JP7426819B2 - Manufacturing method of magnetic material and coil parts including magnetic material - Google Patents
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- Compounds Of Iron (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Soft Magnetic Materials (AREA)
Description
本発明は、磁性体の製造方法及び磁性体を含むコイル部品に関する。 The present invention relates to a method for manufacturing a magnetic material and a coil component including the magnetic material.
磁性体と巻線とを組み合わせたインダクタ等のコイル部品は、電源回路系機器の電圧変換用に用いられることがある。この場合、コイル部品には、１～１０Ａ程度の直流電流が流される。このため、コイル部品には、電流によるインダクタンス特性の変化が小さいこと、すなわち直流重畳特性に優れることが求められている。直流重畳特性に優れるコイル部品を得る手段としては、磁性体として飽和磁束密度の高いものを使用することが挙げられ、このような磁性体を得るために、材料面からの検討が行われている。 Coil components such as inductors that combine magnetic materials and windings are sometimes used for voltage conversion in power supply circuit equipment. In this case, a direct current of about 1 to 10 A is passed through the coil component. For this reason, coil components are required to have small changes in inductance characteristics due to current, that is, to have excellent DC superimposition characteristics. One way to obtain a coil component with excellent DC superimposition characteristics is to use a magnetic material with a high saturation magnetic flux density, and in order to obtain such a magnetic material, studies are being conducted from the material perspective. .
コイル部品に使用される磁性材料のうち、Ｍｎ－Ｚｎ系フェライトは、飽和磁束密度が高く低損失であるため、直流重畳特性に優れたコイル部品を形成可能なものではある。しかし、電気抵抗率が小さく、使用される電圧に対して電気抵抗が十分に高くないため、コイル部品とする際には、絶縁体を介して巻線をする必要がある。このため、絶縁体の分だけコイル部品の体積が大きくなり、サイズの小さなコイル部品を得ることは困難であった。 Among the magnetic materials used for coil parts, Mn--Zn ferrite has a high saturation magnetic flux density and low loss, so it is possible to form coil parts with excellent DC superimposition characteristics. However, since the electrical resistivity is low and the electrical resistance is not high enough for the voltage used, it is necessary to wind the wire through an insulator when making it into a coil component. For this reason, the volume of the coil component increases by the amount of the insulator, making it difficult to obtain a small-sized coil component.
他方、Ｎｉ－Ｚｎ系フェライトは、絶縁性に優れるため、これを用いた磁性体に直接巻線をすることが可能であり、コイル部品の小型化の点では有利な材料である。しかし、Ｍｎ－Ｚｎ系フェライトに比べて飽和磁束密度が小さく、直流重畳特性に劣る傾向にあるため、これを改善するために種々の検討が行われてきた。 On the other hand, Ni--Zn ferrite has excellent insulating properties, so it is possible to directly wind a magnetic material using it, and it is an advantageous material in terms of miniaturization of coil components. However, compared to Mn--Zn-based ferrite, it has a lower saturation magnetic flux density and tends to have inferior DC superimposition characteristics, so various studies have been conducted to improve this.
例えば、特許文献１では、Ｎｉ－Ｚｎ系フェライトの組成を、酸化マンガン（Ｍｎ２Ｏ３）を含む特定のものとしている。特許文献１には、「ＮｉＣｕＺｎ系フェライトのＦｅ２Ｏ３サイトをＭｎ２Ｏ３で置換することによって、従来のＮｉＣｕＺｎ系フェライトと比較し、飽和磁束密度が高く、低損失でしかも、比抵抗が著しく高い酸化物磁性材料が得られる」（段落［００４８］）との記載がある。 For example, in Patent Document 1, the composition of Ni--Zn-based ferrite is specified to include manganese oxide (Mn 2 O 3 ). Patent Document 1 states, ``By replacing the Fe 2 O 3 site of NiCuZn-based ferrite with Mn 2 O 3 , it has a higher saturation magnetic flux density, lower loss, and lower resistivity than conventional NiCuZn-based ferrite. "A significantly high oxide magnetic material can be obtained" (paragraph [0048]).
また、特許文献２では、特許文献１よりも直流重畳特性を向上させるために、酸化マンガン（ＭｎＯ）を添加して特定の組成範囲に調整した主成分の仮焼粉に、副成分としてケイ酸カルシウム（ＣａＳｉＯ３）及び酸化アンチモン（Ｓｂ２Ｏ３）を添加して、Ｎｉ－Ｚｎ系フェライトを得ている。特許文献２には、「このようなＮｉ－Ｚｎフェライト材料は、マンガンＭｎが添加されていることにより、飽和磁束密度が大きく、直流重畳特性が良好である。」（段落［００５０］）との記載がある。 In addition, in Patent Document 2, in order to improve the DC superimposition characteristics compared to Patent Document 1, manganese oxide (MnO) is added to the main component of calcined powder adjusted to a specific composition range, and silicic acid is added as a subcomponent. Calcium (CaSiO 3 ) and antimony oxide (Sb 2 O 3 ) are added to obtain Ni--Zn ferrite. Patent Document 2 states, "Such a Ni-Zn ferrite material has a large saturation magnetic flux density and good DC superposition characteristics due to the addition of manganese Mn" (paragraph [0050]). There is a description.
しかしながら、特許文献１及び特許文献２（いずれも段落［００５０］）にも記載ないし示唆があるように、Ｎｉ－Ｚｎ系フェライトがＭｎを含むことは、透磁率の低下を引き起こす虞がある。 However, as described or suggested in Patent Document 1 and Patent Document 2 (both paragraph [0050]), the Ni--Zn ferrite containing Mn may cause a decrease in magnetic permeability.
特許文献２では、副成分の添加により、磁性体の飽和磁束密度の増加及びコアロスの減少と共に、比透磁率の増加が確認されている。このことから、特許文献２に記載の手法は、コイル部品の直流重畳特性を向上させつつ、Ｍｎに起因する透磁率の低下を抑制するものといえる。しかし、この手法には、劇物であるＳｂ２Ｏ３を添加物として使用しているためその厳重な管理が必要であること、及び副成分の量が主成分に対して微量であるため均一分散させにくいこと、といった問題があった。 In Patent Document 2, it is confirmed that addition of subcomponents increases the saturation magnetic flux density of the magnetic material, reduces core loss, and increases relative magnetic permeability. From this, it can be said that the method described in Patent Document 2 suppresses the decrease in magnetic permeability caused by Mn while improving the DC superimposition characteristics of the coil component. However, since this method uses Sb 2 O 3 , which is a deleterious substance, as an additive, it requires strict control, and the amount of subcomponents is very small compared to the main component, so it cannot be used uniformly. There was a problem that it was difficult to disperse.
本発明は、前述の問題点を鑑みて為されたものであり、Ｎｉ－Ｚｎ系フェライト材料から作られる磁性体において、該Ｎｉ―Ｚｎ系フェライト材料における主成分以外の添加物を必須成分として含有することなく、直流重畳特性及び透磁率特性に優れたコイル部品を得ることを目的とする。 The present invention has been made in view of the above-mentioned problems, and includes a magnetic material made from a Ni-Zn ferrite material that contains additives other than the main components of the Ni-Zn ferrite material as an essential component. The purpose of the present invention is to obtain a coil component that has excellent DC superimposition characteristics and magnetic permeability characteristics without having to do so.
本発明者は、前述の目的を達成するための検討の過程で、同一組成のＮｉ－Ｚｎ系フェライト材料が得られるように原料を配合した場合であっても、使用する原料の種類によって、得られる磁性体及びこれを用いたコイル部品の特性が異なることを見出した。具体的には、Ｎｉ－Ｚｎ系フェライト材料から作られる磁性体の作製において、Ｍｎを、主原料に対する微小量の添加剤として、別途添加する従来の手法では、分散不良の影響を排除しきれず、必ず、コイル部品の特性に悪影響を与えることを見出した。そして、磁性体の製造に用いる原料として、酸化マンガン等の添加剤の使用に代えて、一定量以上のＭｎを含む酸化鉄粉末を採用すること、及び該酸化鉄粉末中のＭｎ含有量に応じて、適切なＮｉとＺｎのモル比（Ｎｉ／Ｚｎ）となるように原料粉末を配合することで、前述の課題を解決できることを見出し、本発明を完成するに至った。 In the course of studies to achieve the above-mentioned objective, the present inventor discovered that even when raw materials are blended so as to obtain Ni-Zn ferrite materials of the same composition, the yield may vary depending on the type of raw materials used. It was discovered that the characteristics of the magnetic material used in the magnetic material and the coil parts using this material are different. Specifically, in the production of magnetic materials made from Ni-Zn-based ferrite materials, the conventional method of separately adding Mn as a minute additive to the main raw material cannot completely eliminate the effects of poor dispersion. It has been found that this always has an adverse effect on the characteristics of the coil components. Instead of using additives such as manganese oxide, iron oxide powder containing a certain amount or more of Mn is used as a raw material for manufacturing the magnetic material, and depending on the Mn content in the iron oxide powder, Therefore, the inventors discovered that the above-mentioned problems can be solved by blending the raw material powders so that the molar ratio of Ni and Zn (Ni/Zn) is appropriate, and the present invention has been completed.
