JP2006118040A - Method for producing nanocrystal magnetic material with oriented crystal grain - Google Patents
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本発明は、高周波トランス磁心や磁気ヘッド等に用いるナノ結晶軟磁性材料の製造方法に関し、更に詳細にはナノサイズの結晶粒の方位が配向したナノ結晶磁性材料薄膜の製造方法に関するものである。 The present invention relates to a method for producing a nanocrystalline soft magnetic material used for a high-frequency transformer magnetic core, a magnetic head or the like, and more particularly to a method for producing a nanocrystalline magnetic material thin film in which the orientation of nanosized crystal grains is oriented.
従来の結晶粒径を有する多結晶材料に比べ、結晶粒径をナノスケール化することにより優れた磁気特性や力学特性が発現することが一般的に知られている。このようなナノ結晶材料の作製方法としては、ガス急冷・固化法、電着法、強加工法、急冷凝固法、アモルファス合金を前駆体とする結晶化法などが用いられており、特にナノ結晶軟磁性材料の製造方法では、アモルファス金属合金の結晶化法が主に用いられている。（例えば、特許文献１，２，３ 非特許文献１参照）また、このようなナノ結晶材料の作製技術についても、詳しい解説記事がある。（例えば、非特許文献２参照）
一方、Ｆｅ−Ｓｉ合金のいわゆる電磁鋼板の研究例からもわかるように、結晶粒方位を配向し、集合組織を形成させることにより、飛躍的に軟磁気特性が向上する。したがって、ナノ結晶軟磁性材料の結晶粒方位を配向することによって、磁気特性のさらなる向上が期待される。しかしながら、このような着想に基づいて、アモルファス合金からのナノ結晶化法において結晶粒方位の配向を試みた研究はほとんど無い。
It is generally known that superior magnetic properties and mechanical properties are manifested by making the crystal grain size nanoscale compared to conventional polycrystalline materials having a crystal grain size. As a method for producing such a nanocrystal material, a gas rapid cooling / solidification method, an electrodeposition method, a strong processing method, a rapid solidification method, a crystallization method using an amorphous alloy as a precursor, and the like are used. In the method for producing a soft magnetic material, an amorphous metal alloy crystallization method is mainly used. (For example, refer to Patent Documents 1, 2 and 3 Non-Patent Document 1) Further, there is a detailed explanation article about the technology for producing such a nanocrystal material. (For example, see Non-Patent Document 2)
On the other hand, as can be seen from research examples of so-called electromagnetic steel sheets made of Fe—Si alloy, the soft magnetic properties are dramatically improved by orienting the crystal grains and forming a texture. Therefore, further improvement in magnetic properties is expected by orienting the crystal grain orientation of the nanocrystalline soft magnetic material. However, based on such an idea, there has been almost no research that attempted the orientation of crystal grain orientation in the nanocrystallization method from an amorphous alloy.
また、アモルファス軟磁性体のキュリー温度をＴｃａ、アモルファス軟磁性体を加熱して結晶相とした時、該結晶相の結晶化温度をＴＣ、さらに、前記結晶相のキュリー温度をＴｃxとすると、一般的に、Ｔｃａ＜ＴＣ＜Ｔｃｃの関係にあることが知られている。（例えば、非特許文献３参照）
前述の先行文献における、従来のアモルファス合金の結晶化技術では、結晶粒方位の配向が全く行われていない。また従来技術のように、結晶化温度以上での熱処理のみによるナノ結晶化では、結晶粒方位の配向は難しいと考えられる。そこで、本発明は、熱処理による結晶化の際に外部磁場を印加することにより、磁場作用によって結晶粒方位を配向させた集合組織をもち、磁気特性が向上した超微細結晶粒材料薄膜およびナノ結晶材料薄膜の製造方法を提供することを目的としている。 In the conventional amorphous alloy crystallization technique in the above-mentioned prior literature, the orientation of crystal grain orientation is not performed at all. In addition, as in the prior art, it is considered that the orientation of the crystal grain orientation is difficult by nanocrystallization only by heat treatment above the crystallization temperature. Therefore, the present invention provides an ultrafine-grain material thin film and a nanocrystal having an improved magnetic property, having a texture in which grain orientation is oriented by magnetic field action by applying an external magnetic field during crystallization by heat treatment. It aims at providing the manufacturing method of a material thin film.
