍの含有量が少なく、またＣ
ｏを全く含有していないので、原料的にＳｍＣ。(Effect of the invention) The magnet of this invention has a low content of expensive Sm and
Since it does not contain any o, it is SmC as a raw material.
系磁石に比し、非常に安価であり、また製造法も簡便で
あるので、優れた特性を有する永久磁石を安価に製造す
ることができ、ＳｍＣｏ系磁石の使用されている用途に
適用して極めて有利である。Compared to SmCo-based magnets, it is very inexpensive and the manufacturing method is simple, so permanent magnets with excellent properties can be manufactured at low cost and can be applied to applications where SmCo-based magnets are used. Extremely advantageous.
特許出願人 東北特殊鋼株式会社Patent applicant: Tohoku Special Steel Co., Ltd.
Claims (3)
そなえることを特徴とする永久磁石。1. A permanent magnet having a composition of Sm: 4 to 10%, Ti: 6 to 11%, and Fe: 81 to 86% in atomic %, and having an SmTiFe_1_1 compound phase inside.
度で冷却凝固させて、内部にＳｍＴｉＦｅ＿１＿１化合
物相を析出させることを特徴とする永久磁石の製造方法
。2. A synthetic molten metal having a composition of Sm: 4 to 10%, Ti: 6 to 11%, and Fe: 81 to 86% in atomic % is cooled and solidified at a cooling rate according to the alloy composition to form an SmTiFe_1_1 compound phase inside. A method for producing a permanent magnet, characterized by precipitating.
ＴｂＣｕ＿７型の非平衡相としたのち、７００〜９００
℃の温度範囲で焼鈍を施してＳｍＴｉＦｅ＿１＿１化合
物相に相変態させることを特徴とする永久磁石の製造方
法。3. A synthetic molten metal having a composition of Sm: 4 to 10%, Ti: 6 to 11%, and Fe: 81 to 86% in atomic percent is rapidly solidified to form an amorphous or TbCu_7 type non-equilibrium phase, and then ~900
A method for producing a permanent magnet, which comprises annealing in a temperature range of 0.degree. C. to transform the magnet into a SmTiFe_1_1 compound phase.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62314235A JPH01155602A (en) | 1987-12-14 | 1987-12-14 | Permanent magnet and manufacture thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62314235A JPH01155602A (en) | 1987-12-14 | 1987-12-14 | Permanent magnet and manufacture thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01155602A true JPH01155602A (en) | 1989-06-19 |
Family
ID=18050911
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62314235A Pending JPH01155602A (en) | 1987-12-14 | 1987-12-14 | Permanent magnet and manufacture thereof |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01155602A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2020132926A (en) * | 2019-02-15 | 2020-08-31 | 学校法人千葉工業大学 | Samarium-iron-based rare earth permanent magnet material and its production method |
-
1987
- 1987-12-14 JP JP62314235A patent/JPH01155602A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2020132926A (en) * | 2019-02-15 | 2020-08-31 | 学校法人千葉工業大学 | Samarium-iron-based rare earth permanent magnet material and its production method |
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