すなわち、前述の課題を解決するための本発明の一実施形態は、Ｆｅ、Ｎｉ及びＺｎを含むフェライト材料から作られる磁性体の製造方法であって、原料粉末として、Ｍｎ含有量が０．２質量％以上である酸化鉄粉末を用いると共に、
前記酸化鉄粉末中のＭｎ含有量に基づいて、前記フェライト材料中のＺｎに対するＮｉのモル比（Ｎｉ／Ｚｎ）を決定し、該モル比が得られるように前記原料粉末を配合することを特徴とする、磁性体の製造方法である。
That is, one embodiment of the present invention for solving the above-mentioned problems is a method for manufacturing a magnetic material made from a ferrite material containing Fe, Ni, and Zn, in which the raw material powder has a Mn content of 0.2. Using iron oxide powder that is at least % by mass,
Based on the Mn content in the iron oxide powder, a molar ratio of Ni to Zn in the ferrite material (Ni/Zn) is determined, and the raw material powder is blended so that the molar ratio is obtained. This is a method for manufacturing a magnetic material.
本発明によれば、Ｆｅ、Ｎｉ及びＺｎを含むフェライト材料から作られる磁性体において、該フェライト材料における主成分以外の添加物を含有させることなく、直流重畳特性及び透磁率特性に優れたコイル部品を提供することができる。 According to the present invention, in a magnetic body made from a ferrite material containing Fe, Ni, and Zn, a coil component that has excellent DC superimposition characteristics and magnetic permeability characteristics without containing additives other than the main components of the ferrite material. can be provided.
以下、本発明の構成及び作用効果について、技術的思想を交えて説明する。但し、作用機構については推定を含んでおり、その正否は、本発明を制限するものではない。また、以下の実施形態における構成要素のうち、最上位概念を示す独立請求項に記載されていない構成要素については、任意の構成要素として説明される。なお、数値範囲の記載（２つの数値を「～」でつないだ記載）については、下限及び上限として記載された数値をも含む意味である。 Hereinafter, the configuration and effects of the present invention will be explained along with technical ideas. However, the mechanism of action includes speculation, and whether it is correct or not does not limit the present invention. Furthermore, among the constituent elements in the following embodiments, constituent elements that are not described in the independent claims indicating the most significant concept will be described as arbitrary constituent elements. Note that descriptions of numerical ranges (descriptions in which two numerical values are connected by "~") include the numerical values described as the lower limit and upper limit.
本発明の一実施形態において、磁性体を構成するＦｅ、Ｎｉ及びＺｎを含むフェライト材料は、Ｎｉ－Ｚｎ系フェライト材料とも言われる。該フェライト材料は、Ｆｅ、Ｎｉ及びＺｎを主成分として含み、また、多くの場合Ｃｕを成分として含み、場合によっては微量の添加物や不純物を含むことができる組成を有する。本発明の一実施形態に係る、前記フェライト材料から作られる磁性体の製造方法（以下、単に「本実施形態」と記載することがある。）は、原料粉末を準備すること、前記原料粉末を混合して混合粉末とすること、前記混合粉末を熱処理して、Ｆｅ、Ｎｉ及びＺｎを主成分とする仮焼粉末とすること、前記仮焼粉末を成形して成形体とすること、及び前記成形体を焼成して磁性体とすることを含む。本実施形態の第１の特徴は、前記原料粉末として、Ｍｎ含有量が０．２０質量％以上である酸化鉄粉末を用いることである。本実施形態の第２の特徴は、前記酸化鉄粉末中のＭｎ含有量に基づいて、前記フェライト材料中のＺｎに対するＮｉのモル比（Ｎｉ／Ｚｎ）を決定し、該モル比が得られるように前記原料粉末を配合することである。 In one embodiment of the present invention, the ferrite material containing Fe, Ni, and Zn constituting the magnetic body is also referred to as Ni--Zn-based ferrite material. The ferrite material has a composition that contains Fe, Ni, and Zn as main components, often contains Cu as a component, and may contain trace amounts of additives and impurities in some cases. A method for manufacturing a magnetic body made from the ferrite material according to an embodiment of the present invention (hereinafter, sometimes simply referred to as "this embodiment") includes preparing a raw material powder, mixing to form a mixed powder; heat-treating the mixed powder to obtain a calcined powder containing Fe, Ni, and Zn as main components; molding the calcined powder to form a compact; It includes firing the molded body to make it into a magnetic body. The first feature of this embodiment is that iron oxide powder having a Mn content of 0.20% by mass or more is used as the raw material powder. A second feature of the present embodiment is that the molar ratio of Ni to Zn in the ferrite material (Ni/Zn) is determined based on the Mn content in the iron oxide powder, and the molar ratio is determined so that the molar ratio is obtained. The above-mentioned raw material powder is blended into the powder.
本実施形態で原料として使用する酸化鉄粉末は、Ｍｎを、元素換算で０．２０質量％以上含む。酸化鉄中のＭｎの含有量を０．２０質量％以上とすることで、得られた磁性体で構成したコイル部品を、直流重畳特性に優れたものとすることができる。より直流重畳特性に優れたコイル部品を得る点からは、酸化鉄粉末中のＭｎ含有量は、０．３０質量％以上とすることが好ましい。酸化鉄粉末中のＭｎ含有量の上限は特に限定されないが、透磁率に優れた磁性体を得る点からは、０．８５質量％以下とすることが好ましく、０．８０質量％以下とすることがより好ましい。また、前記酸化鉄粉末中のＭｎの含有量を０．８０質量％以下とすることで、より直流重畳特性に優れたコイル部品を得ることもできる。 The iron oxide powder used as a raw material in this embodiment contains 0.20% by mass or more of Mn in terms of element. By setting the content of Mn in iron oxide to 0.20% by mass or more, a coil component made of the obtained magnetic material can have excellent DC superimposition characteristics. In order to obtain a coil component with even better DC superimposition characteristics, the Mn content in the iron oxide powder is preferably 0.30% by mass or more. The upper limit of the Mn content in the iron oxide powder is not particularly limited, but from the viewpoint of obtaining a magnetic material with excellent magnetic permeability, it is preferably 0.85% by mass or less, and 0.80% by mass or less. is more preferable. Further, by controlling the content of Mn in the iron oxide powder to 0.80% by mass or less, a coil component with even better DC superimposition characteristics can be obtained.
本実施形態における、酸化鉄粉末中のＭｎ含有量は、入手した酸化鉄粉末をＩＣＰ発光分光分析法で分析して得られた値をいう。また、入手した酸化鉄粉末にＩＣＰ発光分光分析法、もしくはそれと同等以上の精度の分析手法による分析表が付されている場合には、当該分析表に示された値をそのままＭｎ含有量として採用してもよい。 In this embodiment, the Mn content in the iron oxide powder refers to a value obtained by analyzing the obtained iron oxide powder by ICP emission spectroscopy. In addition, if the obtained iron oxide powder comes with an analysis table based on ICP emission spectroscopy or an analysis method with an accuracy equal to or higher than that, the value shown in the analysis table is used as it is as the Mn content. You may.
本実施形態で使用する酸化鉄以外の原料粉末は、磁性体の必須成分であるニッケル（Ｎｉ）及び亜鉛（Ｚｎ）を含むものであれば特に限定されず、金属単体、合金、又は酸化物を始めとする種々の化合物を使用できる。化合物としては、複合酸化物等の、複数の金属元素を含むものであってもよい。これらのうち、粒子形状及び粒径のバラツキが小さく、粒径の小さな粒子からなる粉末が容易に入手可能な点で、酸化物であるＮｉＯ及びＺｎＯの使用が好ましい。 The raw material powder other than iron oxide used in this embodiment is not particularly limited as long as it contains nickel (Ni) and zinc (Zn), which are essential components of magnetic materials, and may be a single metal, an alloy, or an oxide. A variety of compounds can be used, including: The compound may be one containing multiple metal elements, such as a composite oxide. Among these, the use of NiO and ZnO, which are oxides, is preferable because the variation in particle shape and particle size is small and powder consisting of particles with small particle size is easily available.