本発明によれば、アモルファス軟磁性体薄板を加熱して結晶化する工程において、前記アモルファス軟磁性体を加熱し結晶相とした時の該結晶相の晶出温度をＴＣ、さらに、前記結晶相のキュリー温度をＴｃｃとすると、強直流磁場中で、ＴＣ以上でＴｃｃ以下の温度に前記アモルファス軟磁性体薄板を加熱した後結晶化することを特徴とする結晶粒方位配向ナノ結晶磁性材料薄板の製造方法が得られる。 According to the present invention, in the step of heating and crystallizing the amorphous soft magnetic thin plate, the crystallization temperature of the crystalline phase when the amorphous soft magnetic body is heated to be a crystalline phase is set to TC, and further the crystalline phase A crystal grain orientation-oriented nanocrystalline magnetic material sheet characterized in that the amorphous soft magnetic thin film is crystallized after heating the amorphous soft magnetic thin film to a temperature not lower than TC and not higher than Tcc in a strong DC magnetic field. A manufacturing method is obtained.
また、本発明によれば、前記アモルファス軟磁性体は、Ｆｅ−Ｓｉ−Ｂからなる合金であることを特徴とする結晶粒方位配向超微細結晶粒磁性材料薄板の製造方法が得られる。 Further, according to the present invention, there is obtained a method for producing a crystal grain orientation oriented ultrafine grain magnetic material thin plate, wherein the amorphous soft magnetic material is an alloy made of Fe-Si-B.
また、本発明によれば、前記アモルファス軟磁性体は、Ｆｅ−Ｓｉ−Ｂ−Ｃｕ−Ｎｂからなる合金であることを特徴とする結晶粒方位配向ナノ結晶磁性材料薄板の製造方法が得られる。 In addition, according to the present invention, there is obtained a method for producing a crystal grain orientation oriented nanocrystalline magnetic material thin plate, wherein the amorphous soft magnetic material is an alloy made of Fe-Si-B-Cu-Nb.
また、本発明によれば、前記強直流磁場は、磁束密度が２Ｔ以上で、磁場の方向は前記薄板状アモルファス軟磁性体の平面と平行方向であることを特徴とする結晶粒方位配向超微細結晶粒磁性材料薄膜およびナノ結晶磁性材料薄板の製造方法が得られる。 According to the present invention, the strong DC magnetic field has a magnetic flux density of 2T or more, and the direction of the magnetic field is parallel to the plane of the thin plate-like amorphous soft magnetic material. A method for producing a crystalline magnetic material thin film and a nanocrystalline magnetic material thin plate is obtained.
また、本発明によれば、前記強強直流磁場中で結晶化した結晶粒方位配向ナノ結晶磁性材料薄板磁場の飽和磁束密度が、無磁場中で結晶化した結晶粒方位配向ナノ結晶磁性材料薄板磁場の飽和磁束密度より、大きいことを特徴とする結晶粒方位配向ナノ結晶磁性材料薄板の製造方法が得られる。 Further, according to the present invention, the saturation magnetic flux density of the crystal orientation-oriented nanocrystalline magnetic material thin plate crystallized in the strong direct current magnetic field is a crystal orientation oriented nanocrystalline magnetic material thin plate crystallized in the absence of a magnetic field. A method for producing a crystal grain orientation-oriented nanocrystalline magnetic material thin plate characterized by being larger than the saturation magnetic flux density of the magnetic field is obtained.
本発明によれば、２Ｔ程度の通常の電磁石でも容易に作れる磁場強度で、結晶粒方位を配向させた集合組織をもち、磁気特性が向上したナノ結晶材料薄膜を作製する製造方法を提供することができる。 According to the present invention, there is provided a manufacturing method for producing a nanocrystalline material thin film having an improved texture and a texture in which crystal grains are oriented with a magnetic field intensity that can be easily produced even with a normal electromagnet of about 2T. Can do.
