JP6227336B2 - Method for producing soft magnetic core - Google Patents
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Description
本発明は、トランスやインダクタ、リアクトルなどに使用されるＦｅ基ナノ結晶合金を用いた軟磁性コアの製造方法に関する。 The present invention relates to a method for manufacturing a soft magnetic core using an Fe-based nanocrystalline alloy used for a transformer, an inductor, a reactor, and the like.
Ｆｅ基ナノ結晶合金は、高飽和磁束密度と低磁歪の両立が可能な軟磁性材料である。このＦｅ基ナノ結晶合金を用いた軟磁性コアの製造においては、アモルファス構造を有する合金組成物の薄帯を積層してコアを形成し、コアに熱処理を施して微細なｂｃｃＦｅ結晶を析出させる必要がある。 The Fe-based nanocrystalline alloy is a soft magnetic material that can achieve both high saturation magnetic flux density and low magnetostriction. In manufacturing a soft magnetic core using this Fe-based nanocrystalline alloy, it is necessary to form a core by laminating thin ribbons of an alloy composition having an amorphous structure, and heat-treating the core to precipitate fine bccFe crystals There is.
しかし、熱処理によってｂｃｃＦｅ結晶を析出させる際、ｂｃｃＦｅ結晶の結晶化に伴う自己発熱による過剰な温度上昇が起こり、ｂｃｃＦｅ結晶の結晶粒の肥大化とＦｅ−Ｂ、Ｆｅ−ＰなどのＦｅ化合物の析出による軟磁気特性の低下が生じる問題がある。 However, when the bccFe crystal is precipitated by heat treatment, an excessive temperature rise occurs due to self-heating due to the crystallization of the bccFe crystal, and the crystal grains of the bccFe crystal are enlarged and Fe compounds such as Fe-B and Fe-P are precipitated. There is a problem that the soft magnetic characteristics are deteriorated due to.
上記問題の対策として、特許文献１には、微細なｂｃｃＦｅ結晶を析出させる熱処理方法として、アモルファス相を主体とする急冷体を加熱して、ｂｃｃＦｅ結晶の結晶化に伴う発熱が開始した時点で１回目の熱処理を終了し、結晶化の発熱の終了後に２回目の熱処理を行う熱処理方法が開示されている。これにより、結晶化開始温度よりも高く、かつ化合物相を実質的に形成しない温度で熱処理を行うことで、結晶化に伴う自己発熱による過剰な温度上昇を防止して結晶粒の肥大化を防止することができ、軟磁気特性に優れたＦｅ基軟磁性合金の軟磁性コアを製造することができるとしている。
As a countermeasure against the above problem,
特許文献１では、ｂｃｃＦｅ結晶の結晶化による自己発熱の開始時点を検出する方法として、熱処理炉内部の雰囲気温度と、アモルファス構造を有する合金組成物を積層したコアの温度を同時に連続して計測し、コアの温度上昇率が雰囲気温度の上昇率よりも高くなった時点を検出することで検知できるとしている。
In
コアの温度の計測は、実際的には熱処理炉内に収容されている全てのコアについて実施することは製造コストを考慮すると現実的ではないので、温度を計測するコアを限定する必要がある。しかし、ｂｃｃＦｅ結晶の結晶化による自己発熱の開始時点は、炉の場所による温度条件や、熱処理炉の昇温速度、あるいはコアの大きさ、コアの製造時による組成ばらつきなどによって、個々のコアによってばらつきがあるので、限定されたコアによる温度計測では検出にもずれを生じることとなり、コアによっては昇温停止のタイミングに遅れが生じて、結晶化に伴う自己発熱よる過加熱でＦｅ化合物が析出して軟磁気特性が劣化する問題がある。 In practice, it is not practical to measure the temperature of the core with respect to all the cores accommodated in the heat treatment furnace, so that it is not practical to consider the manufacturing cost. However, the starting point of self-heating due to the crystallization of the bccFe crystal depends on the temperature of the furnace location, the heating rate of the heat treatment furnace, the size of the core, the composition variation due to the manufacture of the core, etc. Due to the variation, temperature measurement with a limited core will also cause a deviation in detection. Depending on the core, the timing of temperature rise stop may be delayed, and Fe compound may precipitate due to overheating due to self-heating due to crystallization. Thus, there is a problem that the soft magnetic characteristics deteriorate.
