JP2018041873A - Method for producing L10 type FeNi ordered alloy - Google Patents
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本発明は、第三元素添加法によるＬ１０型ＦｅＮｉ規則合金の製造方法に関する。 The present invention relates to a process for the production of L1 0 type FeNi ordered alloy according to the third element addition method.
近年、大きい一軸磁気異方性を有し、貴金属やレアアースを含まない材料として、Ｌ１０型の結晶構造を有するＦｅＮｉ規則合金が注目されている。このＬ１０型ＦｅＮｉ規則合金を製造する方法として、従来、ＭｇＯ単結晶基板の（００１）面上に複雑な組成を有する多層膜を形成し、その多層膜の上に、Ｆｅ単原子層とＮｉ単原子層とを繰り返し積層する方法（例えば、非特許文献１参照）や、鉄とニッケルとを含有する前駆体粒子を、水素雰囲気下で加熱して還元し、合金粒子の構造をＬ１０型に規則化する方法（例えば、特許文献１参照）がある。また、不活性ガス雰囲気中で、回転するＭｇＯ基板にＦｅとＮｉとを同時にスパッタしてＦｅＮｉ合金薄膜を製造し、規則不規則変態温度近傍で熱処理する方法（例えば、特許文献２参照）もある。 Recently, a large uniaxial magnetic anisotropy, as a material that does not contain precious metals and rare earths, FeNi ordered alloy having an L1 0 type crystal structure has been attracting attention. As a method of manufacturing the L1 0 type FeNi ordered alloy, conventionally, a multilayer film having a complex composition on the (001) plane of MgO single crystal substrate, on top of the multilayer film, Fe monoatomic layer and Ni method for laminating repeatedly the monolayer (e.g., see non-Patent Document 1) and, the precursor particles containing iron and nickel, was reduced by heating in a hydrogen atmosphere, the structure of L1 0 type of the alloy particles There is a method of regularization (see, for example, Patent Document 1). In addition, there is a method in which Fe and Ni are simultaneously sputtered on a rotating MgO substrate in an inert gas atmosphere to produce a FeNi alloy thin film and heat-treated near the regular irregular transformation temperature (see, for example, Patent Document 2). .
しかしながら、非特許文献１に記載の方法は、特殊な装置を必要とし、製造工程が複雑であるという課題があった。また、特許文献１に記載の方法では、Ｌ１０型ＦｅＮｉ合金の粒子を製造することはできるが、より体積の大きい物質として製造することはできない。このため、例えば、薄膜を製造する場合には、水素雰囲気下で、粒子から薄膜を製造する工程が必要となり、煩雑であるという課題があった。また、特許文献２に記載の方法では、薄膜状のＬ１０型ＦｅＮｉ合金を比較的簡便な方法で体積の大きい物質として製造することはできるが、規則相を製造するための温度が４００℃未満に限られていた。 However, the method described in Non-Patent Document 1 has a problem that a special apparatus is required and the manufacturing process is complicated. Further, in the method described in Patent Document 1, although it is possible to produce particles of L1 0 type FeNi alloy, it can not be manufactured as a more volume of large material. For this reason, for example, when manufacturing a thin film, the process which manufactures a thin film from particle | grains in a hydrogen atmosphere is needed, and there existed a subject that it was complicated. Further, in the method described in Patent Document 2, although it is possible to manufacture a thin-film L1 0 type FeNi alloy as the volume of large material in a relatively simple method, the temperature for the production of ordered phase is less than 400 ° C. It was limited to.
本発明は、このような課題に着目してなされたもので、比較的簡便な方法で薄膜状のＬ１０型ＦｅＮｉ規則合金を製造することができる、Ｌ１０型ＦｅＮｉ規則合金の製造方法を提供することを目的とする。 The present invention has been made in view of such problems, it is possible to manufacture a thin-film L1 0 type FeNi ordered alloy in a relatively simple method, a manufacturing method of the L1 0 type FeNi ordered alloy The purpose is to do.
上記目的を達成するために、本発明に係るＬ１０型ＦｅＮｉ規則合金の製造方法は、真空雰囲気中または不活性ガス雰囲気中で、ＦｅＮｉに遷移金属元素を添加した合金薄膜を所定の温度まで加熱した後、前記所定の温度で所定の時間保持する加熱工程を有することを特徴とする。 To achieve the above object, a manufacturing method of the L1 0 type FeNi ordered alloy according to the present invention, in a vacuum atmosphere or an inert gas atmosphere, heating the alloy film obtained by adding a transition metal element in FeNi to a predetermined temperature Then, the method has a heating step of holding at the predetermined temperature for a predetermined time.
