JPWO2016002945A1 - Magnetic core manufacturing method - Google Patents
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 40
- 238000010438 heat treatment Methods 0.000 claims abstract description 108
- 239000000203 mixture Substances 0.000 claims abstract description 51
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 46
- 239000000956 alloy Substances 0.000 claims abstract description 46
- 238000002425 crystallisation Methods 0.000 claims abstract description 24
- 230000008025 crystallization Effects 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims description 27
- 238000004804 winding Methods 0.000 claims description 10
- 230000000630 rising effect Effects 0.000 claims description 6
- 238000010030 laminating Methods 0.000 claims description 4
- 239000013078 crystal Substances 0.000 description 51
- 239000007788 liquid Substances 0.000 description 11
- 238000010791 quenching Methods 0.000 description 11
- 230000000171 quenching effect Effects 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 9
- 230000004907 flux Effects 0.000 description 9
- 230000007423 decrease Effects 0.000 description 7
- 229910001339 C alloy Inorganic materials 0.000 description 5
- 229910000881 Cu alloy Inorganic materials 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 239000000700 radioactive tracer Substances 0.000 description 2
- 229910017082 Fe-Si Inorganic materials 0.000 description 1
- 229910017133 Fe—Si Inorganic materials 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000000113 differential scanning calorimetry Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009689 gas atomisation Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 229910001004 magnetic alloy Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000002076 thermal analysis method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000009692 water atomization Methods 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
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- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D6/00—Heat treatment of ferrous alloys
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C45/02—Amorphous alloys with iron as the major constituent
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/153—Amorphous metallic alloys, e.g. glassy metals
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
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Abstract
磁芯の製造方法は、第１熱処理工程と、中間体作製工程と、第２熱処理工程とを備えている。第１熱処理工程においては、合金組成物からなる薄帯を熱処理する。中間体作製工程においては、第１熱処理工程後の薄帯を使用して中間体を作製する。第２熱処理工程においては、中間体を熱処理する。合金組成物は、主相としてアモルファス相を有し、且つ、組成式Ｆｅ１００−ａ−ｂ−ｃ−ｄ−ｅ−ｆＣｏａＢｂＳｉｃＰｄＣｕｅＣｆ（但し、３．５≦ａ≦４．５ａｔ％、８≦ｂ≦１１ａｔ％、０＜ｃ≦２ａｔ％、３≦ｄ≦５ａｔ％、０．５≦ｅ≦１．１ａｔ％、０≦ｆ≦２ａｔ％）で表される。第１熱処理工程において、薄帯は、合金組成物の結晶化温度よりも高い第１温度まで第１昇温速度で昇温される。第２熱処理工程において、中間体は、結晶化温度以下の第２温度まで昇温される。（図１）The magnetic core manufacturing method includes a first heat treatment step, an intermediate production step, and a second heat treatment step. In the first heat treatment step, the ribbon made of the alloy composition is heat treated. In the intermediate production step, an intermediate is produced using the ribbon after the first heat treatment step. In the second heat treatment step, the intermediate is heat treated. The alloy composition has an amorphous phase as a main phase, and has a composition formula of Fe100-a-b-c-d-e-fCoaBbSicPdCueCf (where 3.5 ≦ a ≦ 4.5 at%, 8 ≦ b ≦ 11 at. %, 0 <c ≦ 2 at%, 3 ≦ d ≦ 5 at%, 0.5 ≦ e ≦ 1.1 at%, 0 ≦ f ≦ 2 at%). In the first heat treatment step, the ribbon is heated at a first temperature increase rate to a first temperature higher than the crystallization temperature of the alloy composition. In the second heat treatment step, the intermediate is heated to a second temperature not higher than the crystallization temperature. (Figure 1)
Description
本発明は、Ｆｅ基アモルファス薄帯を使用した磁芯の製造方法に関する。 The present invention relates to a method for manufacturing a magnetic core using an Fe-based amorphous ribbon.
特許文献１には、Ｆｅ基軟磁性合金からなる薄帯（Ｆｅ基アモルファス薄帯）を使用したコア（磁芯）の製造方法が開示されている。特許文献１によれば、薄帯及び薄帯を巻回して作製したコアのいずれかに対して、ｂｃｃＦｅからなるナノ結晶粒（ｂｃｃＦｅ結晶粒）を析出するための熱処理が施される。熱処理は２回以上に分けて施され、これにより熱処理における自己発熱の影響が低減される。 Patent Document 1 discloses a method for manufacturing a core (magnetic core) using a ribbon (Fe-based amorphous ribbon) made of an Fe-based soft magnetic alloy. According to Patent Document 1, heat treatment for precipitating nanocrystal grains (bccFe crystal grains) made of bccFe is performed on either a ribbon or a core produced by winding the ribbon. The heat treatment is performed in two or more times, thereby reducing the influence of self-heating in the heat treatment.
Ｃｏを３．５ａｔ％以上且つ４．５ａｔ％以下含む適切な組成比のＦｅ−Ｃｏ−Ｂ−Ｓｉ−Ｐ−Ｃｕ合金やＦｅ−Ｃｏ−Ｂ−Ｓｉ−Ｐ−Ｃｕ−Ｃ合金は、高いアモルファス形成能を有する。また、この合金から作製したＦｅ基アモルファス薄帯（以下、単に「薄帯」という。）は、優れた磁気特性を有する。従って、このような組成の薄帯を巻回することで、優れた磁気特性を有する磁芯を製造し得る。 Fe—Co—B—Si—P—Cu alloys and Fe—Co—B—Si—P—Cu—C alloys having an appropriate composition ratio containing 3.5 at% or more and 4.5 at% or less of Co are highly amorphous. Has the ability to form. In addition, an Fe-based amorphous ribbon (hereinafter simply referred to as “strip”) produced from this alloy has excellent magnetic properties. Therefore, a magnetic core having excellent magnetic properties can be manufactured by winding a ribbon having such a composition.
しかしながら、このような組成の薄帯は、熱処理を行ってｂｃｃＦｅ結晶粒を析出すると脆くなり易い。これにより、薄帯を巻回し難くなる。一方、薄帯を巻回した後に熱処理を行う場合、磁芯が大型化するにつれ、磁芯の各部を均一に熱処理することが困難になる。このため、磁芯が十分な磁気特性を有さないおそれがある。 However, a ribbon having such a composition tends to become brittle when heat treatment is performed to precipitate bccFe crystal grains. This makes it difficult to wind the ribbon. On the other hand, when the heat treatment is performed after winding the ribbon, it becomes difficult to uniformly heat each part of the magnetic core as the magnetic core becomes larger. For this reason, there exists a possibility that a magnetic core may not have sufficient magnetic characteristics.
そこで、本発明は、Ｃｏを３．５ａｔ％以上且つ４．５ａｔ％以下含むＦｅ−Ｃｏ−Ｂ−Ｓｉ−Ｐ−Ｃｕ合金又はＦｅ−Ｃｏ−Ｂ−Ｓｉ−Ｐ−Ｃｕ−Ｃ合金からなる薄帯を使用した磁芯の製造方法であって、十分な磁気特性を有する磁芯の製造方法を提供することを目的とする。 Therefore, the present invention provides a thin film comprising an Fe—Co—B—Si—P—Cu alloy or Fe—Co—B—Si—P—Cu—C alloy containing 3.5 at% or more and 4.5 at% or less of Co. An object of the present invention is to provide a method for manufacturing a magnetic core using a band, and a method for manufacturing a magnetic core having sufficient magnetic properties.