また、ｂｃｃＦｅ結晶の結晶化に伴う自己発熱を検知して昇温を停止したとしても、炉内温度が降下するには時間遅れが有るので、自己発熱による温度上昇はしばらくの間継続することになり、ｂｃｃＦｅ結晶化温度（第１結晶化温度）とＦｅ−Ｂなどの化合物の結晶化温度（第２結晶化温度）との差が小さいアモルファス合金組成物の場合には、コア内部の温度はＦｅ化合物の結晶化温度を超え、Ｆｅ化合物が析出して軟磁気特性が劣化する問題もある。 Further, even if self-heating due to crystallization of the bccFe crystal is detected and the temperature rise is stopped, there is a time delay for the furnace temperature to drop, so the temperature rise due to self-heating will continue for a while. In the case of an amorphous alloy composition in which the difference between the bccFe crystallization temperature (first crystallization temperature) and the crystallization temperature of the compound such as Fe-B (second crystallization temperature) is small, the temperature inside the core is There is also a problem that the crystallization temperature of the Fe compound is exceeded, and the Fe compound is precipitated and the soft magnetic properties are deteriorated.
本発明は、上記従来技術が抱える問題点を解決し、Ｆｅ化合物の析出を抑制し、軟磁気特性に優れた軟磁性コアの製造方法を提供することを目的とする。 The object of the present invention is to solve the above-mentioned problems of the prior art and to provide a method for producing a soft magnetic core that suppresses the precipitation of Fe compounds and has excellent soft magnetic properties.
上記の目的を達成するため、本発明による軟磁性コアの製造方法は、Ｆｅを主成分として、すくなくともＢ、Ｐ、およびＣｕを含有するアモルファス合金薄帯を積層して形成される軟磁性コアの製造方法において、前記アモルファス合金薄帯のすくなくとも一方の面に、吸熱反応温度が、前記アモルファス合金薄帯のｂｃｃＦｅの結晶化による発熱が開始する第１結晶化温度と、Ｆｅ化合物の結晶化による発熱が開始する第２結晶化温度の間にある吸熱反応物質を配置して、熱処理を行うことを特徴とする。 In order to achieve the above object, a method of manufacturing a soft magnetic core according to the present invention includes a soft magnetic core formed by laminating amorphous alloy ribbons containing Fe as a main component and at least B, P, and Cu. In the production method, at least one surface of the amorphous alloy ribbon has an endothermic reaction temperature, a first crystallization temperature at which heat generation due to crystallization of bccFe of the amorphous alloy ribbon starts, and heat generation due to crystallization of the Fe compound. An endothermic reaction substance located between the second crystallization temperatures at which is started is disposed and heat treatment is performed.
また本発明では、前記吸熱反応物質が、メラミン樹脂、炭酸塩化合物、ＺｎまたはＺｎを含む合金から選択される一種類以上の物質であることが望ましい。 In the present invention, it is desirable that the endothermic reaction substance is one or more kinds of substances selected from melamine resin, carbonate compound, Zn or an alloy containing Zn.
また本発明では、前記軟磁性コアが、前記アモルファス合金薄帯を、トロイダル状に巻いて形成されることが望ましい。 In the present invention, it is preferable that the soft magnetic core is formed by winding the amorphous alloy ribbon in a toroidal shape.
