JP4412487B2 - Method for producing magnetostrictive material - Google Patents
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- JP4412487B2 JP4412487B2 JP2005015340A JP2005015340A JP4412487B2 JP 4412487 B2 JP4412487 B2 JP 4412487B2 JP 2005015340 A JP2005015340 A JP 2005015340A JP 2005015340 A JP2005015340 A JP 2005015340A JP 4412487 B2 JP4412487 B2 JP 4412487B2
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- 238000004519 manufacturing process Methods 0.000 title claims description 22
- 239000002994 raw material Substances 0.000 claims description 133
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 44
- 239000001301 oxygen Substances 0.000 claims description 44
- 229910052760 oxygen Inorganic materials 0.000 claims description 44
- 230000005291 magnetic effect Effects 0.000 claims description 22
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 18
- 239000001257 hydrogen Substances 0.000 claims description 18
- 229910052739 hydrogen Inorganic materials 0.000 claims description 18
- 229910052742 iron Inorganic materials 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
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- 239000002245 particle Substances 0.000 description 30
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 25
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- 239000000843 powder Substances 0.000 description 12
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- 230000005496 eutectics Effects 0.000 description 2
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- 238000009776 industrial production Methods 0.000 description 2
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Description
本発明は、外部磁界を作用させたときに長さが変化する磁歪材料を製造する方法に関し、特に焼結により磁歪材料を得る際の原料粉末の酸素量を規定することにより磁歪特性に優れた材料を製造する方法に関する。 The present invention relates to a method for producing a magnetostrictive material that changes its length when an external magnetic field is applied, and in particular, it has excellent magnetostrictive characteristics by defining the amount of oxygen in a raw material powder when obtaining a magnetostrictive material by sintering. It relates to a method of manufacturing a material.
強磁性体を磁化したときに、磁性体の寸法が変化する現象を磁歪といい、このような現象が生ずる材料を磁歪材料という。磁歪による飽和変化量である飽和磁歪定数は、一般には１０-5〜１０-6の値を有し、大きな飽和磁歪定数を有する磁歪材料は超磁歪材料とも呼ばれ、振動子、フィルター、センサ等に広く利用されている。現在、Ｒ（希土類元素）とＦｅの化合物であるＲＦｅ2ラーベス型金属間化合物を主体とする磁歪材料が飽和磁歪定数の大きな材料として知られている（例えば、特許文献１〜４）。しかしこれら材料において、印加される外部磁界が大きいときには磁歪値が大きいが、外部磁界が小さいときには磁歪値が十分ではないという問題を有していた。そこで、ＲＦｅ2ラーベス型金属間化合物を主体とする磁歪材料において、低外部磁界でも磁歪値を大きくする検討が行われ、磁化容易軸であって、磁歪定数の大きい［１１１］軸方向に配向させることが提案されている。また、ＲＦｅ2ラーベス型金属間化合物を主体とする材料としては、Ｔｂ0.3Ｄｙ0.7Ｆｅ2.0（原子比）の組成を有する場合に磁歪値が大きいため、専らこの組成が採用されていた。 A phenomenon in which the size of a magnetic material changes when a ferromagnetic material is magnetized is called magnetostriction, and a material in which such a phenomenon occurs is called a magnetostrictive material. The saturation magnetostriction constant, which is the amount of saturation change due to magnetostriction, generally has a value of 10 −5 to 10 −6 , and a magnetostrictive material having a large saturation magnetostriction constant is also called a super magnetostrictive material, such as a vibrator, filter, sensor, etc. Widely used. At present, magnetostrictive materials mainly composed of RFe 2 Laves type intermetallic compound which is a compound of R (rare earth element) and Fe are known as materials having a large saturation magnetostriction constant (for example, Patent Documents 1 to 4). However, these materials have a problem that the magnetostriction value is large when the applied external magnetic field is large, but the magnetostriction value is not sufficient when the external magnetic field is small. Therefore, in a magnetostrictive material mainly composed of RFe 2 Laves-type intermetallic compound, studies have been made to increase the magnetostriction value even in a low external magnetic field, and the orientation is made in the [111] axis direction having an easy axis of magnetization and a large magnetostriction constant. It has been proposed. In addition, as a material mainly composed of RFe 2 Laves type intermetallic compound, this composition was exclusively adopted because it has a large magnetostriction value when it has a composition of Tb 0.3 Dy 0.7 Fe 2.0 (atomic ratio).
磁場中での成形で高い配向を得るため、Ｔｂ、Ｄｙ、Ｔ（鉄族金属）からなる原料Ａ、Ｄｙ、Ｔｂ、Ｔからなる原料Ｂ、Ｔからなる原料Ｃの合金粉を作製し、これら３種類の合金粉を混合し焼結する磁歪材料の製造方法が特許文献５に提案されている。しかし、特許文献５に提案されている磁歪材料の製造方法では、必ずしも焼結密度が十分ではないという問題点があった。 In order to obtain high orientation by forming in a magnetic field, alloy powders of raw material A composed of Tb, Dy, T (iron group metal), raw material B composed of Dy, Tb, T, and raw material C composed of T were prepared. A method of manufacturing a magnetostrictive material in which three types of alloy powders are mixed and sintered is proposed in Patent Document 5. However, the method of manufacturing a magnetostrictive material proposed in Patent Document 5 has a problem that the sintered density is not always sufficient.