本発明の一の側面は、第１熱処理工程と、中間体作製工程と、第２熱処理工程とを備える磁芯の製造方法を提供する。前記第１熱処理工程においては、合金組成物からなる薄帯を熱処理する。前記中間体作製工程においては、前記第１熱処理工程後の前記薄帯を使用して中間体を作製する。前記第２熱処理工程においては、前記中間体を熱処理する。前記合金組成物は、主相としてアモルファス相を有し、且つ、組成式Ｆｅ１００−ａ−ｂ−ｃ−ｄ−ｅ−ｆＣｏａＢｂＳｉｃＰｄＣｕｅＣｆ（但し、３．５≦ａ≦４．５ａｔ％、８≦ｂ≦１１ａｔ％、０＜ｃ≦２ａｔ％、３≦ｄ≦５ａｔ％、０．５≦ｅ≦１．１ａｔ％、０≦ｆ≦２ａｔ％）で表される。前記第１熱処理工程において、前記薄帯は、前記合金組成物の結晶化温度よりも高い第１温度まで第１昇温速度で昇温される。前記第２熱処理工程において、前記中間体は、前記結晶化温度以下の第２温度まで昇温される。One aspect of the present invention provides a method for manufacturing a magnetic core, which includes a first heat treatment step, an intermediate production step, and a second heat treatment step. In the first heat treatment step, the ribbon made of the alloy composition is heat treated. In the intermediate production step, an intermediate is produced using the ribbon after the first heat treatment step. In the second heat treatment step, the intermediate is heat treated. The alloy composition has an amorphous phase as a main phase, and the composition formula Fe 100-a-b-c -d-e-f Co a B b Si c P d Cu e C f ( however, 3. 5 ≦ a ≦ 4.5 at%, 8 ≦ b ≦ 11 at%, 0 <c ≦ 2 at%, 3 ≦ d ≦ 5 at%, 0.5 ≦ e ≦ 1.1 at%, 0 ≦ f ≦ 2 at%) Is done. In the first heat treatment step, the ribbon is heated at a first temperature increase rate to a first temperature higher than a crystallization temperature of the alloy composition. In the second heat treatment step, the intermediate is heated to a second temperature not higher than the crystallization temperature.
本発明によれば、薄帯の熱処理と中間体の熱処理とが互いに異なる工程で行われる。このため、第１熱処理工程において薄帯を短時間だけ第１温度に保持することで、微小なｂｃｃＦｅ結晶粒を析出させることができる。これにより、薄帯の脆弱化を防止でき、薄帯を巻回することで大型の中間体を作製できる。また、第２熱処理工程において中間体を比較的長時間にわたって第２温度に保持することで、第１熱処理工程において析出したｂｃｃＦｅ結晶粒を成長させ、比較的大きなサイズのｂｃｃＦｅ結晶粒を均質に析出させることができる。これにより、優れた磁気特性を有する磁芯が得られる。 According to the present invention, the heat treatment of the ribbon and the heat treatment of the intermediate are performed in different steps. For this reason, minute bccFe crystal grains can be precipitated by maintaining the ribbon at the first temperature for a short time in the first heat treatment step. Thereby, weakening of a thin strip can be prevented and a large-sized intermediate body can be produced by winding a thin strip. Further, by maintaining the intermediate at the second temperature for a relatively long time in the second heat treatment step, the bccFe crystal grains precipitated in the first heat treatment step are grown, and relatively large sized bccFe crystal particles are uniformly precipitated. Can be made. Thereby, the magnetic core which has the outstanding magnetic characteristic is obtained.
添付の図面を参照しながら下記の最良の実施の形態の説明を検討することにより、本発明の目的が正しく理解され、且つその構成についてより完全に理解されるであろう。 The objects of the present invention will be properly understood and more fully understood with reference to the following description of the preferred embodiment with reference to the accompanying drawings.
本発明については多様な変形や様々な形態にて実現することが可能であるが、その一例として、図面に示すような特定の実施の形態について、以下に詳細に説明する。図面及び実施の形態は、本発明をここに開示した特定の形態に限定するものではなく、添付の請求の範囲に明示されている範囲内においてなされる全ての変形例、均等物、代替例をその対象に含むものとする。 The present invention can be realized in various modifications and various forms. As an example, specific embodiments as shown in the drawings will be described in detail below. The drawings and the embodiments are not intended to limit the invention to the specific forms disclosed herein, but to all modifications, equivalents, alternatives made within the scope of the appended claims. It shall be included in the object.
本発明の実施の形態による合金組成物は、Ｆｅ基ナノ結晶合金の出発原料として好適なものであり、組成式Ｆｅ１００−ａ−ｂ−ｃ−ｄ−ｅ−ｆＣｏａＢｂＳｉｃＰｄＣｕｅＣｆのものである。ここで、３．５≦ａ≦４．５ａｔ％、８≦ｂ≦１１ａｔ％、０＜ｃ≦２ａｔ％、３≦ｄ≦５ａｔ％、０．５≦ｅ≦１．１ａｔ％、０≦ｆ≦２ａｔ％である。即ち、Ｃを含まない場合の組成式は、Ｆｅ１００−ａ−ｂ−ｃ−ｄ−ｅＣｏａＢｂＳｉｃＰｄＣｕｅであり、Ｃを０＜ｆ≦２ａｔ％含む場合の組成式は、Ｆｅ１００−ａ−ｂ−ｃ−ｄ−ｅ−ｆＣｏａＢｂＳｉｃＰｄＣｕｅＣｆである。以下、上述の組成式を「本実施の形態による組成式」という。また、主相としてアモルファス相を有し、且つ、上述の組成式を有する合金組成物を「本実施の形態による合金組成物」という。The alloy composition according to the embodiment of the present invention is suitable as a starting material for an Fe-based nanocrystalline alloy, and has a composition formula of Fe 100-ab-c-d-ef Co a B b Si c P d Cu e C f . Here, 3.5 ≦ a ≦ 4.5 at%, 8 ≦ b ≦ 11 at%, 0 <c ≦ 2 at%, 3 ≦ d ≦ 5 at%, 0.5 ≦ e ≦ 1.1 at%, 0 ≦ f ≦ 2 at%. That is, the composition formula in the case of not including C are Fe 100-a-b-c -d-e Co a B b Si c P d Cu e, the composition formula in the case of C and containing 0 <f ≦ 2at% is Fe 100-a-b-c -d-e-f Co a B b Si c P d Cu e C f. Hereinafter, the above composition formula is referred to as “composition formula according to the present embodiment”. An alloy composition having an amorphous phase as a main phase and having the above composition formula is referred to as “alloy composition according to the present embodiment”.
本実施の形態において、Ｃｏ元素はアモルファス相形成を担う必須元素である。Ｆｅ−Ｂ−Ｓｉ−Ｐ−Ｃｕ合金又はＦｅ−Ｂ−Ｓｉ−Ｐ−Ｃｕ−Ｃ合金に対してＣｏ元素を一定量加えると、Ｆｅ−Ｂ−Ｓｉ−Ｐ−Ｃｕ合金又はＦｅ−Ｂ−Ｓｉ−Ｐ−Ｃｕ−Ｃ合金のアモルファス相形成能が向上する。これにより、例えば、厚みのある連続薄帯を安定して作製することができる。Ｃｏの割合が３．５ａｔ％より少ないと、液体急冷条件下におけるアモルファス相の形成能が低下してしまい、熱処理後の結晶粒径が大きくなり保磁力の上昇を招いてしまう。Ｃｏの割合が４．５ａｔ％より多いと、飽和磁束密度が低下する。また、Ｃｏの割合が４．５ａｔ％より多いと、熱処理後の結晶粒径が大きくなってしまい保磁力の上昇を招いてしまう。従って、Ｃｏの割合は、３．５ａｔ％以上、４．５ａｔ％以下であることが望ましい。アモルファス相形成能を高めるためにＣｏの割合を３．５ａｔ％以上と多くした場合であっても、他の元素Ｂ，Ｓｉ，Ｐ，Ｃｕの割合を下記のように調整することにより、良好な磁気特性を得ることができる。 In the present embodiment, Co element is an essential element for forming an amorphous phase. When a certain amount of Co element is added to the Fe-B-Si-P-Cu alloy or Fe-B-Si-P-Cu-C alloy, the Fe-B-Si-P-Cu alloy or Fe-B-Si The amorphous phase forming ability of the -P-Cu-C alloy is improved. Thereby, for example, a thick continuous ribbon can be stably produced. If the proportion of Co is less than 3.5 at%, the ability to form an amorphous phase under liquid quenching conditions decreases, the crystal grain size after heat treatment increases, and the coercive force increases. When the proportion of Co is more than 4.5 at%, the saturation magnetic flux density is lowered. On the other hand, when the proportion of Co is more than 4.5 at%, the crystal grain size after the heat treatment becomes large and the coercive force is increased. Therefore, it is desirable that the ratio of Co is 3.5 at% or more and 4.5 at% or less. Even when the proportion of Co is increased to 3.5 at% or more in order to enhance the amorphous phase forming ability, it is possible to adjust the proportion of other elements B, Si, P, Cu as follows. Magnetic characteristics can be obtained.
