JP2005036302A5 - Rare earth-containing alloy manufacturing method, rare earth-containing alloy, rare earth-containing alloy powder manufacturing method, rare earth-containing alloy powder, rare earth-containing alloy sintered body manufacturing method, rare earth-containing alloy sintered body, magnetostrictive element, magnetostrictive material, magnetic refrigeration operation Material, magnetostrictive sensor, and magnetostrictive vibrator - Google Patents

Rare earth-containing alloy manufacturing method, rare earth-containing alloy, rare earth-containing alloy powder manufacturing method, rare earth-containing alloy powder, rare earth-containing alloy sintered body manufacturing method, rare earth-containing alloy sintered body, magnetostrictive element, magnetostrictive material, magnetic refrigeration operation Material, magnetostrictive sensor, and magnetostrictive vibrator Download PDF

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JP2005036302A5
JP2005036302A5 JP2003349682A JP2003349682A JP2005036302A5 JP 2005036302 A5 JP2005036302 A5 JP 2005036302A5 JP 2003349682 A JP2003349682 A JP 2003349682A JP 2003349682 A JP2003349682 A JP 2003349682A JP 2005036302 A5 JP2005036302 A5 JP 2005036302A5
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本発明は、希土類含有合金（以下「ＲＥ−含有合金」と呼ぶ）の製造方法、ＲＥ−含有合金、ＲＥ−含有合金粉末の製造方法、ＲＥ−含有合金粉末、ＲＥ−含有合金焼結体の製造方法、ＲＥ−含有合金焼結体、磁歪素子、磁歪材料、磁気冷凍作業物質、磁歪センサー、及び磁歪振動子に係り、特に、磁歪素子あるいは磁気冷凍作業物質等として好適に用いられるＮａＺｎ１３型ＲＥ−含有合金を製造する技術に関するものである。 The present invention relates to a method for producing a rare earth-containing alloy (hereinafter referred to as “RE-containing alloy”), an RE-containing alloy, a method for producing an RE-containing alloy powder, an RE-containing alloy powder, and an RE-containing alloy sintered body. manufacturing method, RE- containing alloy sintered body, the magnetostrictive element, the magnetostrictive material, a magnetic refrigeration working substance, a magnetostrictive sensor, and relates to a magnetostrictive transducer, particularly, NaZn 13 type which is suitably used as a magnetostrictive element or magnetic refrigeration working substance such as The present invention relates to a technique for producing an RE-containing alloy.

そこで本発明はかかる事情に鑑みてなされたものであり、長時間の熱処理工程を必要とすることなく効率良くＮａＺｎ１３型ＲＥ−含有合金を製造することが可能な技術、および該技術により得られるＮａＺｎ１３型ＲＥ−含有合金、並びに該ＮａＺｎ１３型ＲＥ−含有合金を用いて得られる磁歪素子、磁歪材料、磁気冷凍作業物質、磁歪センサー、及び磁歪振動子を提供することを目的とする。 Therefore, the present invention has been made in view of such circumstances, and a technique capable of efficiently producing a NaZn 13 type RE-containing alloy without requiring a long heat treatment step, and obtained by the technique. An object is to provide a NaZn 13 type RE-containing alloy, and a magnetostrictive element , a magnetostrictive material, a magnetic refrigeration material , a magnetostrictive sensor, and a magnetostrictive vibrator obtained by using the NaZn 13 type RE-containing alloy.

本発明者は上記課題を解決するべく検討を行った結果、以下のＲＥ−含有合金の製造方法、ＲＥ−含有合金、ＲＥ−含有合金粉末の製造方法、ＲＥ−含有合金粉末、ＲＥ−含有合金焼結体の製造方法、ＲＥ−含有合金焼結体、磁歪素子、磁歪材料、磁気冷凍作業物質、磁歪センサー、及び磁歪振動子を発明するに到った。 As a result of studies conducted by the present inventor to solve the above problems, the following RE-containing alloy manufacturing method, RE-containing alloy, RE-containing alloy powder manufacturing method, RE-containing alloy powder, and RE-containing alloy are described below. It came to invent the manufacturing method of a sintered compact, RE-containing alloy sintered compact, a magnetostrictive element, a magnetostrictive material, a magnetic freezing working substance , a magnetostrictive sensor, and a magnetostrictive vibrator .