それを解決する方法として、式１：（ＴｂxＤｙ1-x）Ｔy（Ｔは、Ｆｅ、Ｎｉ、Ｃｏの群から選択される少なくとも１種類の金属元素であり、ｘ、ｙは０．３５＜ｘ≦０．５０、１．７０≦ｙ≦２．００の範囲）で表される原料Ａと、式２：ＤｙtＴ1-t（Ｄｙは、ＴｂとＨｏの双方又はいずれか一方を含むことがあり、ｔは０．３７≦ｔ≦１．００の範囲）で表され、７０００ｐｐｍ≦水素量≦２２０００ｐｐｍの範囲にある水素を含む原料Ｂと、Ｔを含有する原料Ｃとを混合し、焼結して、式３：（ＴｂvＤｙ1-v）Ｔw（ｖ、ｗは０．２７≦ｖ＜０．５０、１．７０≦ｗ≦２．００の範囲にある。）で表される磁歪材料を製造する方法が、特許文献６に提案されている。 As a method for solving this, Formula 1: (Tb x Dy 1-x ) T y (T is at least one metal element selected from the group of Fe, Ni, Co, and x, y is 0. 35 <x ≦ 0.50, 1.70 ≦ y ≦ 2.00) and the formula 2: Dy t T 1-t (Dy is either or both of Tb and Ho) T is a range of 0.37 ≦ t ≦ 1.00), and a raw material B containing hydrogen in a range of 7000 ppm ≦ hydrogen content ≦ 22000 ppm and a raw material C containing T are mixed. Sintering and formula 3: (Tb v Dy 1-v ) T w (v and w are in the range of 0.27 ≦ v <0.50, 1.70 ≦ w ≦ 2.00) A method of manufacturing a magnetostrictive material represented by the following is proposed in Patent Document 6.
特許文献６によれば、原料Ｂに水素を吸蔵させることにより、水素化物を形成するか又は水素原子が結晶内に侵入するかは別にして、歪みが生じるために内部応力に耐えられなくなり、原料Ｂの粒子には割れが生じる。そのために、原料Ｂを原料Ａと原料Ｃと混合し、成形体を形成する時に圧力を懸ける際に割れの先端に応力が集中して、さらに割れが進行するために、混合した状態の内部で粉砕されて細かくなり、原料Ａの間に入り込むことで、焼結したときに緻密で焼結体の密度は高くなることが開示されている。 According to Patent Document 6, by storing hydrogen in the raw material B, it becomes impossible to withstand internal stress because distortion occurs, regardless of whether a hydride is formed or a hydrogen atom enters the crystal, Cracks occur in the particles of the raw material B. Therefore, the raw material B is mixed with the raw material A and the raw material C, and stress is concentrated at the tip of the crack when the pressure is applied when forming a molded body, and the crack progresses further. It is disclosed that when the material is pulverized to become fine and enter between the raw materials A, the sintered body is dense and the density of the sintered body is increased.
しかし、特許文献６に提案されている磁歪材料の製造方法では、成形体を金型から取り出す際の圧力（以下、「抜き圧」という）が高く離型性に問題点がある。抜き圧を低減するために潤滑剤を添加することも考えられるが、潤滑剤を添加した場合、焼結体中に大量の炭素が残存し磁歪特性が劣化する傾向がある。
そこで本発明は、抜き圧を低減しつつ優れた磁歪特性を有する磁歪材料を製造する方法を提供することを目的とする。
However, the method for producing a magnetostrictive material proposed in Patent Document 6 has a problem in releasability due to a high pressure (hereinafter referred to as “extraction pressure”) when the molded body is taken out from the mold. Although it is conceivable to add a lubricant in order to reduce the punching pressure, when a lubricant is added, a large amount of carbon remains in the sintered body and the magnetostrictive characteristics tend to deteriorate.
Accordingly, an object of the present invention is to provide a method for producing a magnetostrictive material having excellent magnetostrictive characteristics while reducing the drawing pressure.
本発明者らは、原料Ａ及び原料Ｂの酸素量によって磁歪特性が変動すること、ならびに原料Ｂの酸素量と抜き圧が密接に関係していることを知見した。特に、原料Ｂについては、特開２００２−１２９２７４号公報に開示されている量を超える量の酸素を含むことにより、高い磁歪特性を得つつ抜き圧を低減することができることを知見した。この知見に基づく本発明の磁歪材料の製造方法は、式１：（ＴｂxＤｙ1-x）Ｔy（Ｔは、Ｆｅ、Ｎｉ、Ｃｏの群から選択される少なくとも１種類の金属元素であり、ｘ、ｙは０．３５＜ｘ≦０．５０、１．７０≦ｙ≦２．００の範囲）で表される原料Ａと、式２：ＤｙtＴ1-t（ｔは０．５≦ｔ≦１．００の範囲）で表される原料Ｂと、Ｔを含有する原料Ｃとを混合し、得られた混合粉末を所定圧力で磁場中成形し、得られた成形体を成形用金型から抜き出した後に、前記成形体を焼結して、式３：（ＴｂvＤｙ1-v）Ｔw（ｖ、ｗは０．２７≦ｖ＜０．５０、１．７０≦ｗ≦２．００の範囲にある。）で表される磁歪材料を製造する方法であって、原料Ａの酸素量を５００〜３０００ｐｐｍ、原料Ｂの酸素量を２０００〜７０００ｐｐｍとすることを特徴としている。原料Ｂにおいて、Ｄｙの一部がＴｂ及び／又はＨｏで置換されていてもよい。
本発明において、原料Ａの酸素量は１０００〜２５００ｐｐｍであること、原料Ｂの酸素量が３０００〜５０００ｐｐｍであること、原料Ｃの酸素量が５００〜３０００ｐｐｍであることが望ましい。
また本発明において、原料Ｂは水素を７０００〜２２０００ｐｐｍ含むことが望ましい。
The present inventors have found that the magnetostriction characteristics fluctuate depending on the oxygen amounts of the raw material A and the raw material B, and that the oxygen amount of the raw material B and the extraction pressure are closely related. In particular, regarding the raw material B, it has been found that the extraction pressure can be reduced while obtaining high magnetostriction characteristics by including oxygen in an amount exceeding that disclosed in JP-A-2002-129274. The manufacturing method of the magnetostrictive material of the present invention based on this knowledge is represented by the formula 1: (Tb x Dy 1-x ) T y (T is at least one metal element selected from the group of Fe, Ni, Co). , X, y is a raw material A represented by 0.35 <x ≦ 0.50, 1.70 ≦ y ≦ 2.00, and formula 2: Dy t T 1-t (t is 0.5 ≦ t ≦ 1.00)) and a raw material C containing T are mixed, the obtained mixed powder is molded in a magnetic field at a predetermined pressure, and the resulting molded body is used for molding. After being extracted from the mold, the molded body is sintered to obtain a formula 3: (Tb v Dy 1-v ) T w (v and w are 0.27 ≦ v <0.50, 1.70 ≦ w ≦ In the range of 2.00), wherein the oxygen content of the raw material A is 500 to 3000 ppm, and the oxygen content of the raw material B is 2000 to 7000 ppm. It is characterized by doing. In the raw material B, a part of Dy may be substituted with Tb and / or Ho.