本実施の形態において、Ｂ元素はアモルファス相形成を担う必須元素である。Ｂの割合が８ａｔ％より少ないと、液体急冷条件下におけるアモルファス相の形成能が低下してしまい、熱処理後の結晶粒径が大きくなり保磁力の上昇を招いてしまう。Ｂの割合が１１ａｔ％より多いと、液体急冷条件下におけるアモルファス相の形成能が低下してしまい、熱処理後の結晶粒径が大きくなり保磁力の上昇を招いてしまう。従って、Ｂの割合は、８ａｔ％以上、１１ａｔ％以下であることが望ましい。 In the present embodiment, the B element is an essential element responsible for forming an amorphous phase. If the ratio of B is less than 8 at%, the ability to form an amorphous phase under a liquid quenching condition decreases, the crystal grain size after heat treatment increases, and the coercive force increases. If the ratio of B is more than 11 at%, the ability to form an amorphous phase under a liquid quenching condition decreases, the crystal grain size after heat treatment increases, and the coercive force increases. Therefore, the ratio of B is desirably 8 at% or more and 11 at% or less.
本実施の形態において、Ｓｉ元素はアモルファス形成を担う必須元素である。Ｓｉを含まないと、飽和磁束密度が低下してしまう。Ｓｉの割合が２ａｔ％を超えてしまうと、液体急冷条件下におけるアモルファス相の形成能が低下してしまい、熱処理後の結晶粒径が大きくなり保磁力の上昇を招いてしまう。従って、Ｓｉの割合は、２ａｔ％以下（０を含まない）であることが望ましい。 In the present embodiment, Si element is an essential element responsible for amorphous formation. If Si is not included, the saturation magnetic flux density is lowered. If the Si ratio exceeds 2 at%, the ability to form an amorphous phase under a liquid quenching condition decreases, and the crystal grain size after heat treatment increases, leading to an increase in coercivity. Therefore, it is desirable that the ratio of Si is 2 at% or less (not including 0).
本実施の形態において、Ｐ元素はアモルファス形成を担う必須元素である。Ｐの割合が３ａｔ％より少ないと、液体急冷条件下におけるアモルファス相の形成能が低下してしまい、熱処理後の結晶粒径が大きくなり保磁力の上昇を招いてしまう。Ｐの割合が５ａｔ％より多いと、液体急冷条件下におけるアモルファス相の形成能が低下してしまい、熱処理後の結晶粒径が大きくなり保磁力の上昇を招いてしまう。従って、Ｐの割合は、３ａｔ％以上、５ａｔ％以下であることが望ましい。 In the present embodiment, the P element is an essential element responsible for amorphous formation. If the proportion of P is less than 3 at%, the ability to form an amorphous phase under liquid quenching conditions is lowered, the crystal grain size after heat treatment is increased, and the coercive force is increased. When the proportion of P is more than 5 at%, the ability to form an amorphous phase under a liquid quenching condition is lowered, the crystal grain size after the heat treatment is increased, and the coercive force is increased. Therefore, the ratio of P is desirably 3 at% or more and 5 at% or less.
本実施の形態において、Ｃｕ元素はアモルファス形成を担う必須元素である。Ｃｕの割合が０．５ａｔ％より少ないと、液体急冷条件下におけるアモルファス相の形成能が低下してしまい、熱処理後の結晶粒径が大きくなり保磁力の上昇を招いてしまう。Ｃｕの割合が１．１ａｔ％より多いと、液体急冷条件下におけるアモルファス相の形成能が低下してしまい、熱処理後の結晶粒径が大きくなり保磁力の上昇を招いてしまう。従って、Ｃｕの割合は、０．５ａｔ％以上、１．１ａｔ％以下であることが望ましい。 In the present embodiment, Cu element is an essential element responsible for amorphous formation. If the ratio of Cu is less than 0.5 at%, the ability to form an amorphous phase under liquid quenching conditions decreases, the crystal grain size after heat treatment increases, and the coercive force increases. When the ratio of Cu is more than 1.1 at%, the ability to form an amorphous phase under liquid quenching conditions is lowered, the crystal grain size after heat treatment is increased, and the coercive force is increased. Therefore, the ratio of Cu is desirably 0.5 at% or more and 1.1 at% or less.
本実施の形態において、Ｆｅ元素は、本実施の形態による組成式において残部を占める主元素である。また、Ｆｅ元素は、磁性を担う必須元素である。飽和磁束密度の向上及び原料価格の低減のため、Ｆｅの割合が多いことが基本的には好ましい。 In the present embodiment, the Fe element is a main element that occupies the balance in the composition formula according to the present embodiment. Further, the Fe element is an essential element responsible for magnetism. In order to improve the saturation magnetic flux density and reduce the raw material price, it is basically preferable that the ratio of Fe is large.
本実施の形態による組成式の一つであるＦｅ１００−ａ−ｂ−ｃ−ｄ−ｅＣｏａＢｂＳｉｃＰｄＣｕｅを有する合金組成物に対してＣ元素を一定量加えて合金組成物の総材料コストを下げることとしてもよい。Ｃ元素を加えた場合、薄帯が厚くなっても飽和磁束密度や保磁力などの磁気特性が劣化し難い。但し、Ｃの割合が２ａｔ％を超えると、液体急冷条件下におけるアモルファス相の形成能が低下してしまい、熱処理後の結晶粒径が大きくなり保磁力の上昇を招いてしまう。従って、Ｃ元素を加えて合金組成物の組成式をＦｅ１００−ａ−ｂ−ｃ−ｄ−ｅ−ｆＣｏａＢｂＳｉｃＰｄＣｕｅＣｆとする場合であっても、Ｃの割合は、２ａｔ％以下（０を含まない）であることが望ましい。 Fe 100-a-b-c -d-e Co a B b Si c P d Cu certain amount element C the alloy compositions with e added alloy is one of the formula according to this embodiment The total material cost of the composition may be reduced. When C element is added, magnetic properties such as saturation magnetic flux density and coercive force are unlikely to deteriorate even if the ribbon becomes thick. However, if the proportion of C exceeds 2 at%, the ability to form an amorphous phase under a liquid quenching condition decreases, the crystal grain size after heat treatment increases, and the coercive force increases. Therefore, even if the the addition of C elemental composition formula of the alloy composition Fe 100-a-b-c -d-e-f Co a B b Si c P d Cu e C f, of the C The ratio is desirably 2 at% or less (not including 0).
本実施の形態による合金組成物は、様々な形状を有することができる。例えば、合金組成物は、連続薄帯形状を有していてもよいし、粉末形状を有していてよい。連続薄帯形状の合金組成物は、Ｆｅ基アモルファス薄帯などの製造に使用されている単ロール製造装置や双ロール製造装置のような従来の装置を使用して形成することができる。粉末形状の合金組成物は水アトマイズ法やガスアトマイズ法によって作製してもよいし、薄帯の合金組成物を粉砕することで作製してもよい。 The alloy composition according to the present embodiment can have various shapes. For example, the alloy composition may have a continuous ribbon shape or a powder shape. The continuous ribbon-shaped alloy composition can be formed using a conventional apparatus such as a single roll manufacturing apparatus or a twin roll manufacturing apparatus used for manufacturing an Fe-based amorphous ribbon. The alloy composition in powder form may be produced by a water atomizing method or a gas atomizing method, or may be produced by pulverizing a ribbon-like alloy composition.