（１０） 一般式Ｒ（Ｔ１−ｘＡｘ）１３−ｙ（但し、ＲはＬａ、Ｃｅ、Ｐｒ、Ｎｄ、Ｓｍ、Ｅｕ、Ｔｂ、Ｄｙ、Ｈｏ、Ｔｍ、Ｙｂ、Ｇｄ及びＬｕから選択される少なくとも１種、ＴはＦｅ、Ｃｏ、Ｎｉ、Ｍｎ、Ｐｔ及びＰｄから選択される少なくとも１種、ＡはＡｌ、Ａｓ、Ｓｉ、Ｇａ、Ｇｅ、Ｍｎ、Ｓｎ及びＳｂから選択される少なくとも１種、０．０５≦ｘ≦０．２、−１≦ｙ≦１）で表される希土類含有合金において、
ＮａＺｎ１３相の存在比率が９０ｖｏｌ％以上であることを特徴とする希土類含有合金。
（１１） 項（８）から項（１０）までのいずれか１項に記載の希土類含有合金を用いて製造されたことを特徴とする磁歪素子。
（１２） 項（８）から項（１０）までのいずれか１項に記載の希土類含有合金を用いて製造されたことを特徴とする磁気冷凍作業物質。
本発明の磁歪素子および磁気冷凍作業物質は、いずれも上記の本発明の第２のＲＥ−含有合金（ＮａＺｎ１３型ＲＥ−含有合金）を用いて製造されたことを特徴とするものである。 (10) General formula R (T 1-x A x ) 13-y (where R is selected from La, Ce, Pr, Nd, Sm, Eu, Tb, Dy, Ho, Tm, Yb, Gd and Lu) At least one selected from the group consisting of Fe, Co, Ni, Mn, Pt and Pd, and A selected from at least one selected from Al, As, Si, Ga, Ge, Mn, Sn and Sb. , 0.05 ≦ x ≦ 0.2, −1 ≦ y ≦ 1)
A rare earth-containing alloy characterized in that the abundance ratio of NaZn 13 phase is 90 vol% or more.
(11) A magnetostrictive element manufactured using the rare earth-containing alloy according to any one of items (8) to (10).
(12) A magnetic refrigeration work material produced using the rare earth-containing alloy according to any one of items (8) to (10).
Both the magnetostrictive element and the magnetic refrigeration work material of the present invention are characterized by being manufactured using the above-described second RE-containing alloy (NaZn 13 type RE-containing alloy) of the present invention.

（１６） 項（１５）に記載の希土類含有合金粉末に水素を吸蔵させてキュリー温度を制御してなることを特徴とする磁気冷凍作業物質。
（１７） 項（１４）に記載の希土類含有合金粉末の製造方法により得られた希土類含有合金粉末を、成形し、焼結することを特徴とする希土類含有合金焼結体の製造方法。
（１８） 前記焼結を１２００℃〜１４００℃の温度で行うことを特徴とする項（１７）に記載の希土類含有合金焼結体の製造方法。
（１９） 前記希土類含有合金粉末を焼結後、水素雰囲気中で２００℃〜３００℃の温度で保持し、焼結体に水素を吸蔵させることを特徴とする項（１７）または（１８）に記載の希土類含有合金焼結体の製造方法。
（２０） 項（１５）に記載の希土類含有合金粉末を、成形、焼結してなることを特徴する希土類含有合金焼結体。
（２１） 項（２０）の希土類含有合金焼結体に水素を吸蔵させてキュリー温度を制御したことを特徴とする磁歪材料。
（２２） 項（２０）の希土類含有合金焼結体に水素を吸蔵させてキュリー温度を制御したことを特徴とする磁気冷凍作業物質。
（２３） 項（８）から項（１０）又は項（１３）のいずれか１項に記載の希土類含有合金を用いた磁歪センサー。
（２４） 項（８）から項（１０）又は項（１３）のいずれか１項に記載の希土類含有合金を用いた磁歪振動子。 (16) A magnetic refrigeration working material, wherein the rare earth-containing alloy powder according to item (15) is occluded with hydrogen to control the Curie temperature.