In the present invention, it is desirable that the oxygen content of the raw material A is 1000 to 2500 ppm, the oxygen content of the raw material B is 3000 to 5000 ppm, and the oxygen content of the raw material C is 500 to 3000 ppm.
In the present invention, the raw material B preferably contains 7000-22000 ppm of hydrogen.
本発明によれば、原料Ａ及び原料Ｂ、さらには原料Ｃの酸素量を規制することにより、抜き圧を低減しつつ優れた磁歪特性を有する磁歪材料を提供することができる。 According to the present invention, it is possible to provide a magnetostrictive material having excellent magnetostrictive characteristics while reducing the extraction pressure by regulating the oxygen content of the raw material A and the raw material B, and further the raw material C.
以下に、本発明の実施の形態を図面に基づいて詳細に説明する。
図１は、本発明の一実施形態である磁歪材料の製造方法を示すフローチャートである。
本発明の磁歪材料の製造方法は、式１：（ＴｂxＤｙ1-x）Ｔyで表される原料Ａを用いる。ここで、原料ＡのＴは、Ｆｅ、Ｃｏ、Ｎｉの群から選択される少なくとも１種類の金属元素で、特に、ＴはＦｅ単独でもよい。Ｆｅは、Ｔｂ、Ｄｙと磁歪特性の高い（Ｔｂ、Ｄｙ）Ｆｅ2金属間化合物を形成するからである。このときに、Ｆｅの一部をＣｏ、Ｎｉで置換するものであってもよい。但し、Ｃｏは磁気異方性を大きくするが透磁率を低下させる。また、Ｎｉはキュリー温度を下げ、結果として常温・高磁場での磁歪値を低下させる。よって、Ｔに占めるＦｅの割合は７０ｗｔ％以上、一層好ましくは８０ｗｔ％以上が良い。その他に、ＴはＴｂ、Ｄｙ、Ｈｏの希土類金属と合金を形成する遷移金属元素を含んでいてもよい。遷移金属元素としては、具体的にはＭｎ、Ｃｒ、Ｍｏ、Ｗを挙げることができる。原料ＡのＴｂの一部は、Ｄｙ、Ｈｏを除く希土類元素（Ｒ'）と置換してもよい。Ｒ'として、例えば、Ｎｄ、Ｐｒ、Ｇｄ、Ｙ等を挙げることができる。
Embodiments of the present invention will be described below in detail with reference to the drawings.
FIG. 1 is a flowchart showing a method for manufacturing a magnetostrictive material according to an embodiment of the present invention.
The method for producing a magnetostrictive material of the present invention uses a raw material A represented by Formula 1: (Tb x Dy 1-x ) T y . Here, T of the raw material A is at least one metal element selected from the group of Fe, Co, and Ni. In particular, T may be Fe alone. This is because Fe forms a Tb, Dy and (Tb, Dy) Fe 2 intermetallic compound having high magnetostriction characteristics. At this time, a part of Fe may be substituted with Co or Ni. However, Co increases the magnetic anisotropy but decreases the magnetic permeability. Ni lowers the Curie temperature, and as a result, lowers the magnetostriction value at room temperature and high magnetic field. Therefore, the proportion of Fe in T is 70 wt% or more, more preferably 80 wt% or more. In addition, T may contain a transition metal element that forms an alloy with rare earth metals such as Tb, Dy, and Ho. Specific examples of the transition metal element include Mn, Cr, Mo, and W. A part of Tb of the raw material A may be substituted with rare earth elements (R ′) excluding Dy and Ho. Examples of R ′ include Nd, Pr, Gd, and Y.
式１において、ｘ、ｙは、０．３５＜ｘ≦０．５０、１．７０≦ｙ≦２．００の範囲にある。ｘが０．３５以下の小さい値となると、焼結後の［１１１］軸方向の配向度が低くなり、ｘが、０．５０を超えると、磁歪材料全体に対する原料Ａの比率が低下するために焼結後の［１１１］軸方向の配向度が低くなる。ｙが１．７０未満では、原料Ｃの混合比率を高くしなければならず、磁歪材料全体に占める原料Ａの比率が小さくなり、焼結後の［１１１］軸方向の配向度が低くなってしまう。ｙが２．００よりも大きいと（Ｔｂ、Ｄｙ）Ｔ3等のＦｅリッチの相が多くなり、このため、磁場中成形による配向度が低くなり、それにつれて焼結後の磁歪材料の配向度も低くなる。
ｘ、ｙの好ましい値は、０．３７≦ｘ≦０．４５、１．８５≦ｙ≦１．９８である。
In Formula 1, x and y are in the range of 0.35 <x ≦ 0.50 and 1.70 ≦ y ≦ 2.00. When x is a small value of 0.35 or less, the degree of orientation in the [111] axial direction after sintering becomes low, and when x exceeds 0.50, the ratio of the raw material A to the entire magnetostrictive material decreases. In addition, the degree of orientation in the [111] axial direction after sintering becomes low. When y is less than 1.70, the mixing ratio of the raw material C must be increased, the ratio of the raw material A to the entire magnetostrictive material is reduced, and the degree of orientation in the [111] axial direction after sintering is reduced. End up. When y is larger than 2.00, there are many Fe-rich phases such as (Tb, Dy) T 3 , and therefore the degree of orientation due to molding in a magnetic field is lowered, and the degree of orientation of the magnetostrictive material after sintering is accordingly increased. Also lower.
Preferred values of x and y are 0.37 ≦ x ≦ 0.45 and 1.85 ≦ y ≦ 1.98.