前述した各原料粉末の配合比率は、Ｎｉ－Ｚｎ系フェライト材料が得られるものであれば特に限定されない。一例として、Ｎｉ－Ｚｎ系フェライト材料中のＦｅ，Ｚｎ及びＮｉの含有量が、Ｆｅ２Ｏ３、ＺｎＯ、及びＮｉＯ換算で、４７．３～４９．８ｍｏｌ％のＦｅ２Ｏ３、１５．０～３６．９ｍｏｌ％のＺｎＯ、及び１５．０～３６．９ｍｏｌ％のＮｉＯとなるように、各原料粉末を配合することが挙げられる。質量％で表示した原料粉末の配合例としては、Ｎｉ－Ｚｎ系フェライト材料中の前記各成分の含有量が、Ｆｅ２Ｏ３、ＺｎＯ、及びＮｉＯ換算で、６４．４～６７．４質量％のＦｅ２Ｏ３、１０．４～２５．６質量％のＺｎＯ、及び９．４～２３．８質量％のＮｉＯとなるように配合することが挙げられる。原料粉末の配合比率は、製造過程での揮発等による各成分の減少を考慮して、所期の組成のＮｉ－Ｚｎ系フェライト材料が得られるように決定する。製造過程での成分の減少が殆ど無い場合には、得ようとするＮｉ－Ｚｎ系フェライト材料の組成と同一の配合比率とすればよい。なお、一般的には、配合組成と得られたＮｉ－Ｚｎ系フェライト材料の組成にはほとんど差異はない。 The blending ratio of each of the raw material powders described above is not particularly limited as long as a Ni--Zn ferrite material can be obtained. As an example, Fe 2 O 3 and 15.0 mol % of Fe, Zn and Ni in the Ni-Zn ferrite material are 47.3 to 49.8 mol% in terms of Fe 2 O 3 , ZnO and NiO. For example, each raw material powder may be blended so that the ZnO content is ~36.9 mol% and the NiO content is 15.0 ~ 36.9 mol%. As a blending example of the raw material powder expressed in mass %, the content of each of the above components in the Ni-Zn ferrite material is 64.4 to 67.4 mass % in terms of Fe 2 O 3 , ZnO, and NiO. , Fe 2 O 3 of 10.4 to 25.6% by mass, and NiO of 9.4 to 23.8% by mass. The blending ratio of the raw material powder is determined so that a Ni--Zn-based ferrite material having the desired composition can be obtained, taking into account the reduction of each component due to volatilization during the manufacturing process. If there is almost no decrease in the components during the manufacturing process, the blending ratio may be the same as the composition of the Ni--Zn ferrite material to be obtained. Note that, in general, there is almost no difference between the blended composition and the composition of the obtained Ni--Zn-based ferrite material.
本実施形態では、原料として用いる酸化鉄粉末中のＭｎ含有量に基づいて、Ｎｉ－Ｚｎ系フェライト材料中のＺｎに対するＮｉのモル比（Ｎｉ／Ｚｎ）を決定し、該モル比が得られるように前記原料粉末を配合する。具体的には、前記酸化鉄粉末中のＭｎ含有量が多くなるほど、前記モル比（Ｎｉ／Ｚｎ）を小さくする。これは、原料として用いる酸化鉄粉末中のＭｎ含有量が多い場合には、最終的に得られるコイル部品として、直流重畳特性に極めて優れるものが得られる反面、若干ではあるものの透磁率は低下してしまうという、本発明者が新たに知得した事実に基づくものである。Ｎｉ－Ｚｎ系フェライト材料では、Ｎｉ／Ｚｎモル比を小さくすることで、直流重畳特性は若干低下するものの、透磁率を増加させることができるため、これによって前述した透磁率の若干の低下を補償できる。実際にＮｉ－Ｚｎ系フェライト材料におけるＮｉ／Ｚｎモル比を決定するにあたっては、特定組成のＮｉ－Ｚｎ系フェライト材料で構成される磁性体を試作してその特性を測定し、該測定結果を基に組成を変更することを繰り返せばよい。また、事前に測定・収集した組成及び特性のデータベースに基づいてシミュレーションを行うことで、Ｎｉ／Ｚｎモル比を決定してもよい。 In this embodiment, the molar ratio of Ni to Zn in the Ni-Zn ferrite material (Ni/Zn) is determined based on the Mn content in the iron oxide powder used as a raw material, and the molar ratio is determined so as to obtain the molar ratio. The raw material powder is blended into. Specifically, the molar ratio (Ni/Zn) is made smaller as the Mn content in the iron oxide powder increases. This is because when the Mn content in the iron oxide powder used as a raw material is high, the final coil component obtained has extremely excellent DC superimposition characteristics, but on the other hand, the magnetic permeability decreases, albeit slightly. This is based on the fact newly learned by the inventor that In Ni-Zn-based ferrite materials, by reducing the Ni/Zn molar ratio, although the direct current superimposition characteristics decrease slightly, the magnetic permeability can be increased, so this compensates for the slight decrease in magnetic permeability mentioned above. can. To actually determine the Ni/Zn molar ratio in a Ni-Zn ferrite material, a magnetic material made of a Ni-Zn ferrite material with a specific composition is prototyped, its properties are measured, and the measurement results are used as a basis for determining the Ni/Zn molar ratio. All you have to do is repeat changing the composition. Alternatively, the Ni/Zn molar ratio may be determined by performing a simulation based on a database of compositions and properties measured and collected in advance.
前述のようにＮｉ／Ｚｎモル比を小さくすることは、Ｎｉ－Ｚｎ系フェライト材料を製造するための原料粉末における、Ｎｉ含有原料の使用量の低減につながる。ＮｉＯを始めとするＮｉ含有原料は、Ｎｉ－Ｚｎ系フェライト材料の製造に使用する原料粉末の中で、最もコストのかかるものである。このため、Ｎｉ／Ｚｎモル比を小さくすることにより、Ｎｉ－Ｚｎ系フェライト材料及びこれから作られる磁性体の製造コストを低減することもできる。 As described above, reducing the Ni/Zn molar ratio leads to a reduction in the amount of Ni-containing raw material used in the raw material powder for producing the Ni--Zn ferrite material. Ni-containing raw materials such as NiO are the most costly among the raw material powders used in the production of Ni--Zn-based ferrite materials. Therefore, by reducing the Ni/Zn molar ratio, it is also possible to reduce the manufacturing cost of Ni--Zn-based ferrite materials and magnetic bodies made from them.
本実施形態では、原料粉末のひとつに銅（Ｃｕ）を含むことが好ましい。Ｎｉ－Ｚｎ系フェライト材料がＣｕを含むことで、焼成時の焼結性が向上し、磁気特性及び機械的強度に優れた磁性体を得ることができる。原料粉末中のＣｕの含有量は、前述の焼結性向上作用を存分に発揮させる点で、Ｎｉ－Ｚｎ系フェライト材料中のＣｕの含有量がＣｕＯ換算で１ｍｏｌ％以上となるように調整することがより好ましく、３ｍｏｌ％以上となるように調整することがさらに好ましい。他方、焼成時における成形体ないし焼結体の変形を抑制する点で、原料粉末中のＣｕの含有量は、Ｎｉ－Ｚｎ系フェライト材料中のＣｕの含有量がＣｕＯ換算で１３ｍｏｌ％以下となるように調整することがより好ましく、１１ｍｏｌ％以下となるように調整することがさらに好ましい。Ｎｉ－Ｚｎ系フェライト材料がＣｕを含む場合の原料粉末の配合例としては、Ｎｉ－Ｚｎ系フェライト材料中のＦｅ，Ｚｎ、Ｎｉ及びＣｕの含有量が、Ｆｅ２Ｏ３、ＺｎＯ、ＮｉＯ、及びＣｕＯ換算で、４１．６～４９．３ｍｏｌ％のＦｅ２Ｏ３、１３．３～３６．５ｍｏｌ％のＺｎＯ、１３．３～３６．５ｍｏｌ％のＮｉＯ、及び１．０～１２．１ｍｏｌ％のＣｕＯとなるように、各原料粉末を配合することが挙げられる。質量％で表示した原料粉末の配合例としては、Ｎｉ－Ｚｎ系フェライト材料中の前記各成分の含有量が、Ｆｅ２Ｏ３、ＺｎＯ、ＮｉＯ及びＣｕＯ換算で、５８．９～６６．９質量％のＦｅ２Ｏ３、９．５～２５．４質量％のＺｎＯ、８．６～２３．６質量％のＮｉＯ、及び０．６～８．６質量％のＣｕＯとなるように配合することが挙げられる。前述したＣｕ含有量（ＣｕＯ換算）は、２質量％以上とすることがより好ましく、また８質量％以下とすることがより好ましい。 In this embodiment, it is preferable that one of the raw material powders contains copper (Cu). When the Ni--Zn-based ferrite material contains Cu, the sinterability during firing is improved, and a magnetic material with excellent magnetic properties and mechanical strength can be obtained. The content of Cu in the raw material powder is adjusted so that the content of Cu in the Ni-Zn ferrite material is 1 mol% or more in terms of CuO, in order to fully exhibit the aforementioned sinterability improvement effect. It is more preferable to adjust the amount to 3 mol% or more. On the other hand, in terms of suppressing the deformation of the compact or sintered body during firing, the content of Cu in the raw material powder is such that the content of Cu in the Ni-Zn ferrite material is 13 mol% or less in terms of CuO. It is more preferable to adjust it so that it becomes 11 mol% or less, and even more preferably to adjust it so that it becomes 11 mol% or less. As a blending example of the raw material powder when the Ni-Zn ferrite material contains Cu, the content of Fe, Zn, Ni and Cu in the Ni-Zn ferrite material is Fe 2 O 3 , ZnO, NiO, and In terms of CuO, 41.6 to 49.3 mol% of Fe 2 O 3 , 13.3 to 36.5 mol% of ZnO, 13.3 to 36.5 mol% of NiO, and 1.0 to 12.1 mol% of For example, each raw material powder may be blended so as to form CuO. As a blending example of the raw material powder expressed in mass %, the content of each of the above components in the Ni-Zn ferrite material is 58.9 to 66.9 mass in terms of Fe 2 O 3 , ZnO, NiO, and CuO. % Fe 2 O 3 , 9.5 to 25.4 mass % ZnO, 8.6 to 23.6 mass % NiO, and 0.6 to 8.6 mass % CuO. can be mentioned. The aforementioned Cu content (CuO equivalent) is more preferably 2% by mass or more, and more preferably 8% by mass or less.