本実施の形態による合金組成物を成形して、巻磁芯、積層磁芯、圧粉磁芯などの磁芯を形成することができる。また、その磁芯を用いて、トランス、インダクタ、モータや発電機などの部品を提供することができる。 The alloy composition according to the present embodiment can be molded to form a magnetic core such as a wound magnetic core, a laminated magnetic core, or a dust core. Moreover, components, such as a transformer, an inductor, a motor, and a generator, can be provided using the magnetic core.
本実施の形態による合金組成物は主相としてアモルファス相を有している。従って、本実施の形態による合金組成物をＡｒガス雰囲気のような不活性雰囲気中で熱処理すると、２回以上結晶化される。最初に結晶化が開始した温度を第１結晶化開始温度（Ｔｘ１）とし、２回目の結晶化が開始した温度を第２結晶化開始温度（Ｔｘ２）とする。また、第１結晶化開始温度（Ｔｘ１）と第２結晶化開始温度（Ｔｘ２）の間の温度差をΔＴ＝Ｔｘ２−Ｔｘ１とする。これら結晶化温度は、例えば、示差走査熱量分析（ＤＳＣ）装置を用い、４０℃／分程度の昇温速度で熱分析を行うことで評価可能である。 The alloy composition according to the present embodiment has an amorphous phase as a main phase. Therefore, when the alloy composition according to the present embodiment is heat-treated in an inert atmosphere such as an Ar gas atmosphere, it is crystallized twice or more. The temperature at which crystallization starts first is the first crystallization start temperature (Tx1), and the temperature at which the second crystallization starts is the second crystallization start temperature (Tx2). Further, a temperature difference between the first crystallization start temperature (Tx1) and the second crystallization start temperature (Tx2) is set to ΔT = Tx2−Tx1. These crystallization temperatures can be evaluated by performing thermal analysis at a rate of temperature increase of about 40 ° C./min using, for example, a differential scanning calorimetry (DSC) apparatus.
以下、第１結晶化開始温度（Ｔｘ１）を単に「結晶化温度」という。結晶化温度において析出開始するのは、主として、軟磁性を担うｂｃｃＦｅ（αＦｅ，Ｆｅ−Ｓｉ）結晶であり、第２結晶化開始温度（Ｔｘ２）において析出開始するのは、主として、磁気特性を劣化させるＦｅ−ＢやＦｅ−Ｐなどの結晶である。 Hereinafter, the first crystallization start temperature (Tx1) is simply referred to as “crystallization temperature”. Precipitation starts at the crystallization temperature is mainly bccFe (αFe, Fe-Si) crystal that plays a role of soft magnetism, and precipitation starts at the second crystallization start temperature (Tx2) mainly due to deterioration of magnetic properties. It is a crystal such as Fe—B or Fe—P.
本実施の形態による合金組成物（例えば、薄帯）に対して所定の熱処理を行うことで、Ｆｅ基ナノ結晶合金（例えば、Ｆｅ基ナノ結晶合金薄帯）を得ることができる。また、得られたＦｅ基ナノ結晶合金薄帯を用いて磁芯を作製できる。また、作製した磁芯を用いて、トランス、インダクタ、モータや発電機などの部品を構成できる。 An Fe-based nanocrystalline alloy (for example, an Fe-based nanocrystalline alloy ribbon) can be obtained by performing a predetermined heat treatment on the alloy composition (for example, a ribbon) according to the present embodiment. Moreover, a magnetic core can be produced using the obtained Fe-based nanocrystalline alloy ribbon. Moreover, components, such as a transformer, an inductor, a motor, and a generator, can be comprised using the produced magnetic core.
以下、本実施の形態による磁芯の製造方法について、詳しく説明する。 Hereinafter, the manufacturing method of the magnetic core according to the present embodiment will be described in detail.
図１に示されるように、本実施の形態による磁心の製造方法は、４つの工程、具体的には薄帯作製工程（Ｐ１）と、第１熱処理工程（Ｐ２）と、中間体作製工程（Ｐ３）と、第２熱処理工程（Ｐ４）とを備えている。 As shown in FIG. 1, the manufacturing method of the magnetic core according to the present embodiment includes four steps, specifically, a ribbon production step (P1), a first heat treatment step (P2), and an intermediate production step ( P3) and a second heat treatment step (P4).
図１を参照すると、薄帯作製工程（Ｐ１）において、まず、Ｆｅ、Ｃｏ等を含む原料を秤量した後、溶解して合金溶湯を生成する。このときの秤量は、合金溶湯が本実施の形態による組成式を有するようにして行う。次に、この合金溶湯を急冷凝固させて連続薄帯（以下、単に「薄帯」という。）を作製する。具体的には、例えば、合金溶湯をノズルから排出し、回転する冷却基板の表面に接触させて急冷凝固させる。これにより、主相としてアモルファス相を有する合金組成物からなる薄帯が得られる。薄帯の作製方法は、上述した方法に限定されない。得られた薄帯が主相としてアモルファス相を有し、且つ、本実施の形態による組成式を有する限り、どのような方法であってもよい。 Referring to FIG. 1, in the ribbon production step (P1), first, raw materials containing Fe, Co and the like are weighed and then melted to produce a molten alloy. The weighing at this time is performed so that the molten alloy has the composition formula according to the present embodiment. Next, the molten alloy is rapidly solidified to produce a continuous ribbon (hereinafter simply referred to as “strip”). Specifically, for example, molten alloy is discharged from a nozzle and brought into contact with the surface of a rotating cooling substrate to be rapidly solidified. Thereby, a ribbon made of an alloy composition having an amorphous phase as a main phase is obtained. The method for manufacturing the ribbon is not limited to the method described above. Any method may be used as long as the obtained ribbon has an amorphous phase as a main phase and the composition formula according to the present embodiment.
図１及び図２を参照すると、第１熱処理工程（Ｐ２）において、薄帯は熱処理される。このとき、薄帯を加熱することで、薄帯を、本実施の形態による合金組成物の結晶化温度よりも高い第１温度まで第１昇温速度で急速に昇温する。また、薄帯が第１温度に達した後、薄帯を第１温度近傍で保持することなく、薄帯への加熱を停止する。薄帯への加熱を停止すると、薄帯の温度は徐々に所定温度（例えば、室温）まで降下する（図２の１点鎖線参照）。 1 and 2, in the first heat treatment step (P2), the ribbon is heat treated. At this time, by heating the ribbon, the ribbon is rapidly heated to the first temperature higher than the crystallization temperature of the alloy composition according to the present embodiment at the first temperature increase rate. Further, after the ribbon has reached the first temperature, heating to the ribbon is stopped without holding the ribbon in the vicinity of the first temperature. When heating to the ribbon is stopped, the ribbon temperature gradually decreases to a predetermined temperature (for example, room temperature) (see the one-dot chain line in FIG. 2).