本発明は、原料Ａの酸素量を５００〜３０００ｐｐｍの範囲に規制する。工業的な生産規模で５００ｐｐｍ未満にするのは困難であり、また３０００ｐｐｍを超えると磁歪値が低下するためである。原料Ａの酸素量は望ましくは１０００〜２５００ｐｐｍ、さらに望ましくは１０００〜２０００ｐｐｍである。
また、本発明は、原料Ａの粒径（平均粒径）を１〜２００μｍの範囲にすることが望ましい。原料Ａは磁歪特性に影響するもので、焼結後に主相を構成する。原料Ａの粒径が小さい場合は、磁場を印加したときの粒子の回転が容易でなくなり、配向度の低下をもたらす。また、比表面積が大きくなるために、酸素量が増加する。酸素含有により形成された異相が主相の存在量を低下させることにより磁歪特性を低下させる。逆に原料Ａの粒径が大きくなると、一粒子中に複数の結晶が含まれることになり、配向度の向上を阻害する。また、高密度化の妨げにもなる。そこで、原料Ａの平均粒径は１〜２００μｍの範囲にすることが望ましい。より望ましい原料Ａの平均粒径は２〜１００μｍ、さらに望ましい原料Ａの平均粒径は５〜５０μｍである。なお、これらの平均粒径は、フィッシャー社製サブシーブサイザーによって測定される値である。
In the present invention, the oxygen content of the raw material A is restricted to a range of 500 to 3000 ppm. This is because it is difficult to make it less than 500 ppm on an industrial production scale, and when it exceeds 3000 ppm, the magnetostriction value decreases. The amount of oxygen in the raw material A is desirably 1000 to 2500 ppm, and more desirably 1000 to 2000 ppm.
In the present invention, it is desirable that the particle size (average particle size) of the raw material A is in the range of 1 to 200 μm. Raw material A affects the magnetostrictive characteristics and constitutes the main phase after sintering. When the particle diameter of the raw material A is small, the rotation of the particles becomes difficult when a magnetic field is applied, and the degree of orientation is lowered. Moreover, since the specific surface area becomes large, the amount of oxygen increases. The heterogeneous phase formed by containing oxygen reduces the abundance of the main phase, thereby reducing the magnetostriction characteristics. Conversely, when the particle diameter of the raw material A is increased, a plurality of crystals are contained in one particle, which hinders improvement in the degree of orientation. It also hinders higher density. Therefore, the average particle diameter of the raw material A is desirably in the range of 1 to 200 μm. The more preferable average particle diameter of the raw material A is 2 to 100 μm, and the further preferable average particle diameter of the raw material A is 5 to 50 μm. In addition, these average particle diameters are values measured by a Fischer sub-sieve sizer.
また、本発明の磁歪材料の製造方法は、式２：ＤｙtＴ1-tで表され原料Ｂを用いる。原料ＢのＴは、Ｆｅ、Ｃｏ、Ｎｉの群から選択される少なくとも１種類の金属元素で、特に、ＴはＦｅ単独でもよい。このときに、Ｆｅの一部をＣｏ、Ｎｉで置換するものであってもよく、これにより原料Ｂは粉砕されやすくなり、焼結による焼結密度を高くすることができる。原料ＢのＤｙは、その一部がＴｂ及び／又はＨｏと置換されていてもよい。ｔは、０．５≦ｔ≦１．００の範囲にある。ＤｙとＴは共晶点を有するので、ｔがこの範囲以外の組成では、原料Ｂを原料Ａと原料Ｃと混合する際に、共晶組成であるＲ2Ｔが少なくなり、焼結密度を高くすることが難しくなる。
ｔの好ましい値は、０．５≦ｔ≦０．８、より好ましい値は０．６≦ｔ≦０．７である。
A method of manufacturing a magnetostrictive material of the present invention have the formula 2: represented by Dy t T 1-t is used raw material B. T of the raw material B is at least one metal element selected from the group of Fe, Co, and Ni. In particular, T may be Fe alone. At this time, a part of Fe may be substituted with Co and Ni, whereby the raw material B becomes easy to be pulverized and the sintering density by sintering can be increased. Part of Dy of the raw material B may be substituted with Tb and / or Ho. t is in the range of 0.5 ≦ t ≦ 1.00. Since Dy and T have a eutectic point, when t is outside this range, when raw material B is mixed with raw material A and raw material C, R 2 T, which is the eutectic composition, decreases and the sintering density is reduced. It becomes difficult to raise.
A preferable value of t is 0.5 ≦ t ≦ 0.8, and a more preferable value is 0.6 ≦ t ≦ 0.7.
また、原料Ｂは、７０００ｐｐｍ≦水素量≦２２０００ｐｐｍの水素を含むべきである。原料Ｂは水素を吸蔵することにより脆化し、これを原料Ａと原料Ｃと混合し、成形体を形成する時の圧力により混合した状態の内部で粉砕されて微細化する。したがって、原料Ａの間に入り込みやすくなり、焼結したときに緻密で密度の高い焼結体を形成する。 The raw material B should contain hydrogen of 7000 ppm ≦ hydrogen content ≦ 22000 ppm. The raw material B becomes brittle by occlusion of hydrogen, and this is mixed with the raw material A and the raw material C, and is pulverized and refined inside the mixed state by the pressure when forming the molded body. Therefore, it becomes easy to enter between the raw materials A, and when sintered, a dense and dense sintered body is formed.
原料Ｂに、吸蔵させる水素の量としては、７０００ｐｐｍ≦水素量≦２２０００ｐｐｍの範囲がよい。水素の量が７０００ｐｐｍ未満では、水素の量が少なくて原料Ｂの内部歪みが小さく、成形時の割れが少なく、密度が低く、さらに開気孔も多くなる。さらに、長期間の使用により磁歪特性が低下する。また、水素量が２２０００ｐｐｍを超えると、原料Ｂの微細化が飽和し、これ以上吸蔵する効果がない。 The amount of hydrogen stored in the raw material B is preferably in the range of 7000 ppm ≦ hydrogen amount ≦ 22000 ppm. When the amount of hydrogen is less than 7000 ppm, the amount of hydrogen is small, the internal strain of the raw material B is small, cracks during molding are small, the density is low, and open pores are also increased. In addition, the magnetostriction characteristics deteriorate due to long-term use. Moreover, when the amount of hydrogen exceeds 22000 ppm, the refinement | miniaturization of the raw material B will be saturated and there will be no effect which occludes any more.