本発明に係るＬ１０型ＦｅＮｉ規則合金の製造方法は、FeNiの合金薄膜の作製時に、同時にTi、V、Cr、Mn、Co、Cu、Znなどの第一遷移金属元素を第三元素として０％より多く、２０％以下の原子濃度で添加することが好ましい。 Manufacturing method of L1 0 type FeNi ordered alloy according to the present invention, during the production of the alloy thin film of FeNi, simultaneously Ti, V, Cr, Mn, Co, Cu, a first transition metallic element such as Zn as the third element 0 It is preferable to add at an atomic concentration of more than 20% and 20% or less.
本発明に係るＬ１０型ＦｅＮｉ規則合金の製造方法は、前記ＦｅＮｉ合金薄膜を０．１℃／秒以上の昇温速度で加熱することが好ましい。昇温速度は、５０℃／秒以上であることが特に好ましい。 Manufacturing method of L1 0 type FeNi ordered alloy according to the present invention, it is preferable to heat the FeNi alloy thin film at 0.1 ° C. / sec or more Atsushi Nobori rate. The heating rate is particularly preferably 50 ° C./second or more.
本発明に係るＬ１０型ＦｅＮｉ規則合金の製造方法は、ＦｅＮｉ合金薄膜を急速昇温加熱することにより、結晶構造をＬ１０型にすることができ、大きい一軸磁気異方性などの優れた磁気特性を有するＬ１０型ＦｅＮｉ規則合金を製造することができる。ＦｅＮｉ合金薄膜を急速昇温加熱するだけの比較的簡便な方法で、薄膜状のＬ１０型ＦｅＮｉ規則合金を製造することができる。急速昇温加熱は、例えば、ランプ加熱により行うことができる。また、ＦｅＮｉ合金薄膜の膜厚は、５ｎｍ以上、１００ｎｍ以下であることが好ましい。 Manufacturing method of L1 0 type FeNi ordered alloy according to the present invention, by rapid thermal heating of the FeNi alloy thin film, the crystal structure can be L1 0 type, such as a large uniaxial magnetic anisotropy excellent magnetic it is possible to manufacture an L1 0 type FeNi ordered alloy having characteristics. The FeNi alloy thin film with a relatively simple method that only rapid thermal annealing, it is possible to manufacture a thin-film L1 0 type FeNi ordered alloy. The rapid heating and heating can be performed by, for example, lamp heating. The thickness of the FeNi alloy thin film is preferably 5 nm or more and 100 nm or less.
本発明に係るＬ１０型ＦｅＮｉ規則合金の製造方法で、前記所定の温度は３１０℃以上、５００℃未満であることが好ましい。この場合、特に優れた磁気特性を有するＬ１０型ＦｅＮｉ規則合金を得ることができる。所定の温度は４５０℃程度が特に好ましい。所定の温度が５００℃以上では、Ｌ１０型ＦｅＮｉ規則合金が安定して存在できなくなる。また、所定の温度が３１０℃未満では、結晶構造がＬ１０型にならない。 In the production method of the L1 0 type FeNi ordered alloy according to the present invention, the predetermined temperature is 310 ° C. or more and less than 500 ° C.. In this case, it is possible to obtain a particularly excellent L1 0 type FeNi ordered alloy with magnetic properties. The predetermined temperature is particularly preferably about 450 ° C. The predetermined temperature is 500 ° C. or higher, L1 0 type FeNi ordered alloy can not be present stably. Further, it is less than a predetermined temperature is 310 ° C., the crystal structure does not become L1 0 type.
本発明に係るＬ１０型ＦｅＮｉ規則合金の製造方法は、前記加熱工程の前に、不活性ガス雰囲気中で、回転する基板の表面にＦｅとＮｉと第三元素とを同時にスパッタして前記ＦｅＮｉ合金薄膜を得る薄膜製造工程を有していてもよい。この場合、原料のＦｅとＮｉとから、容易にＦｅＮｉ合金薄膜を得ることができる。薄膜製造工程も加熱工程も、既存の技術を応用して実施することができ、比較的簡便な方法で、薄膜状のＬ１０型ＦｅＮｉ規則合金を製造することができる。なお、ＦｅのスパッタとＮｉのスパッタと第三元素のスパッタとを同時に行ってもよいが、ＦｅＮｉ合金と第三元素をスパッタ、あるいはＦｅＮｉおよび第三元素の合金をスパッタしてもよい。また、Ｆｅと第三元素を同時にスパッタし、Ｎｉと交互に作製する方法でもよく、これが最も好ましい。 Manufacturing method of L1 0 type FeNi ordered alloy according to the present invention, the prior heating step, in an inert gas atmosphere, the surface of the rotating substrate by simultaneously sputtering Fe and Ni and a third element said FeNi You may have the thin film manufacturing process which obtains an alloy thin film. In this case, an FeNi alloy thin film can be easily obtained from the raw materials Fe and Ni. Thin film manufacturing process heating step also can be carried out by applying the existing technology, a relatively simple method, it is possible to manufacture a thin-film L1 0 type FeNi ordered alloy. Note that Fe sputtering, Ni sputtering, and third element sputtering may be performed simultaneously, but FeNi alloy and third element may be sputtered, or FeNi and third element alloy may be sputtered. Alternatively, a method of sputtering Fe and a third element at the same time and alternately producing Ni may be used, and this is most preferable.