本発明において、第１結晶化温度とは、アモルファス合金薄帯のｂｃｃＦｅの結晶化による発熱が開始する温度であり、第２結晶化温度とは、Ｆｅ−Ｂ、Ｆｅ−ＰなどのＦｅ化合物の結晶化による発熱が開始する温度である。 In the present invention, the first crystallization temperature is a temperature at which heat generation due to crystallization of bccFe of an amorphous alloy ribbon starts, and the second crystallization temperature is an Fe compound such as Fe-B or Fe-P. This is the temperature at which heat generation due to crystallization starts.
また、本発明において、吸熱反応温度とは、吸熱反応による吸熱量が最大となる温度である。 In the present invention, the endothermic reaction temperature is a temperature at which the endothermic amount due to the endothermic reaction is maximized.
本発明による軟磁性コアの製造方法は、アモルファス合金薄帯に吸熱反応物質を配置して熱処理を行うため、アモルファス合金相から析出するｂｃｃＦｅ結晶の、結晶化による自己発熱による熱量は、吸熱反応物質による吸熱反応によって自律的に吸収することができるので、熱処理炉などのコア外部の温度条件の特別な制御等を必要とせずにコアの過加熱を防ぐことで、結晶粒の肥大化による軟磁気特性の劣化を抑制することが可能となる。 In the method of manufacturing a soft magnetic core according to the present invention, an endothermic reaction material is disposed on an amorphous alloy ribbon and heat treatment is performed. Therefore, the amount of heat generated by self-heating of the bccFe crystal precipitated from the amorphous alloy phase is determined by the endothermic reaction material. Can be absorbed autonomously by the endothermic reaction due to the heat, so the core can be prevented from overheating without requiring special control of the temperature conditions outside the core, such as a heat treatment furnace. It becomes possible to suppress deterioration of characteristics.
また、吸熱反応物質の吸熱反応温度は、アモルファス合金薄帯の第１結晶化温度と第２結晶化温度の間にあるので、熱処理におけるコアの到達温度は第１結晶化温度を超え、ｂｃｃＦｅ結晶を確実に析出させることができる。一方、吸熱反応温度を超える過加熱は、吸熱反応によって抑制されるので、コアが第２結晶化温度へ到達することはなく、Ｆｅ化合物の析出が防止されるため、優れた軟磁気特性を有する軟磁性コアを得ることが可能となる。 In addition, since the endothermic reaction temperature of the endothermic reactant is between the first crystallization temperature and the second crystallization temperature of the amorphous alloy ribbon, the temperature reached by the core in the heat treatment exceeds the first crystallization temperature, and the bccFe crystal Can be reliably deposited. On the other hand, since overheating exceeding the endothermic reaction temperature is suppressed by the endothermic reaction, the core does not reach the second crystallization temperature and the precipitation of the Fe compound is prevented, so that it has excellent soft magnetic characteristics. A soft magnetic core can be obtained.
以上のように、本発明によれば、ｂｃｃＦｅ結晶の肥大化と、Ｆｅ化合物の析出を抑制し、優れた軟磁気特性を有する軟磁性コアの製造方法が提供できる。 As described above, according to the present invention, it is possible to provide a method for producing a soft magnetic core having excellent soft magnetic properties by suppressing the enlargement of bccFe crystals and precipitation of Fe compounds.
以下、本発明の実施の形態を説明する。 Embodiments of the present invention will be described below.