本発明は、原料Ｂの酸素量を２０００〜７０００ｐｐｍに規制する。原料Ｂは原料ＡよりもＲの含有量が多い（原料Ｂは原料ＡよりもＴに対するＲの占める割合が高い）ため、非常に活性である。非常に活性な原料Ｂを含んだ状態で成形を行うと、発火のおそれがある。また、非常に活性な状態では、炭素等の他の元素との反応が起こりやすく、磁歪特性の劣化、ばらつきを生じさせる。そこで、原料Ｂについては、活性度を低減するために、あらかじめ２０００ｐｐｍ以上の酸素を含ませる。
原料Ｂの酸素量は抜き圧に与える影響が大きい。原料Ｂの酸素量が２０００ｐｐｍ未満では、粉の活性度が高いために金型との付着がおきやすく、抜き圧が３．０ｔｏｎ／ｃｍ2以上となる。このレベルまで抜き圧が高くなると、金型寿命が短くなる、成形体に欠け，割れが生じ歩留まりが低下するという問題がある。一方、原料Ｂの酸素量を２０００ｐｐｍ以上とすることにより、磁歪特性に悪影響を及ぼしうる潤滑剤を添加することなく、抜き圧を低減することができる。
ただし、酸素量が多すぎると、高い磁歪特性を得ることができない。そこで原料Ｂの酸素量は２０００〜７０００ｐｐｍとする。原料Ｂの望ましい酸素量は３０００〜６０００ｐｐｍ、さらに望ましい酸素量は４０００〜５５００ｐｐｍである。
また、本発明は、原料Ｂの粒径（平均粒径）を０．１〜１００μｍの範囲にすることが望ましい。原料Ｂは焼結後に主に粒界相を形成する。原料Ｂの粒径が小さくなると、やはり酸素量が増加する。逆に原料Ｂの粒径が大きくなると焼結密度が高くなりにくくなる。そこで、原料Ｂの平均粒径は０．１〜１００μｍの範囲にすることが望ましい。より望ましい原料Ｂの平均粒径は０．２〜７０μｍ、さらに望ましい原料Ｂの平均粒径は５〜５０μｍである。
In the present invention, the oxygen content of the raw material B is regulated to 2000 to 7000 ppm. Since the raw material B has a higher R content than the raw material A (the raw material B has a higher ratio of R to T than the raw material A) , it is very active. If molding is performed in a state containing the very active raw material B, there is a risk of ignition. Also, in a very active state, reaction with other elements such as carbon is likely to occur, causing deterioration and variation in magnetostriction characteristics. Therefore, the raw material B contains 2000 ppm or more of oxygen in advance in order to reduce the activity.
The amount of oxygen in the raw material B has a great influence on the extraction pressure. If the amount of oxygen in the raw material B is less than 2000 ppm, the powder has high activity, so that it easily adheres to the mold, and the extraction pressure becomes 3.0 ton / cm 2 or more. When the punching pressure is increased to this level, there are problems that the mold life is shortened, the molded body is chipped and cracked, and the yield is lowered. On the other hand, by setting the oxygen content of the raw material B to 2000 ppm or more, the extraction pressure can be reduced without adding a lubricant that may adversely affect the magnetostriction characteristics.
However, if the amount of oxygen is too large, high magnetostriction characteristics cannot be obtained. Therefore, the oxygen content of the raw material B is set to 2000 to 7000 ppm. A desirable oxygen amount of the raw material B is 3000 to 6000 ppm, and a more desirable oxygen amount is 4000 to 5500 ppm.
In the present invention, the particle size (average particle size) of the raw material B is desirably in the range of 0.1 to 100 μm. The raw material B mainly forms a grain boundary phase after sintering. As the particle size of the raw material B becomes smaller, the amount of oxygen also increases. Conversely, when the particle size of the raw material B is increased, the sintered density is difficult to increase. Therefore, the average particle size of the raw material B is desirably in the range of 0.1 to 100 μm. A more preferable average particle diameter of the raw material B is 0.2 to 70 μm, and a further preferable average particle diameter of the raw material B is 5 to 50 μm.
本発明の磁歪材料の製造方法は、Ｔを含む原料Ｃを用いる。Ｔは、上述したように、Ｆｅ、Ｃｏ、Ｎｉの群から選択させる少なくとも１種類の金属元素である。その他に、Ｔｂ、Ｄｙ、Ｈｏの希土類金属元素と合金を形成する遷移金属元素を含んでいてもよい。遷移金属元素としては、具体的にはＭｎ、Ｃｒ、Ｍｏ、Ｗを挙げることができる。 The method for producing a magnetostrictive material of the present invention uses a raw material C containing T. As described above, T is at least one metal element selected from the group of Fe, Co, and Ni. In addition, the transition metal element which forms an alloy with the rare earth metal elements of Tb, Dy, and Ho may be included. Specific examples of the transition metal element include Mn, Cr, Mo, and W.
本発明は、原料Ｃの酸素量を特に規制するものではなく、１０００〜７０００ｐｐｍの範囲にあればよい。
また、本発明は、原料Ｃの粒径（平均粒径）を０．５〜１００μｍの範囲にすることが望ましい。原料Ｃの粒径が小さい場合は、やはり酸素量が増加する。逆に原料Ｃの粒径が大きくなると、焼結密度が高くなりにくくなる。そこで、原料Ｃの平均粒径は０．５〜１００μｍの範囲にすることが望ましい。より望ましい原料Ｃの平均粒径は０．５〜５０μｍ、さらに望ましい原料Ｃの平均粒径は０．５〜３０μｍである。
In the present invention, the oxygen content of the raw material C is not particularly restricted, and may be in the range of 1000 to 7000 ppm.
In the present invention, it is desirable that the particle size (average particle size) of the raw material C be in the range of 0.5 to 100 μm. When the particle size of the raw material C is small, the amount of oxygen also increases. Conversely, when the particle size of the raw material C is increased, the sintered density is less likely to be increased. Therefore, the average particle size of the raw material C is desirably in the range of 0.5 to 100 μm. A more preferable average particle diameter of the raw material C is 0.5 to 50 μm, and a further preferable average particle diameter of the raw material C is 0.5 to 30 μm.