この場合、前記基板は、単結晶基板、多結晶基板またはアモルファス基板であることが好ましい。特に、前記基板はＭｇＯ単結晶基板から成り、前記基板の表面が（００１）面であることが好ましい。この場合、特に効率良く、Ｌ１０型ＦｅＮｉ規則合金を製造することができる。 In this case, the substrate is preferably a single crystal substrate, a polycrystalline substrate, or an amorphous substrate. In particular, the substrate is preferably composed of a MgO single crystal substrate, and the surface of the substrate is preferably a (001) plane. In this case, particularly efficient, it is possible to produce the L1 0 type FeNi ordered alloy.
本発明によれば、比較的簡便な方法で薄膜状のＬ１０型ＦｅＮｉ規則合金を製造することができる、Ｌ１０型ＦｅＮｉ規則合金の製造方法を提供することができる。 According to the present invention, it is possible to manufacture a thin-film L1 0 type FeNi ordered alloy in a relatively simple method, it is possible to provide a manufacturing method of the L1 0 type FeNi ordered alloy.
以下、図面に基づき、本発明の実施の形態について説明する。
図１（ａ）に示すように、本発明の実施の形態のＬ１０型ＦｅＮｉ規則合金の製造方法では、まず、不活性ガス雰囲気中で、回転台１１に設置された基板１の表面に、基板１を回転させながら、ＦｅとＮｉと第三元素とを同時にスパッタしてＦｅＮｉ合金薄膜を製造する。また、Ｆｅと第三元素とを同時にスパッタし、Ｎｉと交互に作製する方法でもよく、これが最も好ましい。なお、具体的な一例では、基板１は、表面が（００１）面のＭｇＯ単結晶基板から成っているが、他の単結晶基板や多結晶基板、アモルファス基板から成っていてもよい。
Hereinafter, embodiments of the present invention will be described with reference to the drawings.
As shown in FIG. 1 (a), in the manufacturing method of the L1 0 type FeNi ordered alloy embodiment of the present invention, first, in an inert gas atmosphere, to the installation surface of the substrate 1 to the turntable 11, While rotating the substrate 1, Fe, Ni, and a third element are sputtered simultaneously to produce a FeNi alloy thin film. Further, a method of simultaneously sputtering Fe and a third element and alternately producing Ni may be used, and this is most preferable. In a specific example, the substrate 1 is made of an MgO single crystal substrate having a (001) surface, but may be made of another single crystal substrate, a polycrystalline substrate, or an amorphous substrate.
ＦｅＮｉ合金薄膜を製造した後、図１（ｂ）に示すように、ＦｅＮｉ合金薄膜が載った基板１を、内面１２ａが回転楕円体形状を成す金製の鏡から成る加熱容器１２の下部に設置し、加熱容器１２の頂部に設置された赤外線ランプ１３により、加熱容器１２の内面１２ａからの近赤外線の反射も利用して、ＦｅＮｉ合金薄膜を急速昇温加熱する。このとき、真空雰囲気中または不活性ガス雰囲気中で行い、３１０℃以上５００℃未満の温度まで、０．１℃／秒以上の昇温速度で急速昇温加熱する。また、熱が逃げないよう、基板１の表面を透明な水晶板１４で覆うとともに、基板１の温度を熱電対１５で測定しながら温度を調整する。急速昇温加熱の後、到達した温度で２時間以上保持する。こうして、Ｌ１０型ＦｅＮｉ規則合金を製造することができる。 After the FeNi alloy thin film is manufactured, as shown in FIG. 1B, the substrate 1 on which the FeNi alloy thin film is placed is placed below the heating container 12 made of a gold mirror having an inner surface 12a having a spheroid shape. Then, the FeNi alloy thin film is rapidly heated by the infrared lamp 13 installed at the top of the heating container 12 using the reflection of near infrared rays from the inner surface 12a of the heating container 12. At this time, it is performed in a vacuum atmosphere or an inert gas atmosphere, and is rapidly heated to a temperature of 310 ° C. or higher and lower than 500 ° C. at a temperature rising rate of 0.1 ° C./second or higher. Further, the surface of the substrate 1 is covered with a transparent quartz plate 14 so that heat does not escape, and the temperature is adjusted while measuring the temperature of the substrate 1 with a thermocouple 15. After rapid heating and heating, hold at the reached temperature for 2 hours or more. Thus, it is possible to produce the L1 0 type FeNi ordered alloy.