図１は、本発明による軟磁性コアの製造方法の一例を示す図で、図１（ａ）は、片面に吸熱反応物質の層が形成されたアモルファス合金薄帯をトロイダル状に巻いて積層した熱処理前の軟磁性コアの斜視図を示す。図１（ｂ）は、図１（ａ）におけるＡ面の部分拡大断面図を示している。アモルファス合金薄帯２の片面に吸熱反応物質３の層が形成されており、アモルファス合金薄帯２を積層することによって、吸熱反応物質３とアモルファス合金薄帯２が交互に配置されるので、本発明における吸熱作用が効果的に発揮できる。
FIG. 1 is a diagram showing an example of a method for producing a soft magnetic core according to the present invention. FIG. 1 (a) is a diagram of laminating an amorphous alloy ribbon having an endothermic reaction material layer formed on one side in a toroidal shape. The perspective view of the soft-magnetic core before heat processing is shown. FIG.1 (b) has shown the partial expanded sectional view of the A surface in Fig.1 (a). A layer of the
吸熱反応物質としては、吸熱反応温度がアモルファス合金薄帯の第１結晶化温度と第２結晶化温度の間に有れば、特に限定されない。吸熱反応として昇華を利用する物質、融解を利用する物質、分解反応を利用する物質などを使用することができ、それぞれ昇華温度、融解温度、分解温度が吸熱反応温度として作用する。 The endothermic reaction substance is not particularly limited as long as the endothermic reaction temperature is between the first crystallization temperature and the second crystallization temperature of the amorphous alloy ribbon. As the endothermic reaction, a substance that uses sublimation, a substance that uses melting, a substance that uses a decomposition reaction, or the like can be used, and the sublimation temperature, melting temperature, and decomposition temperature act as the endothermic reaction temperature.
昇華を吸熱反応として利用する吸熱反応物質としては、メラミン樹脂が好ましく、特にメラミンシアヌレートは吸熱量が大きく好適である。 As the endothermic reaction substance utilizing sublimation as an endothermic reaction, a melamine resin is preferable, and melamine cyanurate is particularly preferable because of its large endothermic amount.
融解を吸熱反応として利用する吸熱反応物質としては、ＺｎおよびＺｎを含む合金が好ましい。特にＺｎは融点が４２０℃であり、上述のアモルファス合金薄帯の第１結晶化温度に近く、効率的な吸熱作用を得ることができる。 As an endothermic reaction substance that uses melting as an endothermic reaction, an alloy containing Zn and Zn is preferable. In particular, Zn has a melting point of 420 ° C., is close to the first crystallization temperature of the amorphous alloy ribbon described above, and can obtain an efficient endothermic effect.
またＺｎを主成分とするＣｕやＡｌの合金は、融解温度が組成によって変化するので、融解温度すなわち吸熱反応温度を、アモルファス合金薄帯の第１結晶化温度および第２結晶化温度の高低に合わせて選択することができるため好都合である。 In addition, since the melting temperature of the Cu or Al alloy containing Zn as a main component varies depending on the composition, the melting temperature, that is, the endothermic reaction temperature, is set to be higher or lower than the first crystallization temperature and the second crystallization temperature of the amorphous alloy ribbon. It is convenient because they can be selected together.
分解反応を吸熱反応として利用する吸熱反応物質としては、炭酸マグネシウムや炭酸アルミニウムなどの炭酸塩化合物が好ましい。特に炭酸マグネシウムは吸熱量が大きく好適である。 As the endothermic reaction substance utilizing the decomposition reaction as an endothermic reaction, a carbonate compound such as magnesium carbonate or aluminum carbonate is preferable. Magnesium carbonate is particularly suitable because of its large endotherm.
吸熱反応物質をアモルファス合金薄帯の表面に配置する方法としては、アモルファス合金薄帯の表面に吸熱反応物質の層を形成する方法、吸熱反応物質の薄板をアモルファス合金薄帯と重ねる方法などが有る。これらの方法は、吸熱反応物質の形状に応じて選択することができる。 There are several methods for placing the endothermic reaction material on the surface of the amorphous alloy ribbon, such as a method of forming a layer of the endothermic reaction material on the surface of the amorphous alloy ribbon, and a method of superimposing a thin plate of the endothermic reaction material on the amorphous alloy ribbon. . These methods can be selected according to the shape of the endothermic reactant.
吸熱反応物質の層を形成する方法としては、吸熱反応物質を溶媒に溶解して塗布する方法、吸熱反応物質の粉末を溶媒中に分散させて塗布する方法などが適用できる。 As a method for forming the layer of the endothermic reactant, a method in which the endothermic reactant is dissolved and applied, a method in which powder of the endothermic reactant is dispersed in the solvent, and the like are applicable.