(17) A method for producing a rare earth-containing alloy sintered body, wherein the rare earth-containing alloy powder obtained by the method for producing a rare earth-containing alloy powder according to item (14) is molded and sintered.
(18) The method for producing a rare earth-containing alloy sintered body according to item (17), wherein the sintering is performed at a temperature of 1200 ° C to 1400 ° C.
(19) In the item (17) or (18), the rare earth-containing alloy powder is sintered and then held in a hydrogen atmosphere at a temperature of 200 ° C. to 300 ° C., and the sintered body is made to occlude hydrogen. The manufacturing method of the rare earth containing alloy sintered compact of description.
(20) A rare earth-containing alloy sintered body obtained by molding and sintering the rare earth-containing alloy powder according to item (15).
(21) A magnetostrictive material, wherein the rare earth-containing alloy sintered body according to item (20) is occluded with hydrogen to control the Curie temperature.
(22) A magnetic refrigeration working material, characterized in that hydrogen is occluded in the rare earth-containing alloy sintered body according to item (20) to control the Curie temperature.
(23) A magnetostrictive sensor using the rare earth-containing alloy according to any one of items (8) to (10) or (13).
(24) A magnetostrictive vibrator using the rare earth-containing alloy according to any one of items (8) to (10) or (13).

以上詳述したように、本発明によれば、長時間の熱処理工程を必要とすることなく効率良くＮａＺｎ１３型ＲＥ−含有合金を製造することが可能な技術、および該技術により得られるＮａＺｎ１３型ＲＥ−含有合金、並びに該ＮａＺｎ１３型ＲＥ−含有合金を用いて得られる磁歪素子、磁歪材料、磁気冷凍作業物質、磁歪センサー、及び磁歪振動子を提供することができる。 As described above in detail, according to the present invention, a technique capable of efficiently producing a NaZn 13 type RE-containing alloy without requiring a long heat treatment step, and NaZn 13 obtained by the technique. A magnetoresistive element , a magnetostrictive material, a magnetic refrigeration material , a magnetostrictive sensor, and a magnetostrictive vibrator obtained using the type RE-containing alloy and the NaZn 13 type RE-containing alloy can be provided.

Claims (24)

一般式Ｒ（Ｔ１−ｘＡｘ）１３−ｙ（但し、ＲはＬａ、Ｃｅ、Ｐｒ、Ｎｄ、Ｓｍ、Ｅｕ、Ｔｂ、Ｄｙ、Ｈｏ、Ｔｍ、Ｙｂ、Ｇｄ及びＬｕから選択される少なくとも１種、ＴはＦｅ、Ｃｏ、Ｎｉ、Ｍｎ、Ｐｔ及びＰｄから選択される少なくとも１種、ＡはＡｌ、Ａｓ、Ｓｉ、Ｇａ、Ｇｅ、Ｍｎ、Ｓｎ及びＳｂから選択される少なくとも１種、０．０５≦ｘ≦０．２、−１≦ｙ≦１）で表される希土類含有合金の製造方法において、
合金原料を１２００〜１８００℃の温度で溶解する溶解工程と、該工程により得られた溶湯を急冷凝固し、希土類含有合金を生成する凝固工程とを有すると共に、
前記凝固工程における冷却速度を、少なくとも溶湯の温度から９００℃までの範囲内では１０２〜１０４℃／秒とすることを特徴とする希土類含有合金の製造方法。 Formula R (T 1-x A x ) 13-y ( provided that at least 1 R is the La, Ce, Pr, Nd, Sm, Eu, Tb, Dy, Ho, Tm, Yb, are selected from Gd and Lu Species, T is at least one selected from Fe, Co, Ni, Mn, Pt and Pd, A is at least one selected from Al, As, Si, Ga, Ge, Mn, Sn and Sb; In the method for producing a rare earth-containing alloy represented by 05 ≦ x ≦ 0.2 and −1 ≦ y ≦ 1)