このように、本発明の実施の形態のＬ１０型ＦｅＮｉ規則合金の製造方法は、ＦｅＮｉ合金薄膜を昇温加熱することにより、結晶構造をＬ１０型にすることができ、大きい一軸磁気異方性などの優れた磁気特性を有するＬ１０型ＦｅＮｉ規則合金を製造することができる。スパッタによりＦｅＮｉ合金薄膜を製造し、そのＦｅＮｉ合金薄膜を急速昇温加熱するという、既存の技術を応用した比較的簡便な方法で、薄膜状のＬ１０型ＦｅＮｉ規則合金を容易に製造することができる。製造されたＬ１０型ＦｅＮｉ規則合金は、レアアースを使用したネオジム磁石等の磁石に代わるものとして期待できる。 Thus, the production method of the L1 0 type FeNi ordered alloy embodiment of the present invention, by increasing the temperature heating the FeNi alloy thin film, the crystal structure can be L1 0 type, a large uniaxial magnetic anisotropy it is possible to manufacture an L1 0 type FeNi ordered alloy having excellent magnetic characteristics such as gender. By sputtering to produce a FeNi alloy thin film, the FeNi alloy thin film that rapid thermal annealing, a relatively simple method of applying existing technology, is possible to easily produce a thin-film L1 0 type FeNi ordered alloy it can. L1 0 type FeNi rules prepared alloy can be expected as an alternative to magnet neodymium magnet or the like using rare earth.
本発明の実施の形態のＬ１０型ＦｅＮｉ規則合金の製造方法により、ＦｅＮｉ合金を製造し、各種の試験を行った。ＦｅＮｉ合金を製造では、ＦｅとＮｉと第三元素のＴｉとのスパッタを、マグネトロンスパッタリングにより、０．２Ｐａのアルゴンガス雰囲気中で、室温で行った。Ｆｅと第三元素とを同時にスパッタし、Ｎｉと交互に作製した。Ｆｅ−Ｔｉ層およびＮｉ層の膜厚は、どちらも０．３ｎｍである。基板１は、表面が（００１）面のＭｇＯ単結晶基板から成り、縦横がそれぞれ１ｃｍ、厚みが０．５ｍｍとした。急速昇温加熱を、５×１０−４Ｐａ以下の真空雰囲気中で行い、昇温速度は０．１７℃／秒および５０℃／秒とした。 The manufacturing method of L1 0 type FeNi ordered alloy embodiment of the present invention, to produce a FeNi alloy was subjected to various tests. In producing the FeNi alloy, sputtering of Fe, Ni, and the third element Ti was performed at room temperature in an argon gas atmosphere of 0.2 Pa by magnetron sputtering. Fe and a third element were simultaneously sputtered and alternately formed with Ni. The film thicknesses of the Fe—Ti layer and the Ni layer are both 0.3 nm. The substrate 1 was composed of a MgO single crystal substrate having a (001) surface, and the length and width were 1 cm and the thickness was 0.5 mm, respectively. Rapid temperature increase heating was performed in a vacuum atmosphere of 5 × 10 −4 Pa or less, and the temperature increase rate was 0.17 ° C./second and 50 ° C./second.
試験用の試料として、急速昇温加熱の到達温度での保持時間を１時間、到達温度を３００℃、３５０℃、４００℃、４５０℃、および５００℃としたもの、到達温度を４００℃、保持時間を１秒としたものを製造した。また、比較のために、熱処理前のＦｅＮｉ合金薄膜の試料（ａｓ−ｄｅｐｏ．または、ａｓ−ｄｅｐｏｓｉｔｅｄ）も使用した。なお、得られたＦｅＮｉ合金は、厚さが約１５ｎｍである。 As a test sample, the holding time at the ultimate temperature of the rapid heating and heating is 1 hour, the ultimate temperature is 300 ° C., 350 ° C., 400 ° C., 450 ° C., and 500 ° C., and the ultimate temperature is 400 ° C. A product with a time of 1 second was produced. For comparison, a FeNi alloy thin film sample (as-depo. Or as-deposited) before heat treatment was also used. The obtained FeNi alloy has a thickness of about 15 nm.