また、アモルファス合金薄帯を積層してコアを作成後、吸熱反応物質が溶解している溶液または吸熱反応物質が分散している分散液に浸漬して、アモルファス合金薄帯の積層面の隙間に浸透させても良い。 Also, after creating a core by laminating amorphous alloy ribbons, immersing them in a solution in which endothermic reactants are dissolved or in a dispersion in which endothermic reactants are dispersed, and in the gaps between the laminated surfaces of the amorphous alloy ribbons It may be infiltrated.
吸熱反応物質が金属の場合にはメッキも適用できるが、アモルファス合金薄帯と吸熱反応物質との密着性は特に必要とはしない。アモルファス合金薄帯の表面に吸熱反応物質の層が形成できれば良く、上記の方法に限定されない。 When the endothermic reaction material is a metal, plating can be applied, but the adhesion between the amorphous alloy ribbon and the endothermic reaction material is not particularly required. The layer of the endothermic reaction material only needs to be formed on the surface of the amorphous alloy ribbon, and is not limited to the above method.
吸熱反応物質の吸熱量については、アモルファス合金薄帯の第１結晶化温度と吸熱反応物質の吸熱温度との差や、吸熱反応の温度特性などに依存するが、アモルファス合金薄帯のｂｃｃＦｅ結晶化による発熱量と同じ程度か、それよりも多い吸熱量があることが望ましい。 Although the endothermic amount of the endothermic reaction material depends on the difference between the first crystallization temperature of the amorphous alloy ribbon and the endothermic temperature of the endothermic reaction material, the temperature characteristics of the endothermic reaction, etc., the bccFe crystallization of the amorphous alloy ribbon It is desirable that the amount of heat absorbed is equal to or greater than the amount of heat generated by
一方、吸熱反応物質の層を形成することによって、軟磁性コア中のＦｅ基ナノ結晶合金の占有率は減少する。したがって吸熱反応物質の層厚としては、占有率の減少による熱処理後の軟磁性コアの軟磁気特性の低下が顕著にならない層厚を選択する必要があり、具体的には、吸熱反応物質の層厚はアモルファス合金薄帯の厚さの１／４以下とすることが望ましい。 On the other hand, by forming the endothermic reaction material layer, the occupation ratio of the Fe-based nanocrystalline alloy in the soft magnetic core is reduced. Therefore, as the layer thickness of the endothermic reactant, it is necessary to select a layer thickness that does not cause a significant decrease in the soft magnetic properties of the soft magnetic core after the heat treatment due to the decrease in the occupation ratio. The thickness is desirably ¼ or less of the thickness of the amorphous alloy ribbon.
軟磁性コアの作製方法としては、片面に吸熱反応物質の層が形成されたアモルファス合金薄帯を、トロイダル状に巻いて積層して作製することができる。また打ち抜きなどの方法によってリング状の薄板に加工し、このリング状の薄板を積層して軟磁性コアを作成しても良い。この場合、吸熱反応物質の層の形成は、アモルファス合金薄帯をリング状に加工した後でも良く、コアを作成したときにアモルファス合金薄帯と吸熱反応物質が交互に積層されていれば良く、順序は問わない。 As a method for producing a soft magnetic core, an amorphous alloy ribbon having an endothermic reaction material layer formed on one side can be wound and laminated in a toroidal shape. Alternatively, a soft magnetic core may be formed by processing into a ring-shaped thin plate by a method such as punching and laminating the ring-shaped thin plate. In this case, the layer of the endothermic reactant may be formed after the amorphous alloy ribbon is processed into a ring shape, as long as the amorphous alloy ribbon and the endothermic reactant are alternately laminated when the core is formed, The order does not matter.