Ｃｕを含む原料粉末としては特に限定されず、金属銅、銅合金、又は酸化物を始めとする種々の化合物を使用できる。化合物としては、複合酸化物等の、Ｃｕ以外の金属元素を含むものであってもよい。これらのうち、粒子形状及び粒径のバラツキが小さく、粒径の小さな粒子からなる粉末が容易に入手可能な点で、酸化物であるＣｕＯの使用が好ましい。 The raw material powder containing Cu is not particularly limited, and various compounds including metallic copper, copper alloys, or oxides can be used. The compound may include a metal element other than Cu, such as a composite oxide. Among these, it is preferable to use CuO, which is an oxide, because the variation in particle shape and particle size is small, and powder consisting of particles with small particle size is easily available.
本実施形態では、原料粉末ないし磁性体中に、不可避不純物を数百ｐｐｍ程度まで含むことが許容される。
不可避不純物の例としては、Ｂ、Ｃ、Ｓ、Ｃｌ、Ｓｅ、Ｂｒ、Ｔｅ、Ｉや、Ｌｉ、Ｎａ、Ｍｇ、Ａｌ、Ｋ、Ｇａ、Ｇｅ、Ｓｒ、Ｉｎ、Ｓｎ、Ｓｂ、Ｂａ、Ｐｂ、Ｂｉ等の典型元素、並びにＳｃ、Ｔｉ、Ｖ、Ｃｒ、Ｙ、Ｎｂ、Ｍｏ、Ｐｄ、Ａｇ、Ｃｄ、Ｈｆ、Ｔａ等の遷移元素が挙げられる。
In this embodiment, it is allowed that the raw material powder or the magnetic material contains unavoidable impurities up to several hundred ppm.
Examples of unavoidable impurities include B, C, S, Cl, Se, Br, Te, I, Li, Na, Mg, Al, K, Ga, Ge, Sr, In, Sn, Sb, Ba, Pb, Examples include typical elements such as Bi, and transition elements such as Sc, Ti, V, Cr, Y, Nb, Mo, Pd, Ag, Cd, Hf, and Ta.
本実施形態は、前述した主成分以外の添加物を用いなくとも、直流重畳特性に優れたコイル部品を提供することができるものではあるが、さらに高性能のコイル部品を得るために、Ｎｉ－Ｚｎ系フェライト材料に対して種々の副成分を添加して磁性体を製造してもよい。 Although this embodiment can provide a coil component with excellent DC superimposition characteristics without using any additives other than the above-mentioned main components, in order to obtain a coil component with even higher performance, Ni- The magnetic material may be manufactured by adding various subcomponents to the Zn-based ferrite material.
本実施形態では、原料粉末の混合方法は、不純物の混入を防ぎつつ各粉末が均一に混合されるものであれば特に限定されず、乾式混合、湿式混合のいずれを採用してもよい。ボールミルを用いた湿式混合を採用する場合には、例えば８～２４時間程度混合すればよい。 In the present embodiment, the method of mixing the raw material powders is not particularly limited as long as each powder is mixed uniformly while preventing contamination of impurities, and either dry mixing or wet mixing may be used. When wet mixing using a ball mill is employed, mixing may be carried out for about 8 to 24 hours, for example.
混合粉末の熱処理条件は、各原料が反応して所期の組成を有するＮｉ－Ｚｎ系フェライトの仮焼粉（Ｎｉ－Ｚｎ系フェライト材料）が得られるものであれば限定されず、例えば大気雰囲気中、８００℃～１０００℃で１時間～３時間とすればよい。焼成温度が低すぎたり、焼成時間が短すぎたりすると、未反応の原料や中間生成物が残存する虞がある。反対に、焼成温度が高すぎたり、焼成時間が長すぎたりすると、成分の揮発により所期の組成の化合物が得られない虞や、生成物が固結して解砕しにくくなることで生産性が低下する虞がある。 The heat treatment conditions for the mixed powder are not limited as long as each raw material reacts and a calcined powder of Ni-Zn ferrite (Ni-Zn ferrite material) having the desired composition can be obtained. The temperature may be set at 800°C to 1000°C for 1 to 3 hours. If the firing temperature is too low or the firing time is too short, unreacted raw materials and intermediate products may remain. On the other hand, if the firing temperature is too high or the firing time is too long, there is a risk that a compound with the desired composition will not be obtained due to volatilization of the ingredients, or the product will solidify and become difficult to crush, resulting in production problems. There is a risk that the performance may deteriorate.
本実施形態では、前述の熱処理により得られた仮焼粉末が凝集している場合、成形に先立ってこれを解砕することが好ましい。解砕は、仮焼粉末の凝集をくずして適度の焼結性を有する粉体とするために行われる。解砕は、振動ミル、ハンマーミル、ローラーミル等を用いて乾式で行ってもよいが、仮焼粉末が大きい塊を形成しているときには、粗粉砕を行ってからボールミルやアトライター等を用いて湿式にて行うことが好ましい。解砕は、仮焼粉末の平均粒径が、０．５μｍ～２μｍ程度となるまで行うことが、成形性、保形性及び焼結性の点で好ましい。 In this embodiment, if the calcined powder obtained by the above-described heat treatment is aggregated, it is preferable to crush this prior to molding. Crushing is performed to break the agglomeration of the calcined powder to obtain a powder having appropriate sinterability. Disintegration may be carried out dry using a vibrating mill, hammer mill, roller mill, etc., but if the calcined powder has formed large lumps, it may be performed by coarsely pulverizing it and then using a ball mill, attritor, etc. It is preferable to carry out the wet process. It is preferable to carry out crushing until the average particle size of the calcined powder becomes approximately 0.5 μm to 2 μm from the viewpoint of formability, shape retention, and sinterability.
本実施形態では、仮焼粉末の成形に先立って、当該仮焼粉末の造粒を行って、造粒物（顆粒）を得てもよい。造粒は、粉砕材料を適度な大きさの凝集粒子とし、成形に適した形態に変換するために行われる。こうした造粒法としては、例えば、加圧造粒法やスプレードライ法等が挙げられる。 In this embodiment, prior to molding of the calcined powder, the calcined powder may be granulated to obtain a granulated product (granules). Granulation is performed to convert the pulverized material into agglomerated particles of appropriate size and into a form suitable for molding. Examples of such granulation methods include pressure granulation methods and spray drying methods.
本実施形態では、このようにして得られた仮焼粉末を所定形状に成形し、成形体を得る。成形方法としては特に限定されず、一例として、粉末の一軸加圧成形、粉末を含む坏土の押出成形及び粉末を分散したスラリーの鋳込成形等が挙げられる。成形体の形状も特に限定されず、棒状、板状、トロイダル状、ドラム型等の公知の形状から、用途に応じて適宜選択すればよい。 In this embodiment, the calcined powder thus obtained is molded into a predetermined shape to obtain a molded body. The molding method is not particularly limited, and examples include uniaxial pressure molding of powder, extrusion molding of clay containing powder, and casting molding of slurry in which powder is dispersed. The shape of the molded body is not particularly limited either, and may be appropriately selected from known shapes such as rod, plate, toroidal, and drum shapes depending on the purpose.