A melting step of melting the alloy raw material at a temperature of 1200 to 1800 ° C., and a solidification step of rapidly solidifying the molten metal obtained by the step to generate a rare earth-containing alloy,
A method for producing a rare earth-containing alloy, wherein the cooling rate in the solidification step is 10 2 to 10 4 ° C / second at least in the range from the temperature of the molten metal to 900 ° C. 前記溶解工程において、合金原料を０．１〜０．２ＭＰａの圧力の不活性ガス雰囲気中で溶解することを特徴とする請求項１に記載の希土類含有合金の製造方法。   2. The method for producing a rare earth-containing alloy according to claim 1, wherein in the melting step, the alloy raw material is melted in an inert gas atmosphere having a pressure of 0.1 to 0.2 MPa. 前記凝固工程において、ストリップキャスト法、新遠心鋳造法、遠心鋳造法のうちいずれかの方法により、溶湯を急冷凝固することを特徴とする請求項１又は請求項２に記載の希土類含有合金の製造方法。   The rare earth-containing alloy according to claim 1 or 2, wherein in the solidification step, the molten metal is rapidly solidified by any one of a strip casting method, a new centrifugal casting method, and a centrifugal casting method. Method. 前記凝固工程において、ストリップキャスト法により溶湯を急冷凝固すると共に、該工程後に得られる薄片の厚さを０．１〜２．０ｍｍとすることを特徴とする請求項３に記載の希土類含有合金の製造方法。   4. The rare earth-containing alloy according to claim 3, wherein in the solidification step, the molten metal is rapidly solidified by a strip casting method, and the thickness of the flakes obtained after the step is 0.1 to 2.0 mm. Production method. 前記凝固工程により得られた希土類含有合金を、９００〜１２００℃の温度で熱処理し、ＮａＺｎ１３相を生成させる熱処理工程をさらに有することを特徴とする請求項１から請求項４までのいずれか１項に記載の希土類含有合金の製造方法。 5. The method according to claim 1, further comprising a heat treatment step of heat-treating the rare earth-containing alloy obtained by the solidification step at a temperature of 900 to 1200 ° C. to generate a NaZn 13 phase. A method for producing the rare earth-containing alloy according to item. 前記熱処理工程において、熱処理時間を１分〜２００時間とすることを特徴とする請求項５に記載の希土類含有合金の製造方法。   6. The method for producing a rare earth-containing alloy according to claim 5, wherein the heat treatment time is 1 minute to 200 hours. 前記熱処理工程において、熱処理温度を１０８０℃〜１２００℃とし、熱処理時間を３〜４２時間とする請求項６に記載の希土類含有合金の製造方法。   7. The method for producing a rare earth-containing alloy according to claim 6, wherein in the heat treatment step, a heat treatment temperature is 1080 ° C. to 1200 ° C. and a heat treatment time is 3 to 42 hours. 請求項１から請求項４までのいずれか１項に記載の希土類含有合金の製造方法により製造されたことを特徴とする希土類含有合金。   A rare earth-containing alloy produced by the method for producing a rare earth-containing alloy according to any one of claims 1 to 4. 一般式Ｒ（Ｔ１−ｘＡｘ）１３−ｙ（但し、ＲはＬａ、Ｃｅ、Ｐｒ、Ｎｄ、Ｓｍ、Ｅｕ、Ｔｂ、Ｄｙ、Ｈｏ、Ｔｍ、Ｙｂ、Ｇｄ及びＬｕから選択される少なくとも１種、ＴはＦｅ、Ｃｏ、Ｎｉ、Ｍｎ、Ｐｔ及びＰｄから選択される少なくとも１種、ＡはＡｌ、Ａｓ、Ｓｉ、Ｇａ、Ｇｅ、Ｍｎ、Ｓｎ及びＳｂから選択される少なくとも１種、０．０５≦ｘ≦０．２、−１≦ｙ≦１）で表される希土類含有合金において、