本発明におけるアモルファス合金薄帯は、Ｆｅを主成分として、少なくともＢ、Ｐ、およびＣｕを含有し、組成式ＦｅａＢｂＳｉｃＰｘＣｙＣｕｚで表され、７９．０≦ａ≦８６．０ａｔ％、５≦ｂ≦１３ａｔ％、０≦ｃ≦８ａｔ％、１≦ｘ≦１０ａｔ％、０≦ｙ≦５ａｔ％、０．４≦ｚ≦１．４ａｔ％、および０．０６≦ｚ／ｘ≦１．２０である組成に適用できる。例えば、組成式がＦｅ８３．３Ｂ８Ｐ８Ｃｕ０．７、Ｆｅ８３．３Ｓｉ４Ｂ６Ｐ６Ｃｕ０．７、Ｆｅ８３．３Ｓｉ４Ｂ８Ｐ４Ｃｕ０．７などのアモルファス合金に適用できるが、これらの組成に限定されることはなく、第１結晶化温度と第２結晶化温度を有するアモルファス合金であれば適用が可能である。また、耐食性の改善や電気抵抗の調整などを目的として、Ｆｅの一部をＴｉ、Ｚｒ、Ｈｆ、Ｎｂ，Ｔａ、Ｍｏ、Ｗ、Ｃｒ、Ｃｏ、Ｎｉ、Ａｌ、Ｍｎ、Ａｇ、Ｚｎ、Ｓ、Ｓｎ、Ａｓ、Ｓｂ、Ｂｉ、Ｙ、Ｎ、Ｏおよび希土類元素のうち１種類以上の元素で、組成全体の３ａｔ％以下を置換し、Ｆｅとの合計が７９．０ａｔ％以上、８６．０ａｔ％以下であっても良く、例えば組成式がＦｅ８２．３Ｓｉ４Ｂ８Ｐ４Ｃｕ０．７Ｎｂ１であるアモルファス合金でもよい。 Amorphous alloy ribbon of the present invention, as a main component Fe, contains at least B, P, and Cu, expressed by a composition formula Fe a B b Si c P x C y Cu z, 79.0 ≦ a ≦ 86.0 at%, 5 ≦ b ≦ 13 at%, 0 ≦ c ≦ 8 at%, 1 ≦ x ≦ 10 at%, 0 ≦ y ≦ 5 at%, 0.4 ≦ z ≦ 1.4 at%, and 0.06 ≦ z It can be applied to compositions where /x≦1.20. For example, the composition formula is amorphous such as Fe 83.3 B 8 P 8 Cu 0.7, Fe 83.3 Si 4 B 6 P 6 Cu 0.7 , Fe 83.3 Si 4 B 8 P 4 Cu 0.7 Although it can be applied to an alloy, it is not limited to these compositions, and any amorphous alloy having a first crystallization temperature and a second crystallization temperature is applicable. For the purpose of improving corrosion resistance and adjusting electric resistance, a part of Fe is Ti, Zr, Hf, Nb, Ta, Mo, W, Cr, Co, Ni, Al, Mn, Ag, Zn, S, One or more of Sn, As, Sb, Bi, Y, N, O and rare earth elements replace 3 at% or less of the entire composition, and the total with Fe is 79.0 at% or more, 86.0 at% For example, it may be an amorphous alloy having a composition formula of Fe 82.3 Si 4 B 8 P 4 Cu 0.7 Nb 1 .
（実施例１）
組成式がＦｅ８３．３Ｂ８Ｐ８Ｃｕ０．７となる様に工業鉄、Ｆｅ−Ｂ合金、Ｆｅ−Ｐ合金および電気銅を秤量して高周波誘導加熱炉で溶解し、単ロール液体急冷法を用いて幅３０ｍｍ厚さ２５μｍのアモルファス合金薄帯を作製した。このアモルファス合金薄帯の結晶化温度と、炭酸マグネシウムの吸熱反応温度を示差走査型熱量分析計（ＤＳＣ）を用いて分析を行った。測定結果（ＤＳＣ曲線）を図２に示す。図２より、炭酸マグネシウムの吸熱反応温度は約４３５℃で、アモルファス合金薄帯の第１結晶化温度４０５℃と第２結晶化温度５０５℃の間にあることを確認した。
Example 1
Industrial iron, Fe-B alloy, Fe-P alloy and electrolytic copper are weighed and dissolved in a high-frequency induction heating furnace so that the composition formula is Fe 83.3 B 8 P 8 Cu 0.7. Using this method, an amorphous alloy ribbon having a width of 30 mm and a thickness of 25 μm was produced. The crystallization temperature of the amorphous alloy ribbon and the endothermic reaction temperature of magnesium carbonate were analyzed using a differential scanning calorimeter (DSC). The measurement results (DSC curve) are shown in FIG. From FIG. 2, it was confirmed that the endothermic reaction temperature of magnesium carbonate was about 435 ° C., and was between the first crystallization temperature 405 ° C. and the second crystallization temperature 505 ° C. of the amorphous alloy ribbon.