薄帯を第１温度まで昇温することにより、薄帯には、ｂｃｃＦｅ結晶が析出する。但し、薄帯が第１昇温速度で急速に昇温され、且つ、薄帯が第１温度近傍で保持されないため、析出するｂｃｃＦｅ結晶のサイズは微小、例えば粒径１５ｎｍ以下である。換言すれば、第１熱処理工程（Ｐ２）により、薄帯には、薄帯を脆くしない程度の微小なｂｃｃＦｅ結晶が薄帯全体に亘って均一に析出する。更に、薄帯は急速に昇温され、且つ、薄帯の温度は第１温度に達した後に降下する。このため、仮に薄帯が昇温前にｂｃｃＦｅ結晶を含んでいたとしても、ｂｃｃＦｅ結晶は殆ど成長しない。換言すれば、第１熱処理工程（Ｐ２）は、ｂｃｃＦｅ結晶の結晶核を析出するための工程である。 By heating the ribbon to the first temperature, bccFe crystals are precipitated on the ribbon. However, since the ribbon is rapidly heated at the first temperature rise rate and the ribbon is not held near the first temperature, the size of the bccFe crystal to be precipitated is very small, for example, a particle size of 15 nm or less. In other words, by the first heat treatment step (P2), minute bccFe crystals that do not weaken the ribbon are uniformly deposited on the ribbon throughout the ribbon. Further, the ribbon is rapidly heated and the temperature of the ribbon drops after reaching the first temperature. For this reason, even if the ribbon contains bccFe crystals before the temperature rises, the bccFe crystals hardly grow. In other words, the first heat treatment step (P2) is a step for precipitating the crystal nuclei of the bccFe crystal.
第１熱処理工程（Ｐ２）において、第１温度が４３０℃よりも小さい場合、ｂｃｃＦｅ結晶が十分に析出されないおそれがある。このため、第１温度は、４３０℃以上であることが望ましい。但し、第１温度が４８０℃よりも大きい場合、ｂｃｃＦｅ結晶の粗大化やＦｅ−ＢやＦｅ−Ｐなどの結晶の析出により、薄帯の磁気特性が劣化するおそれがある。このため、第１温度は、４８０℃以下であることが望ましい。また、第１昇温速度が毎秒１００℃よりも小さい場合、ｂｃｃＦｅ結晶の粗大化により薄帯の磁気特性が劣化したり薄帯が脆くなったりするおそれがある。このため、第１昇温速度は、毎秒１００℃以上であることが望ましい。 In the first heat treatment step (P2), when the first temperature is lower than 430 ° C., the bccFe crystal may not be sufficiently precipitated. For this reason, the first temperature is desirably 430 ° C. or higher. However, when the first temperature is higher than 480 ° C., the magnetic properties of the ribbon may be deteriorated due to coarsening of the bccFe crystal or precipitation of crystals such as Fe—B or Fe—P. For this reason, it is desirable that the first temperature be 480 ° C. or lower. In addition, when the first rate of temperature rise is less than 100 ° C. per second, the magnetic properties of the ribbon may be deteriorated or the ribbon may become brittle due to the coarsening of the bccFe crystal. For this reason, it is desirable that the first temperature increase rate be 100 ° C. or more per second.
第１熱処理工程（Ｐ２）における具体的な熱処理方法としては、例えば、赤外線加熱や高周波加熱など急速昇温が可能な装置を用いた熱処理方法が考えられる。しかしながら、本発明は、これらに限定されない。 As a specific heat treatment method in the first heat treatment step (P2), for example, a heat treatment method using an apparatus capable of rapid temperature increase such as infrared heating or high frequency heating is conceivable. However, the present invention is not limited to these.
例えば、薄帯を、毎秒０．１ｍ以上かつ毎秒１ｍ以下の速度で昇温環境内を移動させてもよい。この方法によっても、薄帯を、第１昇温速度で昇温することができる。 For example, the ribbon may be moved in the temperature rising environment at a speed of 0.1 m / second or more and 1 m / second or less. Also by this method, the ribbon can be heated at the first heating rate.
具体的には、図４に示されるように、連続薄帯（薄帯）１０は、送り出しローラ５０により、所定の移動速度で搬送される。薄帯１０は、電気炉６０の入口６４を通過して電気炉６０の内部に搬送される。薄帯１０は、電気炉６０の内部を通過して出口６６から電気炉６０の外に出て、巻き取りローラ７０に巻き取られる。電気炉６０の内部には、加熱用の電極（図示せず）等が設けられた昇温環境６２が形成されている。薄帯１０は、昇温環境６２内を移動している間だけ、電極によって加熱される。これにより、薄帯１０は、第１温度まで第１昇温速度で昇温される。第１温度及び第１昇温速度は、昇温環境６２内の電極の温度や薄帯１０の移動速度を調整することで、調整可能である。また、例えば、薄帯１０が第１温度に達したときに電気炉６０の出口６６に到達するように調整することで、薄帯１０が第１温度で保持されないようにできる。電気炉６０の加熱性能等を考慮すると、薄帯１０の移動速度は、毎秒０．１ｍ以上かつ毎秒１ｍ以下であることが望ましい。薄帯１０の移動速度が毎秒０．１ｍ未満の場合は、薄帯１０は、長時間にわたって昇温環境６２内を移動する。このため、薄帯１０は、急速に第１温度に到達した後、第１温度で保持される間に結晶化による自己発熱で高温化し、所望する組織が得られない。一方、薄帯１０の移動速度が毎秒１ｍを超える場合は、熱伝達に必要な時間が得られない。このため、薄帯１０が昇温環境６２内で所望する第１温度に到達せず第一熱処理工程（Ｐ２）の効果が不足する。
Specifically, as shown in FIG. 4, the continuous ribbon (strip) 10 is transported by the
図３に示されるように、本実施の形態による磁心の製造方法は、第１熱処理工程（Ｐ２）の後に降温工程（Ｐ２Ａ）を備えていてもよい。降温工程（Ｐ２Ａ）において、第１熱処理工程（Ｐ２）後の薄帯は、所定の温度まで降温される。降温工程（Ｐ２Ａ）を設けることで、薄帯を、比較的緩やかに自然に降温（図２の１点鎖線参照）するのでなく、薄帯を冷却して所定の温度まで比較的急速に降温（図２の２点鎖線参照）できる。これにより、ｂｃｃＦｅ結晶の粗大化をより確実に防止できると共に、磁心の製造に必要な時間を短縮できる。 As shown in FIG. 3, the method for manufacturing a magnetic core according to the present embodiment may include a temperature lowering step (P2A) after the first heat treatment step (P2). In the temperature lowering step (P2A), the ribbon after the first heat treatment step (P2) is cooled to a predetermined temperature. By providing the temperature lowering step (P2A), the ribbon is not cooled relatively slowly and naturally (refer to the one-dot chain line in FIG. 2), but the ribbon is cooled and cooled to a predetermined temperature relatively quickly ( (See the two-dot chain line in FIG. 2). Thereby, the coarsening of the bccFe crystal can be prevented more reliably, and the time required for manufacturing the magnetic core can be shortened.
降温工程（Ｐ２Ａ）における所定の温度は、例えば室温である。薄帯を室温まで降温することで、降温後の薄帯を容易に加工できる。降温工程（Ｐ２Ａ）における具体的な降温方法としては、例えば、薄帯を空冷してもかまわないし、冷媒を用いて急冷してもよい。但し、本発明は、これらに限定されない。 The predetermined temperature in the temperature lowering step (P2A) is, for example, room temperature. By cooling the ribbon to room temperature, the ribbon after cooling can be easily processed. As a specific temperature lowering method in the temperature lowering step (P2A), for example, the ribbon may be air-cooled or rapidly cooled using a refrigerant. However, the present invention is not limited to these.
以上の説明から理解できるように、第１熱処理工程（Ｐ２）後の薄帯、及び、降温工程（Ｐ２Ａ）後の薄帯は、９０°曲げ可能である。従って、この薄帯を使用して様々な形状の磁性部品を作製可能である。 As can be understood from the above description, the ribbon after the first heat treatment step (P2) and the ribbon after the temperature lowering step (P2A) can be bent by 90 °. Therefore, it is possible to produce magnetic parts of various shapes using this ribbon.