本実施形態では、このようにして得られた成形体を焼成して磁性体とする。これにより、成形体に含まれる粉体粒子同士が焼結し、緻密な焼結体となる。焼成条件は、緻密な磁性体が得られるものであれば限定されず、例えば、大気雰囲気中、９００～１２００℃の温度で、１～５時間程度とすればよい。焼成温度が低すぎたり、焼成時間が短すぎたりすると、緻密化が不十分であることにより、所期の特性の磁性体が得られない虞がある。反対に、焼成温度が高すぎたり、焼成時間が長すぎたりすると、成分の揮発により組成ずれが生じる虞や、粗大粒子の生成により特性が低下する虞がある。なお、焼成は、大気中よりも酸素分圧が高い雰囲気で行ってもよい。 In this embodiment, the molded body thus obtained is fired to form a magnetic body. As a result, the powder particles contained in the molded body are sintered together to form a dense sintered body. The firing conditions are not limited as long as a dense magnetic material can be obtained, and may be, for example, in the air at a temperature of 900 to 1200° C. for about 1 to 5 hours. If the firing temperature is too low or the firing time is too short, densification may be insufficient and a magnetic material with desired characteristics may not be obtained. On the other hand, if the firing temperature is too high or the firing time is too long, there is a risk that the composition will shift due to volatilization of the components, or that the properties will deteriorate due to the formation of coarse particles. Note that the firing may be performed in an atmosphere where the oxygen partial pressure is higher than that in the atmosphere.
本実施形態に係る製造方法で得られた磁性体は、導体を巻回されてコイル部品となる。このコイル部品は、Ｍｎ含有量が所期の範囲外である酸化鉄粉末を原料とした、同組成の磁性体で形成されたものに比べて、比透磁率が大きく、直流重畳特性に優れたものとなる。 The magnetic material obtained by the manufacturing method according to the present embodiment is wound with a conductor to form a coil component. This coil component has a higher relative magnetic permeability and excellent DC superimposition characteristics than those made of a magnetic material with the same composition made from iron oxide powder whose Mn content is outside the expected range. Become something.
以下、実施例により本発明をさらに具体的に説明するが、本発明は該実施例に限定されるものではない。 EXAMPLES Hereinafter, the present invention will be explained in more detail with reference to Examples, but the present invention is not limited to these Examples.
［実施例１］
＜磁性体及びコイル部品の作製＞
まず、原料粉末として、Ｍｎを０．３０質量％含有するＦｅ２Ｏ３、ＺｎＯ、ＣｕＯ及びＮｉＯの各粉末を準備した。次いで、これらの原料粉末を、Ｆｅ２Ｏ３が６６．２質量％（４９ｍｏｌ％）、ＺｎＯが１５．８質量％（２３ｍｏｌ％）、ＣｕＯが４．７質量％（７ｍｏｌ％）、及びＮｉＯが１３．３質量％（２１ｍｏｌ％）（ＮｉとＺｎの合計が４４ｍｏｌ％でＮｉ／Ｚｎモル比：０．９１３）となるように秤量し、湿式ミルにて混合した。次いで、分散媒を蒸発させて除去して得た混合粉末を、大気雰囲気中、８００℃で２時間熱処理して仮焼粉末を得た。次いで、得られた仮焼粉末を、ＢＥＴ比表面積が２．０～３．０ｍ２／ｇの範囲となるように解砕した。次いで、解砕後の仮焼粉末に分散媒としての蒸留水及びバインダとしてＰＶＡ（ポリビニルアルコール）を添加し、スプレードライヤーにて噴霧乾燥して造粒粉を得た。次いで、得られた造粒粉を金型内に供給し、１０ＭＰａの圧力で一軸圧縮成形してトロイダル形状の成形体を得た。次いで、得られた成形体を大気雰囲気中、１１００℃にて１時間焼成し、外形２５ｍｍ×内径１２ｍｍ×厚み１５ｍｍの磁性体を得た。最後に、得られた磁性体に導線を２０ターン巻回して、実施例１に係るコイル部品を得た。
[Example 1]
<Production of magnetic material and coil parts>
First, powders of Fe 2 O 3 , ZnO, CuO, and NiO containing 0.30% by mass of Mn were prepared as raw material powders. Next, these raw material powders were mixed with 66.2 mass% (49 mol%) of Fe2O3 , 15.8 mass% (23 mol%) of ZnO , 4.7 mass% (7 mol%) of CuO, and 4.7 mass% (7 mol%) of NiO. It was weighed out to be 13.3% by mass (21 mol%) (total of Ni and Zn is 44 mol%, Ni/Zn molar ratio: 0.913) and mixed in a wet mill. Next, the mixed powder obtained by evaporating and removing the dispersion medium was heat-treated at 800° C. for 2 hours in the air to obtain a calcined powder. Next, the obtained calcined powder was crushed so that the BET specific surface area was in the range of 2.0 to 3.0 m 2 /g. Next, distilled water as a dispersion medium and PVA (polyvinyl alcohol) as a binder were added to the crushed calcined powder, and the mixture was spray-dried with a spray dryer to obtain granulated powder. Next, the obtained granulated powder was supplied into a mold and subjected to uniaxial compression molding at a pressure of 10 MPa to obtain a toroidal shaped molded body. Next, the obtained molded body was fired in an air atmosphere at 1100° C. for 1 hour to obtain a magnetic body having an outer diameter of 25 mm, an inner diameter of 12 mm, and a thickness of 15 mm. Finally, a conducting wire was wound 20 turns around the obtained magnetic material to obtain a coil component according to Example 1.
＜透磁率の測定＞
得られたコイル部品について、測定装置としてインピーダンスアナライザ（キーサイト・テクノロジーズ・インク製、Ｅ４９９０Ａ）を用い、室温にて、ＯＳＣレベル５００ｍＶ、周波数１ＭＨｚの条件で、比透磁率の測定を行った。得られた比透磁率は４５１であった。
<Measurement of magnetic permeability>
The relative magnetic permeability of the obtained coil components was measured at room temperature using an impedance analyzer (manufactured by Keysight Technologies, Inc., E4990A) as a measuring device under the conditions of an OSC level of 500 mV and a frequency of 1 MHz. The relative magnetic permeability obtained was 451.
＜直流重畳特性及びインダクタンスの温度依存性の測定＞
前述のコイル部品について、ＬＣＲメーター（キーサイト・テクノロジーズ・インク製、Ｅ４９８０Ａ）を用い、室温にて、ＯＳＣレベル２０ｍＡ、周波数１００ｋＨｚの条件で、電流を０Ａから徐々に増加させながらインダクタンス測定を行った。そして、インダクタンスが電流０Ａの状態から３０％低下した際の電流値を、直流重畳特性とした。この電流値が大きいほど、直流重畳特性に優れたコイル部品といえる。得られた直流重畳特性は、５３６ｍＡであった。
また、同装置を用い、電流を０Ａとした状態で、コイル部品の温度を室温（２５℃）から１５０℃まで昇温してインダクタンスを測定した。そして、室温から１５０℃までのインダクタンスの変化率（（Ｌ１５０℃－Ｌ２５℃）／Ｌ２５℃×１００％）を、インダクタンスの温度依存性とした。ここで、Ｌ２５℃は室温（２５℃）でのインダクタンスの測定値を、Ｌ１５０℃は１５０℃でのインダクタンスの測定値を、それぞれ意味する。得られたインダクタンスの温度依存性は、７２％であった。
<Measurement of DC superposition characteristics and temperature dependence of inductance>
Regarding the above-mentioned coil components, inductance was measured using an LCR meter (manufactured by Keysight Technologies, Inc., E4980A) at room temperature under the conditions of an OSC level of 20 mA and a frequency of 100 kHz while gradually increasing the current from 0 A. . Then, the current value when the inductance decreased by 30% from the current 0A state was defined as the DC superposition characteristic. The larger the current value, the better the coil component has direct current superimposition characteristics. The obtained DC superposition characteristic was 536 mA.
Further, using the same device, the inductance was measured while the temperature of the coil component was raised from room temperature (25° C.) to 150° C. while the current was set to 0 A. Then, the rate of change in inductance from room temperature to 150°C ((L 150°C - L 25°C )/L 25°C × 100%) was defined as the temperature dependence of inductance. Here, L 25°C means a measured value of inductance at room temperature (25°C), and L 150°C means a measured value of inductance at 150°C. The temperature dependence of the obtained inductance was 72%.
以上の結果を、後述する他の実施例及び比較例の結果と合わせて、表１に示す。 The above results are shown in Table 1 together with the results of other Examples and Comparative Examples described later.