次に炭酸マグネシウムの粉末をアルコール中に分散させて分散液とし、幅１０ｍｍにスリット加工したアモルファス合金薄帯の表面に塗布した後、室温で２４時間自然乾燥させ、炭酸マグネシウムの層を形成した。層の厚さは４μｍから５μｍであった。 Next, the magnesium carbonate powder was dispersed in alcohol to form a dispersion, which was applied to the surface of the amorphous alloy ribbon that had been slit to a width of 10 mm, and then naturally dried at room temperature for 24 hours to form a magnesium carbonate layer. The layer thickness was 4 μm to 5 μm.
炭酸マグネシウムの層を形成したアモルファス合金薄帯を、トロイダル状に巻いて外径２２ｍｍ、内径１２ｍｍ、重量が２０ｇのコアを作製した。このトロイダル状のコアを、アルゴン雰囲気中にて３８０℃、２０分間熱処理を行い軟磁性コアを作製した。 An amorphous alloy ribbon having a magnesium carbonate layer was wound in a toroidal shape to produce a core having an outer diameter of 22 mm, an inner diameter of 12 mm, and a weight of 20 g. The toroidal core was heat-treated at 380 ° C. for 20 minutes in an argon atmosphere to produce a soft magnetic core.
熱処理後の軟磁性コアに巻き線を施し、インピーダンスアナライザを用いて１ｋＨｚにおける初透磁率を測定した。また交流ＢＨアナライザを用いてコアロスの測定を行った。また熱処理後の薄帯を、エックス線回折（ＸＲＤ）により測定を行い、析出物の同定を行った。結果を表１に示す。 The soft magnetic core after the heat treatment was wound, and the initial permeability at 1 kHz was measured using an impedance analyzer. The core loss was measured using an AC BH analyzer. Moreover, the thin strip after heat processing was measured by X-ray diffraction (XRD), and the deposit was identified. The results are shown in Table 1.
（実施例２）
実施例１における炭酸マグネシウムを、メラミンシアヌレートに換えて軟磁性コアを作製した。示差走査熱量分析の結果を図２に、初透磁率、コアロスの測定および析出物の結果を表１に示す。図２より、メラミンシアヌレートの吸熱反応温度は約４６０℃である。
(Example 2)
A soft magnetic core was produced by replacing the magnesium carbonate in Example 1 with melamine cyanurate. The results of differential scanning calorimetry are shown in FIG. 2, and the initial permeability and core loss measurements and the results of precipitates are shown in Table 1. From FIG. 2, the endothermic reaction temperature of melamine cyanurate is about 460 ° C.
（実施例３）
実施例１における炭酸マグネシウムを、Ｚｎに換えて軟磁性コアを作製した。示差走査熱量分析の結果を図２に、初透磁率、コアロスの測定および析出物の結果を表１に示す。図２より、Ｚｎの吸熱反応温度は、Ｚｎの融点と同じ４２０℃である。
(Example 3)
A soft magnetic core was produced by replacing the magnesium carbonate in Example 1 with Zn. The results of differential scanning calorimetry are shown in FIG. 2, and the initial permeability and core loss measurements and the results of precipitates are shown in Table 1. From FIG. 2, the endothermic reaction temperature of Zn is 420 ° C., which is the same as the melting point of Zn.