希土類金属Ｒの含有量が相対的に多いＲ−ｒｉｃｈ相と、希土類金属Ｒの含有量が相対的に少ないＲ−ｐｏｏｒ相とが、０．０１〜１００μｍの間隔で分散していることを特徴とする希土類含有合金。 Formula R (T 1-x A x ) 13-y ( provided that at least 1 R is the La, Ce, Pr, Nd, Sm, Eu, Tb, Dy, Ho, Tm, Yb, are selected from Gd and Lu Species, T is at least one selected from Fe, Co, Ni, Mn, Pt and Pd, A is at least one selected from Al, As, Si, Ga, Ge, Mn, Sn and Sb; In the rare earth-containing alloy represented by 05 ≦ x ≦ 0.2 and −1 ≦ y ≦ 1)
The R-rich phase having a relatively high content of rare earth metal R and the R-poor phase having a relatively low content of rare earth metal R are dispersed at an interval of 0.01 to 100 μm. A rare earth-containing alloy. 一般式Ｒ（Ｔ１−ｘＡｘ）１３−ｙ（但し、ＲはＬａ、Ｃｅ、Ｐｒ、Ｎｄ、Ｓｍ、Ｅｕ、Ｔｂ、Ｄｙ、Ｈｏ、Ｔｍ、Ｙｂ、Ｇｄ及びＬｕから選択される少なくとも１種、ＴはＦｅ、Ｃｏ、Ｎｉ、Ｍｎ、Ｐｔ及びＰｄから選択される少なくとも１種、ＡはＡｌ、Ａｓ、Ｓｉ、Ｇａ、Ｇｅ、Ｍｎ、Ｓｎ及びＳｂから選択される少なくとも１種、０．０５≦ｘ≦０．２、−１≦ｙ≦１）で表される希土類含有合金において、
ＮａＺｎ１３相の存在比率が９０ｖｏｌ％以上であることを特徴とする希土類含有合金。 Formula R (T 1-x A x ) 13-y ( provided that at least 1 R is the La, Ce, Pr, Nd, Sm, Eu, Tb, Dy, Ho, Tm, Yb, are selected from Gd and Lu Species, T is at least one selected from Fe, Co, Ni, Mn, Pt and Pd, A is at least one selected from Al, As, Si, Ga, Ge, Mn, Sn and Sb; In the rare earth-containing alloy represented by 05 ≦ x ≦ 0.2 and −1 ≦ y ≦ 1)
A rare earth-containing alloy characterized in that the abundance ratio of NaZn 13 phase is 90 vol% or more. 請求項８から請求項１０までのいずれか１項に記載の希土類含有合金を用いて製造されたことを特徴とする磁歪素子。 A magnetostrictive element manufactured using the rare earth-containing alloy according to any one of claims 8 to 10. 請求項８から請求項１０までのいずれか１項に記載の希土類含有合金を用いて製造されたことを特徴とする磁気冷凍作業物質。 A magnetic refrigeration working material manufactured using the rare earth-containing alloy according to any one of claims 8 to 10. ＲｒＴｔＡａ（但し、ＲはＬａ、Ｃｅ、Ｐｒ、Ｎｄ、Ｓｍ、Ｅｕ、Ｔｂ、Ｄｙ、Ｈｏ、Ｔｍ、Ｙｂ、Ｇｄ及びＬｕのうちから選択される少なくとも一種の希土類元素、ＴはＦｅを必須とし、任意にその一部がＣｏ、Ｎｉ、Ｍｎ、Ｐｔ及びＰｄのうちから選択される少なくとも一種の元素で置換されている遷移金属元素、ＡはＡｌ、Ａｓ、Ｓｉ、Ｇａ、Ｇｅ、Ｍｎ、Ｓｎ及びＳｂのうちから選択される少なくとも一種の元素であり、組成比を示すｒ、ｔ、ａは５．０原子％≦ｒ≦６．８原子％、７３．８原子％≦ｔ≦８８．７原子％、４．６原子％≦ａ≦１９．４原子％である。）なる組成式で示される合金であって、該合金は組織中に８５質量％以上のＮａＺｎ１３型の結晶構造と５質量％以上１５質量％以下のα−Ｆｅとを含有してなる希土類含有合金。 R r T t A a (where R is La, Ce, Pr, Nd, Sm, Eu, Tb, Dy, Ho, Tm, Yb, Gd, and Lu, and T is A transition metal element in which Fe is essential and a part thereof is optionally substituted with at least one element selected from Co, Ni, Mn, Pt and Pd, A is Al, As, Si, Ga, Ge , Mn, Sn and Sb are at least one element selected from the group consisting of r, t, and a indicating a composition ratio of 5.0 atomic% ≦ r ≦ 6.8 atomic%, 73.8 atomic% ≦ t ≦ 88.7 atomic%, 4.6 atomic% ≦ a ≦ 19.4 atomic%)), which is an alloy of NaZn 13 type with 85 mass% or more in the structure. Containing 5% by mass to 15% by mass of α-Fe with a crystal structure. The rare earth-containing alloy. 