［実施例２、３］
原料として使用するＦｅ２Ｏ３粉末をそれぞれ、Ｍｎ含有量が０．６０質量％のもの（実施例２）及び０．８０質量％（実施例３）のものに変更すると共に、Ｎｉ－Ｚｎ系フェライト材料のＮｉとＺｎの合計の４４ｍｏｌ％は実施例１と同様のままでＮｉ／Ｚｎモル比がそれぞれ０．９０（実施例２）及び０．８９（実施例３）となるように原料粉末の配合割合を変更した以外は実施例１と同様の手順にて、実施例２、３に係るコイル部品をそれぞれ作製した。実際の配合では、実施例２はＺｎＯを１５．９質量％、及びＮｉＯを１３．２質量％とし、実施例３はＺｎＯを１６．０質量％、及びＮｉＯを１３．１質量％とした。
得られたコイル部品について、実施例１と同様の方法で透磁率、直流重畳特性及びインダクタンスの温度依存性を測定した。その結果、実施例２に係るコイル部品では、比透磁率が４５１、直流重畳特性が５３５ｍＡ、インダクタンスの温度依存性が８５％となった。また、実施例３に係るコイル部品では、比透磁率が４５２、直流重畳特性が５１７ｍＡ、インダクタンスの温度依存性が７５％となった。これらの結果をまとめて後掲の表１に示す。
[Example 2, 3]
The Fe 2 O 3 powder used as a raw material was changed to one with a Mn content of 0.60% by mass (Example 2) and 0.80% by mass (Example 3), respectively, and Ni-Zn-based The total 44 mol% of Ni and Zn in the ferrite material remained the same as in Example 1, and the raw material powder was adjusted so that the Ni/Zn molar ratio was 0.90 (Example 2) and 0.89 (Example 3), respectively. Coil parts according to Examples 2 and 3 were respectively produced in the same manner as in Example 1 except that the blending ratio was changed. In the actual formulation, Example 2 contained 15.9% by mass of ZnO and 13.2% by mass of NiO, and Example 3 contained 16.0% by mass of ZnO and 13.1% by mass of NiO.
Regarding the obtained coil component, magnetic permeability, DC superimposition characteristics, and temperature dependence of inductance were measured in the same manner as in Example 1. As a result, the coil component according to Example 2 had a relative magnetic permeability of 451, a DC superimposition characteristic of 535 mA, and an inductance temperature dependence of 85%. Further, in the coil component according to Example 3, the relative magnetic permeability was 452, the DC superposition characteristic was 517 mA, and the temperature dependence of inductance was 75%. These results are summarized in Table 1 below.
［比較例１～３］
原料として使用するＦｅ２Ｏ３粉末を、Ｍｎ含有量が０．１５質量％のものに変更すると共に、Ｎｉ－Ｚｎ系フェライト材料のＮｉとＺｎの合計の４４ｍｏｌ％は実施例１と同様のままでＮｉ／Ｚｎモル比がそれぞれ０．９２（比較例１）、０．９０（比較例２）及び０．８９（比較例３）となるように原料粉末の配合割合を変更した以外は実施例１と同様の手順にて、比較例１～３に係るコイル部品をそれぞれ作製した。実際の配合では、比較例１はＺｎＯを１５．８質量％、及びＮｉＯを１３．３質量％とし、比較例２はＺｎＯを１５．９質量％、及びＮｉＯを１３．２質量％とし、比較例３はＺｎＯを１６．０質量％、及びＮｉＯを１３．１質量％とした。
一般的にＮｉ－Ｚｎ系フェライト材料の合成に用いられる、電子部品用途のＦｅ２Ｏ３原料粉末には、Ｍｎ含有量の極力少ないものが用いられる。これは、Ｍｎが、Ｍｎ－Ｚｎ系フェライトを生成して部分的な絶縁抵抗率の低下を招く有害成分と考えられていることによる。こうしたＦｅ２Ｏ３原料粉末は、理論的には、Ｍｎ含有量が０．００１質量％未満という、Ｍｎがほとんど含有されていない水準にまで純度を向上することもできるが、実際の製造に用いる場合には、コスト等を勘案して、Ｍｎ含有量が０．１５質量％程度のものが用いられている。このため、ここで説明する比較例１～３並びに後述する比較例４～６では、Ｆｅ２Ｏ３原料粉として、このＭｎ含有量０．１５質量％のものを用いた。得られたコイル部品について、実施例１と同様の方法で透磁率、直流重畳特性及びインダクタンスの温度依存性を測定した。その結果、比較例１に係るコイル部品では、比透磁率が４５１、インダクタンスの温度変化率が６４％となり、前述の各実施例と同程度の値が得られたが、直流重畳特性は５００ｍＡとなり、前述の各実施例よりも低下した。比較例２、３でも同様の傾向が確認され、比較例２では、比透磁率が４５７、インダクタンスの温度変化率が６９％、直流重畳特性が４９２となり、比較例３では、比透磁率が４６５、インダクタンスの温度変化率が７２％、直流重畳特性が４８４となった。これらの結果をまとめて後掲の表１に示す。
[Comparative Examples 1 to 3]
The Fe 2 O 3 powder used as a raw material was changed to one with a Mn content of 0.15% by mass, and the total 44 mol% of Ni and Zn in the Ni-Zn ferrite material remained the same as in Example 1. Example except that the mixing ratio of the raw material powder was changed so that the Ni/Zn molar ratio was 0.92 (Comparative Example 1), 0.90 (Comparative Example 2), and 0.89 (Comparative Example 3), respectively. Coil parts according to Comparative Examples 1 to 3 were each manufactured in the same manner as in Example 1. In the actual formulation, Comparative Example 1 contains 15.8% by mass of ZnO and 13.3% by mass of NiO, and Comparative Example 2 contains 15.9% by mass of ZnO and 13.2% by mass of NiO. Example 3 contained 16.0% by mass of ZnO and 13.1% by mass of NiO.
Fe 2 O 3 raw material powder for electronic parts, which is generally used in the synthesis of Ni--Zn-based ferrite materials, has a minimal Mn content. This is because Mn is considered to be a harmful component that produces Mn--Zn ferrite and causes a partial decrease in insulation resistivity. Theoretically, the purity of such Fe 2 O 3 raw material powder can be improved to a level where the Mn content is less than 0.001% by mass, which is almost no Mn. In some cases, a material with a Mn content of about 0.15% by mass is used in consideration of cost and the like. Therefore, in Comparative Examples 1 to 3 described here and Comparative Examples 4 to 6 described later, this Fe 2 O 3 raw material powder with a Mn content of 0.15% by mass was used. Regarding the obtained coil component, magnetic permeability, DC superimposition characteristics, and temperature dependence of inductance were measured in the same manner as in Example 1. As a result, the coil component according to Comparative Example 1 had a relative magnetic permeability of 451 and a temperature change rate of inductance of 64%, which were comparable to those of the above-mentioned examples, but the DC superposition characteristic was 500 mA. , which was lower than each of the above-mentioned examples. Similar trends were confirmed in Comparative Examples 2 and 3. In Comparative Example 2, the relative magnetic permeability was 457, the temperature change rate of inductance was 69%, and the DC superimposition characteristic was 492, and in Comparative Example 3, the relative magnetic permeability was 465. , the temperature change rate of inductance was 72%, and the DC superposition characteristic was 484. These results are summarized in Table 1 below.
以下に説明する比較例４～６では、添加剤としての酸化マンガン（Ｍｎ３Ｏ４）を使用した場合には、Ｎｉ－Ｚｎ系フェライト材料中のＭｎ含有量が前述の実施例と同一であっても、Ｎｉ／Ｚｎモル比の調整により優れた直流重畳特性と高透磁率とを両立させることはできないことを確認した。 In Comparative Examples 4 to 6 described below, when manganese oxide (Mn 3 O 4 ) was used as an additive, the Mn content in the Ni-Zn ferrite material was the same as in the above-mentioned examples. However, it was confirmed that it was not possible to achieve both excellent DC superimposition characteristics and high magnetic permeability by adjusting the Ni/Zn molar ratio.
［比較例４］
以下の点を除き実施例１と同様の手順にて、比較例４に係るコイル部品を作成した。原料として使用するＦｅ２Ｏ３粉末を、Ｍｎ含有量が０．１５質量％のものに変更した。また、原料粉末に、添加剤としてさらにＭｎ３Ｏ４粉末を使用して、混合粉末ないしＮｉ－Ｚｎ系フェライト材料中に含まれるＭｎの総量を、前述したＦｅ２Ｏ３粉末の変更前（実施例１）の量に一致させた。さらに、コイル部品の比透磁率が実施例１に係るコイル部品と同程度となるように、Ｎｉ－Ｚｎ系フェライト材料のＮｉとＺｎの合計の４４ｍｏｌ％は実施例１と同様のままでＮｉ／Ｚｎモル比を０．８６とした。実際の配合では、ＺｎＯを１６．３質量％、及びＮｉＯを１２．９質量％とした。
得られたコイル部品について、実施例１と同様の方法で透磁率、直流重畳特性及びインダクタンスの温度依存性を測定したところ、比透磁率は４５２であったが、直流重畳特性は４５０ｍＡまで、インダクタンスの温度依存性は１２１％まで、それぞれ悪化した。
[Comparative example 4]
A coil component according to Comparative Example 4 was created in the same manner as in Example 1 except for the following points. The Fe 2 O 3 powder used as a raw material was changed to one with a Mn content of 0.15% by mass. In addition, by using Mn 3 O 4 powder as an additive in the raw material powder, the total amount of Mn contained in the mixed powder or Ni-Zn ferrite material can be adjusted as described above before changing the Fe 2 O 3 powder (implemented). The amounts corresponded to those in Example 1). Furthermore, in order to make the relative magnetic permeability of the coil component similar to that of the coil component according to Example 1, 44 mol% of the total of Ni and Zn in the Ni-Zn-based ferrite material remained the same as in Example 1, and Ni/ The Zn molar ratio was set to 0.86. In the actual formulation, ZnO was 16.3% by mass and NiO was 12.9% by mass.