図１及び図３を参照すると、中間体作製工程（Ｐ３）において、第１熱処理工程（Ｐ２）後の薄帯又は降温工程（Ｐ２Ａ）後の薄帯を使用して中間体を作製する。本実施の形態による中間体は、薄帯を巻回又は積層させることで作製される。薄帯の巻回回数や積層回数は何回であってもよい。本発明によれば、第１熱処理工程（Ｐ２）において、薄帯の脆弱化が防止されているため、薄帯を必要な回数だけ巻回又は積層して大型の中間体を作製できる。但し、中間体は、薄帯を巻回又は積層させる以外の方法で作製してもよい。 Referring to FIGS. 1 and 3, in the intermediate production step (P3), an intermediate is produced using the thin strip after the first heat treatment step (P2) or the thin strip after the temperature lowering step (P2A). The intermediate body according to the present embodiment is manufactured by winding or laminating a ribbon. The number of windings and the number of laminations of the ribbon may be any number. According to the present invention, since the thin strip is prevented from being weakened in the first heat treatment step (P2), the large strip can be produced by winding or laminating the thin strip as many times as necessary. However, the intermediate may be produced by a method other than winding or laminating the ribbon.
図１乃至図３を参照すると、第２熱処理工程（Ｐ４）において、中間体は熱処理される。このとき、薄帯を加熱することで、中間体を、合金組成物の結晶化温度以下の第２温度まで昇温する。 Referring to FIGS. 1 to 3, in the second heat treatment step (P4), the intermediate is heat treated. At this time, by heating the ribbon, the temperature of the intermediate is raised to a second temperature not higher than the crystallization temperature of the alloy composition.
前述したように、第１熱処理工程（Ｐ２）において、薄帯には既に微小なｂｃｃＦｅ結晶が十分に析出している。このため、第２熱処理工程（Ｐ４）において、中間体には新たなｂｃｃＦｅ結晶が殆ど析出しない。但し、中間体を第２温度まで昇温することにより、中間体に含まれるｂｃｃＦｅ結晶が成長する。また、成長したｂｃｃＦｅ結晶は、互いに衝突して微細な組織を形成する。これにより、優れた磁気特性を有する磁芯が得られる。換言すれば、第２熱処理工程（Ｐ４）は、ｂｃｃＦｅ結晶の結晶核を成長させ、ｂｃｃＦｅ結晶による微細な組織を形成するための工程である。 As described above, in the first heat treatment step (P2), fine bccFe crystals are already sufficiently deposited on the ribbon. For this reason, in the second heat treatment step (P4), almost no new bccFe crystals are precipitated in the intermediate. However, the bccFe crystal contained in the intermediate grows by raising the temperature of the intermediate to the second temperature. The grown bccFe crystals collide with each other to form a fine structure. Thereby, the magnetic core which has the outstanding magnetic characteristic is obtained. In other words, the second heat treatment step (P4) is a step for growing a crystal nucleus of the bccFe crystal and forming a fine structure by the bccFe crystal.
ｂｃｃＦｅ結晶の過度な成長やＦｅ−ＢやＦｅ−Ｐなどの結晶の析出を防止するためには、第２温度は、結晶化温度以下にする必要がある。ｂｃｃＦｅ結晶を緩やかに成長させることで、自己発熱による熱暴走を回避し易く、且つ、ｂｃｃＦｅ結晶からなる微細な組織が得やすい。ｂｃｃＦｅ結晶を緩やかに成長させるという観点からは、第２温度は結晶化温度以下であり、且つ、より低いほうが好ましい。一方、ｂｃｃＦｅ結晶の体積分率を増加させ磁気特性を向上させるという観点からは、第２温度は結晶化温度近傍であることが好ましい。 In order to prevent excessive growth of bccFe crystals and precipitation of crystals such as Fe-B and Fe-P, the second temperature needs to be lower than the crystallization temperature. By slowly growing the bccFe crystal, it is easy to avoid thermal runaway due to self-heating, and a fine structure made of the bccFe crystal is easily obtained. From the viewpoint of gradually growing the bccFe crystal, the second temperature is preferably equal to or lower than the crystallization temperature and lower. On the other hand, from the viewpoint of increasing the volume fraction of the bccFe crystal and improving the magnetic properties, the second temperature is preferably in the vicinity of the crystallization temperature.
具体的には、第２熱処理工程（Ｐ４）において、第２温度が結晶化温度よりも大きい場合、ｂｃｃＦｅ結晶の粒径が大きくなりすぎて中間体の磁気特性が劣化するおそれがある。このため、第２温度は、４３０℃以下であることが望ましい。但し、第２温度が３８５℃よりも小さい場合、ｂｃｃＦｅ結晶が十分に成長せず、十分な磁気特性が得られないおそれがある。このため、第２温度は、３８５℃以上であることが望ましい。 Specifically, in the second heat treatment step (P4), when the second temperature is higher than the crystallization temperature, the particle size of the bccFe crystal becomes too large, and the magnetic characteristics of the intermediate may be deteriorated. For this reason, the second temperature is desirably 430 ° C. or lower. However, when the second temperature is lower than 385 ° C., the bccFe crystal does not grow sufficiently, and sufficient magnetic properties may not be obtained. For this reason, it is desirable that the second temperature is 385 ° C. or higher.
第２熱処理工程（Ｐ４）において、中間体を、第２温度まで昇温した後、比較的長時間にわたって第２温度近傍（例えば、第２温度±１℃あるいは第２温度±３℃の範囲）に保持してもよい。換言すれば、第２温度まで昇温した中間体に、中間体を第２温度に維持するための熱を、所定の保持時間だけ加えてもよい。これにより、ｂｃｃＦｅ結晶の体積分率を十分に増加させ、ｂｃｃＦｅ結晶粒を均質に成長させることができる。この結果、優れた磁気特性を有する磁芯が得られる。 In the second heat treatment step (P4), after raising the temperature of the intermediate to the second temperature, in the vicinity of the second temperature over a relatively long time (for example, the range of the second temperature ± 1 ° C or the second temperature ± 3 ° C). May be retained. In other words, heat for maintaining the intermediate body at the second temperature may be applied to the intermediate body heated to the second temperature for a predetermined holding time. Thereby, the volume fraction of the bccFe crystal can be sufficiently increased, and the bccFe crystal grains can be grown uniformly. As a result, a magnetic core having excellent magnetic properties can be obtained.
具体的には、第２温度近傍における保持時間が３分よりも小さい場合、ｂｃｃＦｅ結晶が十分に成長しないおそれがある。一方、保持時間が２０分よりも大きい場合、ｂｃｃＦｅ結晶粒が粗大に成長しすぎるおそれがある。このため、保持時間は、３分以上かつ２０分であることが望ましい。換言すれば、中間体を、第２温度まで昇温した後、３分以上かつ２０分以下の間、第２温度近傍に保持することが望ましい。 Specifically, when the holding time in the vicinity of the second temperature is less than 3 minutes, the bccFe crystal may not grow sufficiently. On the other hand, if the holding time is longer than 20 minutes, the bccFe crystal grains may grow too coarse. For this reason, the holding time is desirably 3 minutes or more and 20 minutes. In other words, it is desirable to maintain the intermediate in the vicinity of the second temperature for 3 minutes or more and 20 minutes or less after the temperature is raised to the second temperature.
第２熱処理工程（Ｐ４）における具体的な熱処理方法としては、第１熱処理工程（Ｐ２）における熱処理方法と同様に、様々な方法が可能である。 As a specific heat treatment method in the second heat treatment step (P4), various methods are possible as in the heat treatment method in the first heat treatment step (P2).
以上のようにして作製された本実施の形態による磁芯は、２１ｎｍ以下の平均結晶粒径を有すると共に１．８Ｔ以上の高い飽和磁束密度と１０Ａ／ｍ以下の低い保磁力を有する。 The magnetic core according to the present embodiment manufactured as described above has an average crystal grain size of 21 nm or less, a high saturation magnetic flux density of 1.8 T or more, and a low coercive force of 10 A / m or less.
以下、本発明の実施の形態について、複数の実施例及び複数の比較例を参照しながら更に詳細に説明する。 Hereinafter, embodiments of the present invention will be described in more detail with reference to a plurality of examples and a plurality of comparative examples.