（比較例１）
実施例１と同じアモルファス合金薄帯を、幅１０ｍｍにスリット加工し、トロイダル状に巻いて外径２２ｍｍ、内径１２ｍｍ、重量が２０ｇのコアを作製した。このトロイダル状のコアを、実施例と同様にアルゴン雰囲気中にて３８０℃、２０分間熱処理を行い軟磁性コアを作製し、インピーダンスアナライザを用いて１ｋＨｚにおける初透磁率を測定した。また交流ＢＨアナライザを用いてコアロスの測定を行った。結果を表１に示す。
(Comparative Example 1)
The same amorphous alloy ribbon as in Example 1 was slit to a width of 10 mm and wound in a toroidal shape to produce a core having an outer diameter of 22 mm, an inner diameter of 12 mm, and a weight of 20 g. This toroidal core was heat-treated in an argon atmosphere at 380 ° C. for 20 minutes in the same manner as in the Example to produce a soft magnetic core, and the initial permeability at 1 kHz was measured using an impedance analyzer. The core loss was measured using an AC BH analyzer. The results are shown in Table 1.
表１より、本発明による軟磁性コアは、初透磁率が大きくコアロスが小さく、軟磁気特性に優れている。比較例１ではＦｅ−Ｐ相やＦｅ−Ｂ相のＦｅ化合物が薄帯中に析出して特性が大幅に低下しているが、本発明である実施例１〜３ではＦｅ−Ｐ相やＦｅ−Ｂ相などのＦｅ化合物は析出しておらず、初透磁率、コアロスとも良好な特性を得た。 From Table 1, the soft magnetic core according to the present invention has a high initial magnetic permeability and a small core loss, and is excellent in soft magnetic characteristics. In Comparative Example 1, the Fe-P phase and Fe-B phase Fe compounds are precipitated in the ribbon and the characteristics are greatly reduced. In Examples 1 to 3, which are the present invention, the Fe-P phase and Fe Fe compounds such as -B phase were not precipitated, and good characteristics were obtained for both initial permeability and core loss.
図３に、実施例２、３における熱処理後の薄帯表面のエックス線回折（ＸＲＤ）結果を示す。表１に示したようにｂｃｃＦｅ相以外にはアモルファス合金に由来するＦｅ化合物は検出されていない。一方、吸熱反応物質であるメラミンシアヌレート（実施例２）およびＺｎ（実施例３）が表面に残存しているが、軟磁気特性への影響は、Ｆｅ化合物の析出に比べると非常に小さいものである。 FIG. 3 shows X-ray diffraction (XRD) results of the ribbon surface after heat treatment in Examples 2 and 3. As shown in Table 1, no Fe compound derived from the amorphous alloy was detected other than the bccFe phase. On the other hand, melamine cyanurate (Example 2) and Zn (Example 3), which are endothermic reactants, remain on the surface, but the influence on soft magnetic properties is very small compared to precipitation of Fe compounds. It is.
以上の通り、アモルファス合金薄帯のすくなくとも一方の面に、吸熱反応温度が前記アモルファス合金薄帯の第１結晶化温度と第２結晶化温度の間にある吸熱反応物質の層を形成して積層したコアを熱処理して軟磁性コアを製造することにより、Ｆｅ化合物の析出を抑制し、軟磁気特性の優れた軟磁性コアの製造方法が得られる。 As described above, an endothermic reaction material layer having an endothermic reaction temperature between the first crystallization temperature and the second crystallization temperature of the amorphous alloy ribbon is formed on at least one surface of the amorphous alloy ribbon. By producing a soft magnetic core by heat-treating the prepared core, a method for producing a soft magnetic core excellent in soft magnetic properties can be obtained by suppressing the precipitation of Fe compounds.
１ 軟磁性コア
２ アモルファス合金薄帯
３ 吸熱反応物質
1 Soft
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