Regarding the obtained coil component, the temperature dependence of magnetic permeability, DC superposition characteristics, and inductance was measured in the same manner as in Example 1. The relative permeability was 452, but the DC superposition characteristics were up to 450 mA, and the inductance The temperature dependence of was worsened to 121%.
［比較例５］
以下の点を除き実施例２と同様の手順にて、比較例５に係るコイル部品を作成した。原料として使用するＦｅ２Ｏ３粉末を、Ｍｎ含有量が０．１５質量％のものに変更した。また、原料粉末に、添加剤としてさらにＭｎ３Ｏ４粉末を使用して、混合粉末ないしＮｉ－Ｚｎ系フェライト材料中に含まれるＭｎの総量を、前述したＦｅ２Ｏ３粉末の変更前（実施例２）の量に一致させた。さらに、コイル部品の比透磁率が実施例２に係るコイル部品と同程度になるように、Ｎｉ－Ｚｎ系フェライト材料のＮｉとＺｎの合計の４４ｍｏｌ％は実施例１と同様のままでＮｉ／Ｚｎモル比を０．８２とした。実際の配合では、ＺｎＯを１６．６質量％、及びＮｉＯを１２．５質量％とした。
得られたコイル部品について、実施例１と同様の方法で透磁率、直流重畳特性及びインダクタンスの温度依存性を測定したところ、比透磁率は４５０であったが、直流重畳特性は４３０ｍＡまで、インダクタンスの温度依存性は１７４％までそれぞれ悪化した。
[Comparative example 5]
A coil component according to Comparative Example 5 was created in the same manner as in Example 2 except for the following points. The Fe 2 O 3 powder used as a raw material was changed to one with a Mn content of 0.15% by mass. In addition, by using Mn 3 O 4 powder as an additive in the raw material powder, the total amount of Mn contained in the mixed powder or Ni-Zn ferrite material can be adjusted as described above before changing the Fe 2 O 3 powder (implemented). The amount corresponded to that of Example 2). Furthermore, in order to make the relative magnetic permeability of the coil component comparable to that of the coil component according to Example 2, the total 44 mol% of Ni and Zn in the Ni-Zn-based ferrite material remained the same as in Example 1, and Ni/ The Zn molar ratio was set to 0.82. In the actual formulation, ZnO was 16.6% by mass and NiO was 12.5% by mass.
Regarding the obtained coil component, the temperature dependence of magnetic permeability, DC bias characteristics, and inductance was measured in the same manner as in Example 1. The relative permeability was 450, but the DC bias characteristics were up to 430 mA, and the inductance was The temperature dependence of the values worsened to 174%.
［比較例６］
以下の点を除き実施例３と同様の手順にて、比較例６に係るコイル部品を作成した。原料として使用するＦｅ２Ｏ３粉末を、Ｍｎ含有量が０．１５質量％のものに変更した。また、原料粉末に、添加剤としてさらにＭｎ３Ｏ４粉末を使用して、混合粉末ないしＮｉ－Ｚｎ系フェライト材料中に含まれるＭｎの総量を、前述したＦｅ２Ｏ３粉末の変更前（実施例３）の量に一致させた。さらに、コイル部品の比透磁率が実施例３に係るコイル部品に近づくように、Ｎｉ－Ｚｎ系フェライト材料のＮｉとＺｎの合計の４４ｍｏｌ％は実施例１と同様のままでＮｉ／Ｚｎモル比を０．８０まで低減した。実際の配合では、ＺｎＯを１６．８質量％、及びＮｉＯを１２．３質量％とした。
得られたコイル部品について、実施例１と同様の方法で透磁率、直流重畳特性及びインダクタンスの温度依存性を測定した。その結果、比透磁率は４３５に留まった。このとき、直流重畳特性は４０１ｍＡまで、インダクタンスの温度依存性は１８８％までそれぞれ悪化した。
比較例４～６の結果を、上述の実施例及び比較例と合わせて表１に示す。
[Comparative example 6]
A coil component according to Comparative Example 6 was created in the same manner as in Example 3 except for the following points. The Fe 2 O 3 powder used as a raw material was changed to one with a Mn content of 0.15% by mass. In addition, by using Mn 3 O 4 powder as an additive in the raw material powder, the total amount of Mn contained in the mixed powder or Ni-Zn ferrite material can be adjusted as described above before changing the Fe 2 O 3 powder (implemented). The amount corresponded to Example 3). Furthermore, in order to make the relative magnetic permeability of the coil component approach that of the coil component according to Example 3, the Ni/Zn molar ratio was changed while keeping the total of Ni and Zn in the Ni-Zn ferrite material at 44 mol% as in Example 1. was reduced to 0.80. In the actual formulation, ZnO was 16.8% by mass and NiO was 12.3% by mass.
Regarding the obtained coil component, magnetic permeability, DC superimposition characteristics, and temperature dependence of inductance were measured in the same manner as in Example 1. As a result, the relative magnetic permeability remained at 435. At this time, the DC superposition characteristic deteriorated to 401 mA, and the temperature dependence of inductance deteriorated to 188%.
The results of Comparative Examples 4 to 6 are shown in Table 1 together with the above-mentioned Examples and Comparative Examples.
実施例１～３と比較例１～３との対比からは、所期の量のＭｎを含むＦｅ２Ｏ３粉末を原料として使用した実施例１～３に係るコイル部品は、一般的なＮｉ－Ｚｎ系フェライト材料の工業的な合成に用いられる、Ｍｎ含有量の少ないＦｅ２Ｏ３粉末を原料として使用した比較例１～３に係るものとは異なり、Ｎｉ－Ｚｎ系フェライト材料のＮｉ／Ｚｎモル比の調整により、優れた直流重畳特性と比透磁率とが両立可能であることが判る。比較例１～３の結果からは、Ｍｎ含有量の少ないＦｅ２Ｏ３粉末を原料として使用した場合には、Ｎｉ－Ｚｎ系フェライト材料のＮｉ／Ｚｎモル比の調整のみでは、比透磁率を保持しつつ直流重畳特性に優れたコイル部品を製造することはできないことが判る。また、本実施例のようにＮｉ／Ｚｎモル比の調整することで、高価な原料であるＮｉＯの使用量を少なくでき、原料コストを抑えることができる。 A comparison between Examples 1 to 3 and Comparative Examples 1 to 3 shows that the coil parts of Examples 1 to 3, which used Fe 2 O 3 powder containing a desired amount of Mn as a raw material, - Unlike Comparative Examples 1 to 3, which used Fe 2 O 3 powder with low Mn content as a raw material, which is used for the industrial synthesis of Zn-based ferrite materials, the Ni/Zn-based ferrite materials It can be seen that by adjusting the Zn molar ratio, it is possible to achieve both excellent DC superimposition characteristics and relative magnetic permeability. The results of Comparative Examples 1 to 3 show that when Fe 2 O 3 powder with a low Mn content is used as a raw material, adjusting the Ni/Zn molar ratio of the Ni-Zn ferrite material alone will not increase the relative permeability. It is clear that it is not possible to manufacture a coil component with excellent DC superimposition characteristics while maintaining the same characteristics. Furthermore, by adjusting the Ni/Zn molar ratio as in this example, the amount of NiO, which is an expensive raw material, used can be reduced, and raw material costs can be suppressed.