（実施例１〜１７及び比較例１〜２８）
まず、Ｃを含まないＦｅ−Ｃｏ−Ｂ−Ｓｉ−Ｐ−Ｃｕ合金について検証した。詳しくは、原料を下記の表１に掲げられた本発明の実施例１〜１７及び比較例１〜２８の合金組成となるように秤量し、高周波誘導加熱により溶解した。その後、溶解した合金組成物を大気中において単ロール液体急冷法にて処理し、２５μｍ程度の厚さを持つ幅約５０ｍｍ、長さ約５０〜１００ｍの連続薄帯（薄帯）を作製した（薄帯作製工程）。これらの薄帯の合金組成物の相を、Ｘ線回折法にて同定した。これらの薄帯は、いずれも主相としてアモルファス相を有していた。次に、表２記載の熱処理条件の下で、実施例１〜１７及び比較例１〜２８の薄帯を熱処理した（第１熱処理工程）。次に、第１熱処理工程後の薄帯を巻回して中間体を作製した（中間体作製工程）。このとき、第１熱処理工程後の実施例１〜１７の薄帯は、容易に巻回できた。一方、第１熱処理工程後の比較例１〜２８の薄帯のうち、比較例３、４、６、９、１０、１２、１５、１６及び１８の薄帯は、やや脆くなっており、巻回に手間がかかった。更に、表２記載の熱処理条件の下で、中間体を熱処理した（第２熱処理工程）。熱処理された中間体の夫々の飽和磁束密度Ｂｓは振動試料型磁力計（ＶＭＳ）を用いて８００ｋＡ／ｍの磁場にて測定した。各合金組成物の保磁力Ｈｃは直流ＢＨトレーサーを用い２ｋＡ／ｍの磁場にて測定した。測定結果を表２に示す。(Examples 1-17 and Comparative Examples 1-28)
First, an Fe—Co—B—Si—P—Cu alloy containing no C was verified. Specifically, the raw materials were weighed so as to have the alloy compositions of Examples 1 to 17 and Comparative Examples 1 to 28 of the present invention listed in Table 1 below, and dissolved by high frequency induction heating. Thereafter, the melted alloy composition was processed in the atmosphere by a single roll liquid quenching method to produce a continuous ribbon (strip) having a thickness of about 25 μm and a width of about 50 mm and a length of about 50 to 100 m ( (Strip production process). The phases of these ribbon alloy compositions were identified by X-ray diffraction. Each of these ribbons had an amorphous phase as a main phase. Next, the ribbons of Examples 1 to 17 and Comparative Examples 1 to 28 were heat-treated under the heat treatment conditions shown in Table 2 (first heat treatment step). Next, the ribbon after the first heat treatment step was wound to produce an intermediate (intermediate production step). At this time, the ribbons of Examples 1 to 17 after the first heat treatment step could be easily wound. On the other hand, among the ribbons of Comparative Examples 1 to 28 after the first heat treatment step, the ribbons of Comparative Examples 3, 4, 6, 9, 10, 12, 15, 16, and 18 are slightly brittle and wound. It took time and effort. Furthermore, the intermediate was heat-treated under the heat treatment conditions described in Table 2 (second heat treatment step). The saturation magnetic flux density Bs of each heat-treated intermediate was measured using a vibrating sample magnetometer (VMS) in a magnetic field of 800 kA / m. The coercive force Hc of each alloy composition was measured in a magnetic field of 2 kA / m using a direct current BH tracer. The measurement results are shown in Table 2.
表２を参照すると、実施例の薄帯を第１熱処理工程において熱処理し、中間体を第２熱処理工程において熱処理した結果、Ｆｅ基ナノ結晶合金からなる磁芯が得られた。実施例の磁芯の結晶粒径は、すべて２１ｎｍ以下と小さく、１０Ａ／ｍ以下の小さい保磁力を有していると共に、１．８Ｔ以上の高い飽和磁束密度を有していた。 Referring to Table 2, the ribbon of the example was heat treated in the first heat treatment step, and the intermediate was heat treated in the second heat treatment step. As a result, a magnetic core made of Fe-based nanocrystalline alloy was obtained. The crystal grain sizes of the magnetic cores of the examples were all as small as 21 nm or less and had a small coercive force of 10 A / m or less and a high saturation magnetic flux density of 1.8 T or more.
（実施例１７及び比較例２９）
更にＣを含めたＦｅ−Ｃｏ−Ｂ−Ｓｉ−Ｐ−Ｃｕ−Ｃ合金について検証した。詳しくは、原料を下記の表３に掲げられた本発明の実施例１８及び比較例２９の合金組成となるように秤量し、アーク溶解した。その後、溶解した合金組成物を大気中において単ロール液体急冷法にて処理し、２５μｍ程度の厚さを持つ幅約３ｍｍ、長さ約５〜１５ｍの薄帯を作製した。これらの薄帯の合金組成物の相を、Ｘ線回折法にて同定した。これらの薄帯は、いずれも主相としてアモルファス相を有していた。次に、表４記載の熱処理条件の下で、実施例１８及び比較例２９の薄帯を熱処理した（第１熱処理工程）。次に、第１熱処理工程後の薄帯を巻回して中間体を作製した（中間体作製工程）。更に、表４記載の熱処理条件の下で、中間体を熱処理した（第２熱処理工程）。熱処理された中間体の夫々の飽和磁束密度Ｂｓは振動試料型磁力計（ＶＭＳ）を用いて８００ｋＡ／ｍの磁場にて測定した。各合金組成物の保磁力Ｈｃは直流ＢＨトレーサーを用い２ｋＡ／ｍの磁場にて測定した。測定結果を表４に示す。(Example 17 and Comparative Example 29)
Furthermore, it verified about the Fe-Co-B-Si-P-Cu-C alloy containing C. Specifically, the raw materials were weighed so as to have the alloy compositions of Example 18 and Comparative Example 29 listed in Table 3 below, and arc-melted. Thereafter, the melted alloy composition was processed in the atmosphere by a single roll liquid quenching method to produce a ribbon having a thickness of about 25 μm and a width of about 3 mm and a length of about 5 to 15 m. The phases of these ribbon alloy compositions were identified by X-ray diffraction. Each of these ribbons had an amorphous phase as a main phase. Next, the ribbons of Example 18 and Comparative Example 29 were heat-treated under the heat treatment conditions shown in Table 4 (first heat treatment step). Next, the ribbon after the first heat treatment step was wound to produce an intermediate (intermediate production step). Furthermore, the intermediate was heat-treated under the heat treatment conditions described in Table 4 (second heat treatment step). The saturation magnetic flux density Bs of each heat-treated intermediate was measured using a vibrating sample magnetometer (VMS) in a magnetic field of 800 kA / m. The coercive force Hc of each alloy composition was measured in a magnetic field of 2 kA / m using a direct current BH tracer. Table 4 shows the measurement results.
表４を参照すると、実施例１８の薄帯を第１熱処理工程において熱処理し、中間体を第２熱処理工程において熱処理した結果、Ｆｅ基ナノ結晶合金からなる磁芯が得られた。実施例１８の磁芯の結晶粒径は、１６ｎｍと小さく、７．９Ａ／ｍの小さい保磁力を有していると共に、１．８１Ｔの高い飽和磁束密度を有していた。 Referring to Table 4, as a result of heat treating the ribbon of Example 18 in the first heat treatment step and heat treating the intermediate in the second heat treatment step, a magnetic core made of Fe-based nanocrystalline alloy was obtained. The crystal grain size of the magnetic core of Example 18 was as small as 16 nm, had a small coercive force of 7.9 A / m, and had a high saturation magnetic flux density of 1.81 T.
本発明は２０１４年７月３日に日本国特許庁に提出された日本特許出願第２０１４−１３７９３３号に基づいており、その内容は参照することにより本明細書の一部をなす。 The present invention is based on Japanese Patent Application No. 2014-137933 filed with the Japan Patent Office on July 3, 2014, the contents of which are incorporated herein by reference.