まず、Ｘ線回折（ＸＲＤ）により、Ｉｎ−Ｐｌａｎｅ測定を行い、その結果を図２に示す。測定には、保持時間が１時間の異なる到達温度の試料を用いた。図２（ａ）に示すように、全ての試料において、ＦｅＮｉ（２２０）ピークが確認され、ＦｅＮｉが結晶配向していることが確認された。また、到達温度が３５０℃、４００℃および４５０℃の試料の、ＦｅＮｉ（１１０）ピークが大きく、Ｌ１０型ＦｅＮｉの規則化が促進されていることが確認された。 First, In-Plane measurement was performed by X-ray diffraction (XRD), and the results are shown in FIG. For the measurement, samples having different holding temperatures with holding times of 1 hour were used. As shown to Fig.2 (a), in all the samples, the FeNi (220) peak was confirmed and it was confirmed that FeNi has crystal orientation. Further, the reaching temperature of 350 ° C., 400 ° C. and 450 ° C. sample, FeNi (110) peak is large, it was confirmed that L1 0 type FeNi regularization is promoted.
図２（ｂ）に示すように、Ｔｉを添加しない試料と比較して、Ｔｉを１．６％添加した試料では、規則度（Order parameter）のピークが３５０℃〜４５０℃付近にある。これは、この温度で加熱を行うことにより、Ｌ１０型ＦｅＮｉの規則化が進むことを表しており、Ｔｉを添加することにより、より高い温度で熱処理ができることが分かった。一般に、高い温度での熱処理はより原子移動を促進する効果があり、規則度を、向上させることができる。また、到達温度を４００℃、保持時間を１秒としたものについて、ＸＲＤのＩｎ−Ｐｌａｎｅ測定を行った結果、ＦｅＮｉ（１１０）ピークがより大きく確認され、規則度は０．３程度であることが分かった。これは、Ｔｉを添加しない場合の値を大きく超える値である。 As shown in FIG. 2 (b), the order parameter peak is in the vicinity of 350 ° C. to 450 ° C. in the sample added with 1.6% Ti as compared to the sample without added Ti. This is by heating at this temperature, and indicates that the L1 0 type FeNi regularization progresses, by the addition of Ti, it was found that it is heat-treated at higher temperatures. In general, heat treatment at a high temperature has an effect of promoting atom migration, and can improve the degree of order. In addition, as a result of XRD In-Plane measurement with an arrival temperature of 400 ° C. and a holding time of 1 second, a larger FeNi (110) peak was confirmed, and the degree of ordering was about 0.3. I understood. This is a value that greatly exceeds the value when Ti is not added.
図３に、第一原理計算法により、Ｌ１０型ＦｅＮｉ規則合金およびＡ１型ＦｅＮｉ不規則合金の生成エネルギーの差分（L10 to A1 energy difference）を計算した結果を示す。５％の第三元素がＦｅあるいはＮｉを置換した時の例を示す。ＴｉやＶ、Ｇａ、Ａｌ、Ｓｉ、Ｇｅなどの遷移金属がＦｅ層を置換したときに、エネルギー差が大きくなり、Ｌ１０型ＦｅＮｉの規則化がおきやすいことを示している。この結果は、上記の実施例に一致していると考えられる。 3, the first-principles calculation method, shows the results of calculating the L1 0 type FeNi ordered alloy and type A1 FeNi generation energy disordered alloy difference (L1 0 to A1 energy difference) . An example when 5% of the third element replaces Fe or Ni is shown. Ti and V, Ga, Al, Si, when the transition metals such as Ge is substituted with Fe layer, the energy difference becomes large, indicating that easily place the ordering of the L1 0 type FeNi. This result is considered to be consistent with the above example.
１ 基板
１１ 回転台
１２ 加熱容器
１２ａ 内面
１３ 赤外線ランプ
１４ 水晶板
１５ 熱電対
DESCRIPTION OF SYMBOLS 1 Board | substrate 11 Turntable 12 Heating container 12a Inner surface 13 Infrared lamp 14 Crystal plate 15 Thermocouple
Claims (6)
The substrate consists of MgO single crystal substrate, a manufacturing method of claim 4 L1 0 type FeNi ordered alloy, wherein a surface of the substrate is a (001) plane.
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