以下、本発明の実施の最良の形態について図面を参照して詳細に説明する。図１は、本発明のアモルファス合金の磁場中結晶化の概念図である。アモルファス相からの結晶化による微細組織形成は、結晶核の形成およびその後の結晶相の粒成長によって起こる。一般には、ランダムな結晶方位を有する核が形成され、またある方位の結晶が優先成長することは無いので、結晶粒方位が集合化した組織は得られない。しかし、強磁性相である結晶相には磁気異方性があり、結晶核形成段階において強磁場を印加することにより、磁気異方性エネルギーを最も小さくすることができる方位の結晶核が優先して形成され、また、その後そのような核が優先成長することが期待される。その結果、結晶粒方位がシャープに配向した集合組織を形成することができる。 DESCRIPTION OF THE PREFERRED EMBODIMENTS The best mode for carrying out the present invention will be described below in detail with reference to the drawings. FIG. 1 is a conceptual diagram of crystallization of an amorphous alloy of the present invention in a magnetic field. Microstructure formation by crystallization from the amorphous phase occurs by the formation of crystal nuclei and subsequent grain growth of the crystal phase. In general, nuclei having random crystal orientations are formed, and crystals with a certain orientation never preferentially grow, so that a structure in which crystal grain orientations are aggregated cannot be obtained. However, the crystalline phase, which is a ferromagnetic phase, has magnetic anisotropy. By applying a strong magnetic field during the formation of crystal nuclei, crystal nuclei with the orientation that can minimize the magnetic anisotropy energy take precedence. It is also expected that such nuclei will grow preferentially. As a result, it is possible to form a texture in which the crystal grain orientation is oriented sharply.
図２は、Ｆｅ78Ｓｉ9Ｂ13アモルファス合金薄板をアモルファス相の結晶化温度（８００Ｋ）以上、結晶化相のキュリー温度（９７０Ｋ）以下の温度８５３Ｋで３０分間、０〜６Ｔの磁場作用下で結晶化させた後のX線回折プロファイルである。磁場はアモルファス合金薄板の平面と平行方向で、この場合は平面長手方向に印かされている。図２から明らかに、６Ｔの磁場を印加することにより、Ｓｉを固溶したα鉄（α-Ｆｅ（Ｓｉ））に於ける｛１１０｝のピークが非常に強くなっており、結晶化した相が｛１１０｝方位へ配向していることを示唆している。ここでＦｅ2Ｂも若干形成される為記載してあるがその寄与度は低い。 FIG. 2 shows that an Fe 78 Si 9 B 13 amorphous alloy sheet is subjected to a magnetic field of 0 to 6 T for 30 minutes at a temperature of 853 K, which is not lower than the crystallization temperature (800 K) of the amorphous phase and not higher than the Curie temperature (970 K) of the crystallization phase. It is an X-ray diffraction profile after crystallization. The magnetic field is in the direction parallel to the plane of the amorphous alloy sheet, in this case the plane longitudinal direction. As apparent from FIG. 2, by applying a magnetic field of 6T, the {110} peak in α-iron (α-Fe (Si)) in which Si is dissolved is very strong, and the crystallized phase Is oriented in the {110} orientation. Here, Fe 2 B is also formed because it is slightly formed, but its contribution is low.
図３は、前記Ｆｅ78Ｓｉ9Ｂ13アモルファス合金を温度８５３Ｋで３０分間、結晶化した後の微細組織を方位像顕微鏡 （ＯＩＭ）により観察した結果である。図３（ａ）は無磁場中結晶化、図３（ｂ）は試料長さ方向に平行に６Ｔの磁場を印加したもの、図３（ｃ）は試料表面に垂直に６Ｔの磁場を印加したものである。図３（ａ）および図３（ｃ）では、結晶粒の方位はランダムに分布しているのに対し、試料表面に平行に６Ｔの磁場を印加した図３（ｂ）の試料では、試料表面法線方向が＜１１０＞方位にシャープに配向しているのがわかる。 FIG. 3 shows the result of observation of the microstructure after crystallization of the Fe 78 Si 9 B 13 amorphous alloy at a temperature of 853 K for 30 minutes with an orientation image microscope (OIM). 3A shows crystallization in the absence of a magnetic field, FIG. 3B shows a 6T magnetic field applied in parallel to the sample length direction, and FIG. 3C shows a 6T magnetic field applied perpendicular to the sample surface. Is. 3 (a) and 3 (c), the orientation of crystal grains is randomly distributed, whereas in the sample of FIG. 3 (b) in which a 6T magnetic field is applied in parallel to the sample surface, the sample surface It can be seen that the normal direction is sharply oriented in the <110> direction.