また、本発明の磁歪材料の製造方法は、前記原料Ａと原料Ｂと原料Ｃとを混合し、焼結して、式３：（ＴｂvＤｙ1-v）Ｔwで表される磁歪材料を製造するものである。ここで、ｖ、ｗは、０．２７≦ｖ＜０．５０、１．７０≦ｗ≦２．００の範囲にある。ｖが０．２７未満では、常温より低い温度域で十分な磁歪値を示さず、ｖが０．５０以上では常温域で十分な磁歪値を示さない。ｗが１．７０未満では希土類リッチな相が多くなり、ｗが２．００を超えると、（Ｔｂ、Ｄｙ）Ｔ3相等の異相が生じ磁歪値が低下する。好ましいｖは０．２７≦ｖ≦０．４０、より好ましくは０．２７≦ｖ≦０．３３である。好ましいｗは１．８０≦ｗ≦１．９５、より好ましくは１．８５≦ｗ≦１．９０である。 Also, in the method for producing a magnetostrictive material according to the present invention, the raw material A, the raw material B, and the raw material C are mixed and sintered, and the magnetostrictive material represented by the formula 3: (Tb v Dy 1-v ) T w Is to be manufactured. Here, v and w are in the range of 0.27 ≦ v <0.50 and 1.70 ≦ w ≦ 2.00. When v is less than 0.27, a sufficient magnetostriction value is not shown in a temperature range lower than room temperature, and when v is 0.50 or more, a sufficient magnetostriction value is not shown in a room temperature range. If w is less than 1.70, the number of rare earth-rich phases increases. If w exceeds 2.00, a different phase such as a (Tb, Dy) T 3 phase is generated and the magnetostriction value is lowered. Preferred v is 0.27 ≦ v ≦ 0.40, more preferably 0.27 ≦ v ≦ 0.33. Preferred w is 1.80 ≦ w ≦ 1.95, more preferably 1.85 ≦ w ≦ 1.90.
前記原料Ａと原料Ｂと原料Ｃとの混合の割合は、式３で表される磁歪材料になるように適宜決定することができる。磁歪材料に対して、原料Ａは５０ｗｔ％以上で１００ｗｔ％未満、一層好ましくは６０ｗｔ％以上で９５ｗｔ％以下である。原料Ａが５０ｗｔ％より少ないと、磁場中成形で配向するものが少なく、焼結した磁歪材料の配向度が低くくなる。原料Ａが多いと、水素を含有した原料Ｂが少なくなるために、焼結密度が高くならず、又、開気孔も多くなるために長期間の使用により飽和磁歪値が低下する。磁歪材料に対して、原料Ｂは４０ｗｔ％以下で、一層好ましくは５ｗｔ％以上で３０ｗｔ％以下がよい。原料Ｂが少ないと、焼結が進みにくく、緻密で密度の高い焼結体を得ることができない。原料Ｂが多いと、原料Ａが少なくなるため飽和磁歪定数が低下する。また、原料Ｃは、磁歪材料としたとき式３のＴの範囲になるように、原料Ａ、Ｂの割合を考慮して、添加量を決定する。 The mixing ratio of the raw material A, the raw material B, and the raw material C can be determined as appropriate so that the magnetostrictive material represented by Formula 3 is obtained. For the magnetostrictive material, the raw material A is 50 wt% or more and less than 100 wt%, more preferably 60 wt% or more and 95 wt% or less. When the amount of the raw material A is less than 50 wt%, there is little that is oriented by molding in a magnetic field, and the degree of orientation of the sintered magnetostrictive material is low. When the amount of the raw material A is large, the raw material B containing hydrogen decreases, so that the sintered density does not increase, and the number of open pores increases, so that the saturation magnetostriction value decreases due to long-term use. For the magnetostrictive material, the raw material B is 40 wt% or less, more preferably 5 wt% or more and 30 wt% or less. When the amount of the raw material B is small, sintering is difficult to proceed, and a dense and dense sintered body cannot be obtained. If the amount of the raw material B is large, the amount of the raw material A is decreased, so that the saturation magnetostriction constant is lowered. In addition, when the raw material C is a magnetostrictive material, the amount of the raw material C is determined in consideration of the ratio of the raw materials A and B so as to be in the range of T in Formula 3.
これらの原料Ａ、Ｂ、Ｃは、図１に示すように、秤量してから混合し、粉砕処理される。粉砕処理では、湿式ボールミル、アトライタ、アトマイザー等の粉砕機から適宜選択することができる。特に、アトマイザーが好ましい。衝撃と剪断を同時にかけることができ、粉体の凝集を防ぎ、かつ生産性が高いからである。混合したものは、焼結前に所望の形状に成形するが、この成形を磁場中で行うことで、原料Ａ等を一定方向に揃えて、焼結後の磁歪材料を［１１１］軸方向に配向させる。印加する磁場は、２．４×１０4Ａ／ｍ以上、好ましくは４．８×１０4Ａ／ｍ以上がよい。磁場の方向は、圧力の方向に垂直でも、平行でもよい。成形圧力は、４．９×１０4Ｐａ以上、好ましくは２．９×１０5Ｐａ以上がよい。また、成形体の焼結条件は、適宜行うことができるが、１１００℃以上で、好ましくは１１５０〜１２５０℃で、１〜１０時間行うことがよい。焼結の雰囲気は、非酸化性雰囲気が良く、Ａｒガス等の不活性ガス又は真空中がよい。 These raw materials A, B, and C are weighed, mixed, and pulverized as shown in FIG. In the pulverization treatment, a pulverizer such as a wet ball mill, an attritor, or an atomizer can be appropriately selected. In particular, an atomizer is preferable. This is because impact and shear can be applied at the same time, preventing aggregation of the powder and high productivity. The mixed material is formed into a desired shape before sintering. By performing this forming in a magnetic field, the raw materials A and the like are aligned in a certain direction, and the sintered magnetostrictive material is aligned in the [111] axial direction. Orient. The applied magnetic field is 2.4 × 10 4 A / m or more, preferably 4.8 × 10 4 A / m or more. The direction of the magnetic field may be perpendicular or parallel to the direction of pressure. The molding pressure is 4.9 × 10 4 Pa or more, preferably 2.9 × 10 5 Pa or more. Moreover, although the sintering conditions of a molded object can be performed suitably, it is good to carry out at 1100 degreeC or more, Preferably it is 1150-1250 degreeC for 1 to 10 hours. The sintering atmosphere is preferably a non-oxidizing atmosphere, and is preferably an inert gas such as Ar gas or in a vacuum.