請求項１３に記載の希土類合金を機械的手段によって平均粒径０．１μｍ〜１．０ｍｍの粉末に粉砕することを特徴とする希土類含有合金粉末の製造方法。   A method for producing a rare earth-containing alloy powder, wherein the rare earth alloy according to claim 13 is pulverized into a powder having an average particle size of 0.1 μm to 1.0 mm by mechanical means. 請求項１３に記載の希土類含有合金からなり、平均粒径０．１〜１．０ｍｍであることを特徴とする希土類合金粉末。   A rare earth alloy powder comprising the rare earth-containing alloy according to claim 13 and having an average particle size of 0.1 to 1.0 mm. 請求項１５に記載の希土類含有合金粉末に水素を吸蔵させてキュリー温度を制御してなることを特徴とする磁気冷凍作業物質。   A magnetic refrigeration working material obtained by storing hydrogen in the rare earth-containing alloy powder according to claim 15 and controlling a Curie temperature. 請求項１４に記載の希土類含有合金粉末の製造方法により得られた希土類含有合金粉末を、成形し、焼結することを特徴とする希土類含有合金焼結体の製造方法。   A method for producing a rare earth-containing alloy sintered body, wherein the rare earth-containing alloy powder obtained by the method for producing a rare earth-containing alloy powder according to claim 14 is molded and sintered. 前記焼結を１２００℃〜１４００℃の温度で行うことを特徴とする請求項１７に記載の希土類含有合金焼結体の製造方法。   The method for producing a rare earth-containing alloy sintered body according to claim 17, wherein the sintering is performed at a temperature of 1200 ° C to 1400 ° C. 前記希土類含有合金粉末を焼結後、水素雰囲気中で２００℃〜３００℃の温度で保持し、焼結体に水素を吸蔵させることを特徴とする請求項１７または１８に記載の希土類含有合金焼結体の製造方法。   The rare earth-containing alloy powder according to claim 17 or 18, wherein after sintering the rare earth-containing alloy powder, the sintered body is held at a temperature of 200 ° C to 300 ° C, and hydrogen is occluded in the sintered body. A method for producing a knot. 請求項１５に記載の希土類含有合金粉末を、成形、焼結してなることを特徴する希土類含有合金焼結体。   A rare earth-containing alloy sintered body obtained by molding and sintering the rare earth-containing alloy powder according to claim 15. 請求項２０の希土類含有合金焼結体に水素を吸蔵させてキュリー温度を制御したことを特徴とする磁歪材料。   A magnetostrictive material, wherein the rare earth-containing alloy sintered body according to claim 20 stores hydrogen and controls the Curie temperature. 請求項２０の希土類含有合金焼結体に水素を吸蔵させてキュリー温度を制御したことを特徴とする磁気冷凍作業物質。   21. A magnetic refrigeration working material, wherein the rare earth-containing alloy sintered body of claim 20 stores hydrogen and controls the Curie temperature. 請求項８から請求項１０又は請求項１３のいずれか１項に記載の希土類含有合金を用いた磁歪センサー。A magnetostrictive sensor using the rare earth-containing alloy according to any one of claims 8 to 10 or claim 13. 請求項８から請求項１０又は請求項１３のいずれか１項に記載の希土類含有合金を用いた磁歪振動子。A magnetostrictive vibrator using the rare earth-containing alloy according to any one of claims 8 to 10 or claim 13.
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