また、図４は図３に示した各試料の逆極点図である。図４（ａ）は無磁場中結晶化、図４（ｂ）は試料長さ方向に平行に６Ｔの磁場を印加したもの、図４（ｃ）は試料表面に垂直に６Ｔの磁場を印加したものである。図４（ａ）および図４（ｃ）では、結晶粒は試料表面内方位はランダムに分布している。これに対して、図４（ｂ）では、密度分布が各極付近集中しており、磁場作用により１軸集合組織が形成されていることが明らかである。
図５は、Ｆｅ73.5Ｓｉ13.5Ｂ9Ｎｂ3Ｃｕ1アモルファス合金薄板をアモルファス相の結晶化温度（７５０Ｋ）以上、結晶化相のキュリー温度（９２０Ｋ）以下の温度８２３Ｋで３０分間、真空中において０〜６Ｔの磁場作用下で結晶化させた後のＸ線回折プロファイルである。磁場はアモルファス合金薄板の平面と平行方向で、この場合は平面長手方向に印加されている。磁場強度の増加とともに、Ｓｉを固溶したα鉄（α−Ｆｅ（Ｓｉ））の｛１１０｝のピークがしだいに強くなっており、結晶化した相が｛１１０｝方位へ配向、または結晶化が促進されていることを示唆している。また、Ｘ線回折プロファイルから求めた結晶粒径は25nmであった。
図６はＦｅ73.5Ｓｉ13.5Ｂ9Ｎｂ3Ｃｕ1アモルファス合金薄板を磁場中（８２３Ｋ, ３０分）および無磁場中で結晶化した試料の磁化曲線を示している。無磁場中で結晶化した試料の飽和磁束密度は１．２２Ｔであり，アモルファス状態の試料の１．２９Ｔに比べ減少するのに対し，磁場中で結晶化した試料の飽和磁束密度は１．３６Ｔから１．４０Ｔと増加することが見出された．また，６Ｔの磁場中で結晶化した試料では透磁率が，無磁場中で結晶化した試料に比べ約３１％大きくなった。
FIG. 4 is a reverse pole figure of each sample shown in FIG. 4A shows crystallization in the absence of a magnetic field, FIG. 4B shows a case where a 6T magnetic field is applied parallel to the sample length direction, and FIG. 4C shows a case where a 6T magnetic field is applied perpendicularly to the sample surface. Is. In FIG. 4A and FIG. 4C, the crystal grains are randomly distributed in the sample surface orientation. On the other hand, in FIG. 4B, the density distribution is concentrated near each pole, and it is clear that a uniaxial texture is formed by the magnetic field action.
FIG. 5 shows that an Fe 73.5 Si 13.5 B 9 Nb 3 Cu 1 amorphous alloy sheet is heated at 823 K for 30 minutes at a temperature not lower than the crystallization temperature (750 K) of the amorphous phase and not higher than the Curie temperature (920 K) of the crystallization phase. It is an X-ray-diffraction profile after crystallizing under the magnetic field effect of -6T. The magnetic field is applied in a direction parallel to the plane of the amorphous alloy thin plate, in this case, in the plane longitudinal direction. As the magnetic field strength increases, the {110} peak of α-iron (α-Fe (Si)) in which Si is dissolved is gradually strengthened, and the crystallized phase is oriented or crystallized in the {110} direction. Suggests that this is being promoted. The crystal grain size obtained from the X-ray diffraction profile was 25 nm.
FIG. 6 shows a magnetization curve of a sample obtained by crystallizing a Fe 73.5 Si 13.5 B 9 Nb 3 Cu 1 amorphous alloy thin plate in a magnetic field (823 K, 30 minutes) and in a non-magnetic field. The saturation magnetic flux density of the sample crystallized in the magnetic field is 1.22 T, which is lower than that of the amorphous sample 1.29 T, whereas the saturation magnetic flux density of the sample crystallized in the magnetic field is 1.36 T. It was found to increase to 1.40T. Further, the permeability of the sample crystallized in the 6T magnetic field was about 31% larger than that of the sample crystallized in the absence of a magnetic field.