このようにして製造された磁歪材料は、多結晶体であり、磁歪が最も大きくなる［１１１］軸方向に配向している。この磁歪材料の結晶粒の平均粒径は、１０μｍ以上である。結晶粒の平均粒径が小さいと結晶粒界が多くなり外部磁場による磁化率が低くなる。結晶粒の平均粒径の上限は特にないが、２００μｍ以上になると磁歪値はほとんど飽和するためにこれ以上大きくする必要がなく、また、焼結等の時間がかかりすぎ実用的ではない。 The magnetostrictive material manufactured in this way is a polycrystal and is oriented in the [111] axial direction where the magnetostriction is greatest. The average grain size of crystal grains of the magnetostrictive material is 10 μm or more. If the average grain size of the crystal grains is small, the crystal grain boundaries increase and the magnetic susceptibility due to the external magnetic field decreases. The upper limit of the average grain size of the crystal grains is not particularly limited. However, if the grain size is 200 μm or more, the magnetostriction value is almost saturated and does not need to be increased any more.
原料Ａとして、Ｔｂ0.4Ｄｙ0.6Ｆｅ1.95の組成となるようにＴｂ、Ｄｙ、Ｆｅを秤量し、Ａｒガス雰囲気中で溶解して原料合金を作製した。この合金に１１７０℃で２０時間保持するアニール処理を施し、合金作製時の各金属元素の濃度分布を一様にし、また、析出した異相を消滅させた。次に、図１に示すように、このアニール処理した原料合金をブラウンミルにて粉砕（粗粉砕）する。粗粉砕後、メッシュにて２ｍｍ以上の粗大粒子を除去した。粗大粒子除去後の粉末の平均粒径は５００μｍである。なお、平均粒径はサブシーブサイザー測定装置（フィッシャー社製）で測定した値である。また、粉末の取り扱い条件を変えることにより、種々の酸素量の原料Ａを得た。
ここで、酸素量は、酸素量測定装置（ＨＯＲＩＢＡ社製：ＺＷＧＡ−６５０Ａ）で、また後述する水素量は、水素量測定装置（ＨＯＲＩＢＡ社製：ＺＷＧＡ−Ｇ２１）で測定した値である。
As the raw material A, Tb, Dy, and Fe were weighed so as to have a composition of Tb 0.4 Dy 0.6 Fe 1.95 and dissolved in an Ar gas atmosphere to prepare a raw material alloy. This alloy was annealed at 1170 ° C. for 20 hours to make the concentration distribution of each metal element uniform during the preparation of the alloy, and the precipitated heterogeneous phase disappeared. Next, as shown in FIG. 1, the annealed raw material alloy is pulverized (coarsely pulverized) with a brown mill. After coarse pulverization, coarse particles of 2 mm or more were removed with a mesh. The average particle size of the powder after removal of coarse particles is 500 μm. In addition, an average particle diameter is the value measured with the subsieve sizer measuring apparatus (made by a Fischer company). Moreover, the raw material A of various oxygen amount was obtained by changing the powder handling conditions.
Here, the oxygen amount is a value measured with an oxygen amount measuring device (manufactured by HORIBA: ZWGA-650A), and the hydrogen amount described later is a value measured with a hydrogen amount measuring device (manufactured by HORIBA: ZWGA-G21).
原料Ｂとして、Ｄｙ2.0Ｆｅ（ｔ＝０．６７）の組成になるようにＤｙ、Ｆｅを秤量して、Ａｒガス雰囲気中で溶解して原料合金を作製した。この原料合金をブラウンミルにて粉砕して原料Ｂとする。次に原料Ｂに対して、水素ガス雰囲気中、１５０℃で１時間保持する水素吸蔵処理を行った。この処理により、原料Ｂの結晶格子中に水素原子が侵入し、又は水素化物になる。また、この処理により原料Ｂには多数の割れが発生する。その後、メッシュにて２ｍｍ以上の粗大粒子を除去した。粗大粒子除去後の粉末の平均粒径は５００μｍである。なお、粉末の取り扱い条件を変えることにより、種々の酸素量の原料Ｂを得た。また、このときの各原料Ｂの水素量は１７８００〜１８２００ｐｐｍの範囲にあった。 As the raw material B, Dy and Fe were weighed so as to have a composition of Dy 2.0 Fe (t = 0.67) and dissolved in an Ar gas atmosphere to prepare a raw material alloy. This raw material alloy is pulverized by a brown mill to form a raw material B. Next, the hydrogen storage process which hold | maintains at 150 degreeC in the hydrogen gas atmosphere for 1 hour with respect to the raw material B was performed. By this treatment, hydrogen atoms enter the crystal lattice of the raw material B or become hydrides. Moreover, many cracks generate | occur | produce in the raw material B by this process. Thereafter, coarse particles of 2 mm or more were removed with a mesh. The average particle size of the powder after removal of coarse particles is 500 μm. In addition, the raw material B of various oxygen amount was obtained by changing the handling conditions of powder. Moreover, the hydrogen content of each raw material B at this time was in the range of 17800 to 18200 ppm.
原料Ｃとして、３００℃の水素ガス雰囲気中で酸素を除去する還元処理を１時間行った平均粒径８μｍのＦｅ粉末を用いた。原料Ｃの酸素量は２０００ｐｐｍ程度である。 As the raw material C, Fe powder having an average particle diameter of 8 μm subjected to reduction treatment for removing oxygen in a hydrogen gas atmosphere at 300 ° C. for 1 hour was used. The oxygen content of the raw material C is about 2000 ppm.
以上の原料を、以下の最終組成になるように秤量、混合した。
組成ａ：Ｔｂ0.36Ｄｙ0.64Ｆｅ1.87
組成ｂ：Ｔｂ0.34Ｄｙ0.66Ｆｅ1.87
組成ｃ：Ｔｂ0.30Ｄｙ0.70Ｆｅ1.87
組成ｄ：Ｔｂ0.28Ｄｙ0.72Ｆｅ1.87
The above raw materials were weighed and mixed so as to have the following final composition.