本発明の最良の実施の形態について説明したが、当業者には明らかなように、本発明の精神を逸脱しない範囲で実施の形態を変形することが可能であり、そのような実施の形態は本発明の範囲に属するものである。 Although the best embodiment of the present invention has been described, it will be apparent to those skilled in the art that the embodiment can be modified without departing from the spirit of the present invention. It belongs to the scope of the present invention.
１０ 連続薄帯（薄帯）
５０ 送り出しローラ
６０ 電気炉
６２ 昇温環境
６４ 入口
６６ 出口
７０ 巻き取りローラ10 Continuous ribbon (strip)
50
Claims (7)
前記第１熱処理工程後の前記薄帯を使用して中間体を作製する中間体作製工程と、
前記中間体を熱処理する第２熱処理工程と
を備える磁芯の製造方法であって、
前記合金組成物は、主相としてアモルファス相を有し、且つ、組成式Ｆｅ１００−ａ−ｂ−ｃ−ｄ−ｅ−ｆＣｏａＢｂＳｉｃＰｄＣｕｅＣｆ（但し、３．５≦ａ≦４．５ａｔ％、８≦ｂ≦１１ａｔ％、０＜ｃ≦２ａｔ％、３≦ｄ≦５ａｔ％、０．５≦ｅ≦１．１ａｔ％、０≦ｆ≦２ａｔ％）で表され、
前記第１熱処理工程において、前記薄帯は、前記合金組成物の結晶化温度よりも高い第１温度まで第１昇温速度で昇温され、
前記第２熱処理工程において、前記中間体は、前記結晶化温度以下の第２温度まで昇温される
磁芯の製造方法。A first heat treatment step for heat-treating a ribbon made of the alloy composition;
An intermediate production step of producing an intermediate using the ribbon after the first heat treatment step;
A method of manufacturing a magnetic core comprising: a second heat treatment step of heat treating the intermediate;
The alloy composition has an amorphous phase as a main phase, and the composition formula Fe 100-a-b-c -d-e-f Co a B b Si c P d Cu e C f ( however, 3. 5 ≦ a ≦ 4.5 at%, 8 ≦ b ≦ 11 at%, 0 <c ≦ 2 at%, 3 ≦ d ≦ 5 at%, 0.5 ≦ e ≦ 1.1 at%, 0 ≦ f ≦ 2 at%) And
In the first heat treatment step, the ribbon is heated at a first heating rate to a first temperature higher than a crystallization temperature of the alloy composition,
In the second heat treatment step, the intermediate is heated to a second temperature lower than the crystallization temperature.
前記中間体は、前記第１熱処理工程後の前記薄帯を巻回又は積層させることで作製される
磁芯の製造方法。A method of manufacturing a magnetic core according to claim 1,
The said intermediate body is a manufacturing method of the magnetic core produced by winding or laminating | stacking the said strip after the said 1st heat treatment process.
前記第１熱処理工程後の前記薄帯を所定の温度まで降温する降温工程を備えており、
前記中間体は、前記降温工程後の前記薄帯を使用して作製される
磁芯の製造方法。A method of manufacturing a magnetic core according to claim 1 or 2,
A temperature lowering step of lowering the ribbon after the first heat treatment step to a predetermined temperature;
The intermediate body is a method of manufacturing a magnetic core that is manufactured using the ribbon after the temperature lowering step.
前記第１熱処理工程における前記第１昇温速度は、毎秒１００℃以上であり、
前記第１熱処理工程における前記第１温度は、４３０℃以上である
磁芯の製造方法。A method of manufacturing a magnetic core according to any one of claims 1 to 3,
The first temperature increase rate in the first heat treatment step is 100 ° C. or more per second,
The method for manufacturing a magnetic core, wherein the first temperature in the first heat treatment step is 430 ° C. or higher.
前記第１熱処理工程における前記第１温度は、４８０℃以下である
磁芯の製造方法。A method of manufacturing a magnetic core according to claim 4,
The method for manufacturing a magnetic core, wherein the first temperature in the first heat treatment step is 480 ° C. or less.
前記第２熱処理工程における前記第２温度は、３８５℃以上であり、
前記第２熱処理工程において、前記中間体は、前記第２温度まで昇温された後、３分以上かつ２０分以下の間、前記第２温度近傍に保持される
磁芯の製造方法。A method of manufacturing a magnetic core according to any one of claims 1 to 5,
The second temperature in the second heat treatment step is 385 ° C. or higher,
In the second heat treatment step, the intermediate is heated to the second temperature, and then the magnetic core is maintained near the second temperature for 3 minutes to 20 minutes.
前記第１熱処理工程において、前記薄帯は、毎秒０．１ｍ以上かつ毎秒１ｍ以下の速度で昇温環境内を移動し、これにより前記第１昇温速度で昇温される
磁芯の製造方法。A method of manufacturing a magnetic core according to any one of claims 1 to 6,
In the first heat treatment step, the ribbon moves in the temperature rising environment at a speed of 0.1 m / second or more and 1 m / second or less, and thereby the magnetic core is heated at the first temperature rising speed. .
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| PCT/JP2015/069328 WO2016002945A1 (en) | 2014-07-03 | 2015-07-03 | Method for producing magnetic core |
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| JP6862711B2 (en) * | 2016-08-04 | 2021-04-21 | トヨタ自動車株式会社 | Manufacturing method of soft magnetic material |
| US20210310097A1 (en) * | 2017-07-04 | 2021-10-07 | Hitachi Metals, Ltd. | Amorphous alloy ribbon, production method therefor, and amorphous alloy ribbon piece |
| WO2019009311A1 (en) * | 2017-07-04 | 2019-01-10 | 日立金属株式会社 | Tape-wound core, and method for producing tape-wound core |
| CN111910054B (en) * | 2020-08-03 | 2022-10-25 | 东莞理工学院 | Heat treatment method of high-performance iron-based amorphous nanocrystalline strip |
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| JPS59205455A (en) * | 1983-05-07 | 1984-11-21 | Kawasaki Steel Corp | Heat treatment of winding core made of amorphous alloy |
| JPH0196909A (en) * | 1987-10-09 | 1989-04-14 | Mitsui Petrochem Ind Ltd | Saturable inductor and manufacture thereof and pulse laser exciting power source device using saturable inductor |
| JPH03268305A (en) * | 1990-03-16 | 1991-11-29 | Tdk Corp | Manufacture of tape wound core and tape wound core |
| JPH04267314A (en) * | 1991-02-21 | 1992-09-22 | Hitachi Metals Ltd | Wound magnetic core for saturable reactor production method |
| JPH0917623A (en) * | 1995-06-30 | 1997-01-17 | Hitachi Metals Ltd | Nano crystal alloy magnetic core and its manufacture |
| JP2000160241A (en) * | 1998-11-20 | 2000-06-13 | Alps Electric Co Ltd | PRODUCTION OF Fe BASE SOFT MAGNETIC ALLOY |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS59205455A (en) * | 1983-05-07 | 1984-11-21 | Kawasaki Steel Corp | Heat treatment of winding core made of amorphous alloy |
| JPH0196909A (en) * | 1987-10-09 | 1989-04-14 | Mitsui Petrochem Ind Ltd | Saturable inductor and manufacture thereof and pulse laser exciting power source device using saturable inductor |
| JPH03268305A (en) * | 1990-03-16 | 1991-11-29 | Tdk Corp | Manufacture of tape wound core and tape wound core |
| JPH04267314A (en) * | 1991-02-21 | 1992-09-22 | Hitachi Metals Ltd | Wound magnetic core for saturable reactor production method |
| JPH0917623A (en) * | 1995-06-30 | 1997-01-17 | Hitachi Metals Ltd | Nano crystal alloy magnetic core and its manufacture |
| JP2000160241A (en) * | 1998-11-20 | 2000-06-13 | Alps Electric Co Ltd | PRODUCTION OF Fe BASE SOFT MAGNETIC ALLOY |
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| JP6283417B2 (en) | 2018-02-21 |
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