さらに、磁場中結晶化したＦｅ73.5Ｓｉ13.5Ｂ9Ｎｂ3Ｃｕ1試料について、結晶化の際に印加した磁場に平行な方向とそれに垂直な方向に磁場を印加して測定された磁化曲線から測定された磁気異方性定数Ｋｕは約８０Ｊ／ｍ3であり、無磁場結晶化された試料について報告されているＫｕ＝１５Ｊ／ｍ3の５倍以上となった。これらのことは、磁場中結晶化によりナノ結晶材料の優れた軟磁気特性と結晶磁気異方性を兼ねそなえた特徴を有する磁性材料の開発が可能であることを示している。この特徴は、特に高周波領域でのナノ結晶軟磁性材料の使用を可能とするものである。 Furthermore, the Fe 73.5 Si 13.5 B 9 Nb 3 Cu 1 sample crystallized in the magnetic field was measured from the magnetization curve measured by applying the magnetic field in the direction parallel to and perpendicular to the magnetic field applied during crystallization. The measured magnetic anisotropy constant Ku was about 80 J / m 3 , which was more than 5 times the Ku = 15 J / m 3 reported for the sample subjected to magnetic field crystallization. These facts indicate that it is possible to develop a magnetic material having characteristics that combine excellent soft magnetic properties and crystal magnetic anisotropy of a nanocrystalline material by crystallization in a magnetic field. This feature enables the use of nanocrystalline soft magnetic materials, particularly in the high frequency region.
また、本発明である磁場中結晶化によるナノ結晶材料の結晶粒方位配向は、実施例に記載したＦｅ78Ｓｉ9Ｂ13アモルファス合金に限らず、強磁性材料であるならば同様の効果が期待でき、特にＦｅ−Ｓｉ−Ｂ合金に限定されるものではない。さらに、近年、強磁場作用下では、非磁性材料に関しても磁場の影響が発現することが報告されており、そのような強磁性材料以外の材料に関しても応用可能である。 Further, the crystal grain orientation orientation of the nanocrystalline material by crystallization in a magnetic field according to the present invention is not limited to the Fe 78 Si 9 B 13 amorphous alloy described in the examples, and the same effect is expected if it is a ferromagnetic material. In particular, it is not limited to the Fe—Si—B alloy. Furthermore, in recent years, it has been reported that the influence of a magnetic field is exerted even on nonmagnetic materials under the action of a strong magnetic field, and the present invention can be applied to materials other than such ferromagnetic materials.
本発明に係る製造方法で得られるアモルファス合金の磁場中結晶化による結晶粒方位配向ナノ結晶材料は高周波トランス、磁気ヘッド、磁気シールド等の電子機器の様々な分野に利用できる。 The crystal grain orientation oriented nanocrystalline material obtained by crystallization of an amorphous alloy in a magnetic field obtained by the production method according to the present invention can be used in various fields of electronic equipment such as a high frequency transformer, a magnetic head, and a magnetic shield.
Claims (6)
The saturation magnetic flux density of the grain orientation oriented nanocrystalline magnetic material thin plate magnetic field crystallized in the strong DC magnetic field is larger than the saturation magnetic flux density of the crystal grain orientation oriented nanocrystalline magnetic material thin magnetic field crystallized in the absence of a magnetic field. A method for producing a crystal grain orientation-oriented nanocrystalline magnetic material thin plate according to claim 1 and 3-5.
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| JP2009543370A (en) * | 2006-07-12 | 2009-12-03 | ファキュウムシュメルゼ ゲーエムベーハー ウント コンパニー カーゲー | Method for manufacturing magnetic core, magnetic core and inductive member with magnetic core |
| US8287664B2 (en) | 2006-07-12 | 2012-10-16 | Vacuumschmelze Gmbh & Co. Kg | Method for the production of magnet cores, magnet core and inductive component with a magnet core |
| JP2008142895A (en) * | 2006-12-05 | 2008-06-26 | Fujifilm Corp | Mold structure |
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| JP6260667B1 (en) * | 2016-09-30 | 2018-01-17 | Tdk株式会社 | Soft magnetic alloy |
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| WO2019189614A1 (en) * | 2018-03-29 | 2019-10-03 | 新東工業株式会社 | Iron-based soft magnetic powder, method of manufacturing same, article including iron-based soft magnetic alloy powder, and method of manufacturing same |
| JPWO2019189614A1 (en) * | 2018-03-29 | 2021-04-22 | 新東工業株式会社 | Iron-based soft magnetic powder and its manufacturing method, and articles containing iron-based soft magnetic alloy powder and its manufacturing method |
| JP7024859B2 (en) | 2018-03-29 | 2022-02-24 | 新東工業株式会社 | Iron-based soft magnetic powder and its manufacturing method, and articles containing iron-based soft magnetic alloy powder and its manufacturing method |
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