Composition a: Tb 0.36 Dy 0.64 Fe 1.87
Composition b: Tb 0.34 Dy 0.66 Fe 1.87
Composition c: Tb 0.30 Dy 0.70 Fe 1.87
Composition d: Tb 0.28 Dy 0.72 Fe 1.87
次いで、アトマイザー （東京アトマイザー製造（株）社製）を用いてＡｒガス雰囲気中で粉砕して平均粒径９μｍの微粉砕粉末を得た。次いで、微粉砕粉末を１２ｋＯｅの磁場中で８ｔｏｎ／ｃｍ2の圧力で磁場中成形を行い、１２ｍｍ×１２ｍｍ×１６ｍｍのサイズを有する成形体を作製した。なお、成形は加圧方向に対して磁場垂直方向に印加する横磁場成形とした。各成形体の抜き圧を測定した結果を表１〜表８に示す。抜き圧は成形体をプレスした後、金型から成形体を抜き出す際の最大荷重とした。
得られた成形体を１２３５℃のＡｒガス雰囲気中において３時間焼結した。
Subsequently, it was pulverized in an Ar gas atmosphere using an atomizer (manufactured by Tokyo Atomizer Manufacturing Co., Ltd.) to obtain a finely pulverized powder having an average particle size of 9 μm. Subsequently, the finely pulverized powder was molded in a magnetic field at a pressure of 8 ton / cm 2 in a magnetic field of 12 kOe to produce a molded body having a size of 12 mm × 12 mm × 16 mm. The forming was transverse magnetic field forming in which the magnetic field was applied in the direction perpendicular to the pressing direction. Tables 1 to 8 show the results of measuring the punching pressure of each molded body. The punching pressure was the maximum load when the molded body was extracted from the mold after pressing the molded body.
The obtained molded body was sintered in an Ar gas atmosphere at 1235 ° C. for 3 hours.
得られた焼結体の磁歪値（λ1.0）を測定した。その結果を表１〜表８に示す。なお、表１及び表２は組成ａによる焼結体の測定結果、表３及び表４は組成ｂによる焼結体の測定結果、表５及び表６は組成ｃによる焼結体の測定結果、表７及び表８は組成ｄによる焼結体の測定結果を示している。 The magnetostriction value (λ 1.0 ) of the obtained sintered body was measured. The results are shown in Tables 1-8. Tables 1 and 2 show the measurement results of the sintered body with the composition a, Tables 3 and 4 show the measurement results of the sintered body with the composition b, Tables 5 and 6 show the measurement results of the sintered body with the composition c, Tables 7 and 8 show the measurement results of the sintered body with the composition d.
表１、３、５及び７に示すように、原料Ａの酸素量が低いほど磁歪特性は向上する。原料Ａの酸素量を３０００ｐｐｍ以下にすることにより１０００ｐｐｍ以上の磁歪値（λ1.0）を得ることができる。ただし、原料Ａの酸素量を５００ｐｐｍ未満にすることは工業的生産規模では困難であることから、原料Ａの酸素量は５００〜３０００ｐｐｍの範囲とした。
また、表２、４、６及び８に示すように、原料Ｂについては、酸素量が増加するにつれて抜き圧が小さくなる。酸素量が２０００〜７０００ｐｐｍと本発明が推奨する範囲内であれば、１０００ｐｐｍ以上の磁歪値（λ1.0）を得つつ、抜き圧を３．０ｔｏｎ／ｃｍ2より小さくすることができる。
As shown in Tables 1, 3, 5 and 7, the lower the amount of oxygen in the raw material A, the better the magnetostriction characteristics. By setting the oxygen content of the raw material A to 3000 ppm or less, a magnetostriction value (λ 1.0 ) of 1000 ppm or more can be obtained. However, since it is difficult to reduce the oxygen content of the raw material A to less than 500 ppm on an industrial production scale, the oxygen content of the raw material A is set in the range of 500 to 3000 ppm.
Further, as shown in Tables 2, 4, 6, and 8, with regard to the raw material B, the extraction pressure decreases as the oxygen amount increases. If the amount of oxygen is within the range recommended by the present invention of 2000 to 7000 ppm, the drawing pressure can be made smaller than 3.0 ton / cm 2 while obtaining a magnetostriction value (λ 1.0 ) of 1000 ppm or more.
Claims (6)
式２：ＤｙtＴ1-t（ｔは０．５≦ｔ≦１．００の範囲）で表される原料Ｂと、
前記Ｔを含有する原料Ｃとを混合し、得られた混合粉末を所定圧力で磁場中成形し、得られた成形体を成形用金型から抜き出した後に、前記成形体を焼結して、
式３：（ＴｂvＤｙ1-v）Ｔw（ｖ、ｗは０．２７≦ｖ＜０．５０、１．７０≦ｗ≦２．００の範囲にある。）で表される磁歪材料を製造する方法であって、
前記原料Ａの酸素量を５００〜３０００ｐｐｍ、前記原料Ｂの酸素量を２０００〜７０００ｐｐｍとすることを特徴とする磁歪材料の製造方法。 Formula 1: (Tb x Dy 1-x ) T y (T is at least one metal element selected from the group of Fe, Ni, and Co, and x and y are 0.35 <x ≦ 0.50. 1. A range of 1.70 ≦ y ≦ 2.00),
Formula 2: Dy t T 1-t (t is a range of 0.5 ≦ t ≦ 1.00),
The raw material C containing T is mixed, the obtained mixed powder is molded in a magnetic field at a predetermined pressure, and after the obtained molded body is extracted from the molding die, the molded body is sintered,
A magnetostrictive material represented by Formula 3: (Tb v Dy 1-v ) T w (v and w are in the range of 0.27 ≦ v <0.50 and 1.70 ≦ w ≦ 2.00) A method of manufacturing comprising:
A method for producing a magnetostrictive material, wherein the raw material A has an oxygen content of 500 to 3000 ppm, and the raw material B has an oxygen content of 2000 to 7000 ppm.
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