また、実施例１と比較例４との対比、実施例２と比較例５との対比、及び実施例３と比較例６との対比からは、所期の量のＭｎを含むＦｅ２Ｏ３粉末を原料として使用した以外に別途Ｍｎを添加していない実施例に係るコイル部品は、一般的なＮｉ－Ｚｎ系フェライトの工業的な合成に用いられる、Ｍｎ含有量の少ないＦｅ２Ｏ３粉末を原料として使用し、さらにＭｎを別途添加した比較例に係るものとは異なり、Ｎｉ－Ｚｎ系フェライト材料のＮｉ／Ｚｎモル比の調整により、優れた直流重畳特性と比透磁率とが両立可能であることが判る。そして、Ｍｎ含有量の少ないＦｅ２Ｏ３粉末を原料として使用した場合には、Ｍｎを別途添加してＮｉ－Ｚｎ系フェライト材料におけるＭｎの総量を増加させても、Ｎｉ／Ｚｎモル比の調整のみでは、比透磁率を保持しつつ、直流重畳特性に優れ、かつインダクタンスの温度依存性の小さいコイル部品を製造することはできないことが判る。 Moreover, from the comparison between Example 1 and Comparative Example 4, the comparison between Example 2 and Comparative Example 5, and the comparison between Example 3 and Comparative Example 6, it is found that Fe 2 O 3 containing the expected amount of Mn The coil parts according to the examples in which Mn is not separately added other than using powder as a raw material are Fe 2 O 3 powders with low Mn content, which are used in the industrial synthesis of general Ni-Zn ferrite. Unlike the comparative example in which Mn was added as a raw material and Mn was added separately, by adjusting the Ni/Zn molar ratio of the Ni-Zn ferrite material, it is possible to achieve both excellent DC superimposition characteristics and relative magnetic permeability. It turns out that. When Fe 2 O 3 powder with low Mn content is used as a raw material, even if Mn is added separately to increase the total amount of Mn in the Ni-Zn ferrite material, the Ni/Zn molar ratio cannot be adjusted. It can be seen that it is not possible to manufacture a coil component that maintains relative magnetic permeability, has excellent DC superimposition characteristics, and has small temperature dependence of inductance by using only the above method.
さらに、実施例１～３の対比からは、原料として使用するＦｅ２Ｏ３粉末のＭｎ含有量が多くなるほど、所期の比透磁率が得られるＮｉ／Ｚｎモル比が小さくなることが判る。 Further, from a comparison of Examples 1 to 3, it can be seen that as the Mn content of the Fe 2 O 3 powder used as a raw material increases, the Ni/Zn molar ratio at which the desired relative magnetic permeability can be obtained becomes smaller.
上述のように、所期の量のＭｎを含むＦｅ２Ｏ３粉末を原料として使用した以外に別途Ｍｎを添加せずに製造された実施例に係るコイル部品が、一般的なＮｉ－Ｚｎ系フェライトの工業的な合成に用いられる、Ｍｎ含有量の少ないＦｅ２Ｏ３粉末を原料として使用し、さらにＭｎを別途添加した比較例に係るものとは異なり、直流重畳特性に優れたものとなる原因は明らかでない。本発明者は、Ｍｎを別途添加していない実施例とＭｎを別途添加した比較例の両方のコイル部品について、各々の試料断面をＥＤＸにて測定し、面内におけるＭｎの分布状態の差異の確認を試みたが、両試料共、Ｍｎの偏在部分はほとんど観察されず、両者の差異は確認できなかった。しかし、Ｍｎを含むＦｅ２Ｏ３粉末中では、Ｍｎを含む微細な粒子が均一に分散していることが、何らかの形で特性向上に寄与していると考えられる。すなわち、微量成分であるＭｎを原料粉末として別途添加した場合には、その量が他の成分に比べて少ないことに起因して、原料粉末中に均一に分散させることが困難である。このため、得られる磁性体中にＥＤＸによっても検出が困難な微視的な組成の偏りが生じ、十分な特性を発揮することができない。これに対し、Ｍｎが均一に分散したＦｅ２Ｏ３粉末を原料とすることで、前述した組成の偏りが低減され、優れた直流重畳特性を示すものと推測される。 As mentioned above, the coil component according to the example, which was manufactured using Fe 2 O 3 powder containing the desired amount of Mn as a raw material and without adding Mn separately, was manufactured using a general Ni-Zn-based Unlike the comparative example in which Fe 2 O 3 powder with low Mn content, which is used for industrial synthesis of ferrite, is used as a raw material and Mn is added separately, it has excellent DC superimposition characteristics. The cause is not clear. The present inventor measured the cross section of each sample using EDX for both the coil parts of the example in which Mn was not separately added and the comparative example in which Mn was separately added, and determined the difference in the distribution state of Mn in the plane. Although an attempt was made to confirm this, almost no unevenly distributed Mn was observed in both samples, and no difference between the two could be confirmed. However, in the Fe 2 O 3 powder containing Mn, it is thought that the uniform dispersion of fine particles containing Mn contributes to the improvement of the characteristics in some way. That is, when Mn, which is a trace component, is added separately as a raw material powder, it is difficult to uniformly disperse it in the raw material powder because its amount is small compared to other components. For this reason, microscopic compositional deviations that are difficult to detect even by EDX occur in the obtained magnetic material, making it impossible to exhibit sufficient characteristics. On the other hand, by using Fe 2 O 3 powder in which Mn is uniformly dispersed as a raw material, it is presumed that the above-described compositional deviation is reduced and excellent direct current superimposition characteristics are exhibited.
本発明によれば、主成分以外の添加物を用いなくとも、直流重畳特性及び透磁率に優れたコイル部品を提供することができる。また、本発明によれば、直流重畳特性及び透磁率の調整も容易となる。このため、簡便な操作で所期の性能のコイル部品を製造することができ、開発及び製造コストを低減できる点で本発明は有用である。また、本発明は、Ｎｉ－Ｚｎ系フェライト材料を製造するための原料粉末において、高価なＮｉ含有原料の使用量を低減することができるため、製造コストを低減できる点でも有用なものである。さらに、本発明は、磁性体中の微視的な組成の偏りを低減し、製造されるコイル部品の特性のバラツキを抑制することができる点でも有用と考えられる。 According to the present invention, it is possible to provide a coil component with excellent DC superimposition characteristics and magnetic permeability without using any additives other than the main components. Further, according to the present invention, it becomes easy to adjust the DC superimposition characteristics and the magnetic permeability. Therefore, the present invention is useful in that a coil component with desired performance can be manufactured with a simple operation, and development and manufacturing costs can be reduced. Further, the present invention is useful in that it can reduce the amount of expensive Ni-containing raw materials used in the raw material powder for producing Ni--Zn-based ferrite materials, thereby reducing manufacturing costs. Furthermore, the present invention is considered to be useful in that it can reduce microscopic composition bias in a magnetic material and suppress variations in characteristics of manufactured coil components.
Claims (4)
Ｆｅ ２ Ｏ ３ ５８．９～６６．９質量％、
ＺｎＯ ９．５～２５．４質量％、
ＮｉＯ ８．６～２３．６質量％、
ＣｕＯ ０．６～ ８．６質量％
の割合で含むフェライト材料から作られる磁性体の製造方法であって、
原料粉末として、Ｍｎ含有量が０．２０質量％以上である酸化鉄粉末を用いると共に、
前記酸化鉄粉末中のＭｎ含有量に基づいて、所定の直流重畳特性及び透磁率特性を有するコイル部品が得られるように前記フェライト材料中のＺｎに対するＮｉのモル比（Ｎｉ／Ｚｎ）を決定し、該モル比が得られるように前記原料粉末を配合する
ことを特徴とする、磁性体の製造方法。 Fe, Ni , Zn and Cu in terms of Fe 2 O 3 , ZnO, NiO and CuO,
Fe 2 O 3 58.9-66.9% by mass,
ZnO 9.5-25.4% by mass,
NiO 8.6-23.6% by mass,
CuO 0.6-8.6% by mass
A method for producing a magnetic material made from a ferrite material containing a proportion of
As the raw material powder, iron oxide powder having a Mn content of 0.20% by mass or more is used, and
Based on the Mn content in the iron oxide powder, the molar ratio of Ni to Zn (Ni/Zn) in the ferrite material is determined so as to obtain a coil component having predetermined DC superimposition characteristics and magnetic permeability characteristics. , a method for producing a magnetic material, characterized in that the raw material powders are blended so as to obtain the molar ratio.
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| JP2004107103A (en) | 2002-09-13 | 2004-04-08 | Kyocera Corp | Ferrite material and ferrite core using the same |
| JP2006282437A (en) | 2005-03-31 | 2006-10-19 | Tdk Corp | Ferrite sintered compact, method for manufacturing the same, and coil component |
| WO2013115064A1 (en) | 2012-01-31 | 2013-08-08 | 株式会社村田製作所 | Magnetic body material and wound coil component provided with core formed using same |
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| JP2004107103A (en) | 2002-09-13 | 2004-04-08 | Kyocera Corp | Ferrite material and ferrite core using the same |
| JP2006282437A (en) | 2005-03-31 | 2006-10-19 | Tdk Corp | Ferrite sintered compact, method for manufacturing the same, and coil component |
| WO2013115064A1 (en) | 2012-01-31 | 2013-08-08 | 株式会社村田製作所 | Magnetic body material and wound coil component provided with core formed using same |
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