JP6442251B2 - Magnetic material and magnetic porcelain composition - Google Patents
Magnetic material and magnetic porcelain composition Download PDFInfo
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- JP6442251B2 JP6442251B2 JP2014238649A JP2014238649A JP6442251B2 JP 6442251 B2 JP6442251 B2 JP 6442251B2 JP 2014238649 A JP2014238649 A JP 2014238649A JP 2014238649 A JP2014238649 A JP 2014238649A JP 6442251 B2 JP6442251 B2 JP 6442251B2
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- 239000000696 magnetic material Substances 0.000 title claims description 33
- 239000000203 mixture Substances 0.000 title claims description 22
- 229910052573 porcelain Inorganic materials 0.000 title description 8
- 238000005245 sintering Methods 0.000 claims description 12
- 239000000654 additive Substances 0.000 claims description 11
- 230000000996 additive effect Effects 0.000 claims description 9
- 239000000919 ceramic Substances 0.000 claims description 9
- JCLFHZLOKITRCE-UHFFFAOYSA-N 4-pentoxyphenol Chemical compound CCCCCOC1=CC=C(O)C=C1 JCLFHZLOKITRCE-UHFFFAOYSA-N 0.000 claims description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 21
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 15
- 238000000034 method Methods 0.000 description 11
- 230000035699 permeability Effects 0.000 description 9
- 239000002994 raw material Substances 0.000 description 7
- 239000011701 zinc Substances 0.000 description 7
- 229910007565 Zn—Cu Inorganic materials 0.000 description 6
- 238000010304 firing Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 229910018605 Ni—Zn Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 238000004804 winding Methods 0.000 description 4
- 239000004020 conductor Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 229910017518 Cu Zn Inorganic materials 0.000 description 2
- 229910017752 Cu-Zn Inorganic materials 0.000 description 2
- 229910017943 Cu—Zn Inorganic materials 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 241000270295 Serpentes Species 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- Compounds Of Iron (AREA)
- Magnetic Ceramics (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Soft Magnetic Materials (AREA)
Description
本発明は積層チップ部品などに用いられる磁性材に関する。 The present invention relates to a magnetic material used for laminated chip parts and the like.
周知のごとく、積層チップ部品である積層インダクタでは、電気絶縁性の磁性層と導体パターンが交互に積層されるとともに、各層の導体パターンが順次層間で接続されることで、磁性体中で積層方向に重畳しながら螺旋状に周回するコイルが形成される。このような積層インダクタは、コイルの周囲がフェライト材料からなる磁性体で囲まれているため、外部への磁気漏洩が少なく、比較的少ない巻数で必要なインダクタンスが得られる特徴があり、小型化、薄型化に適している。 As is well known, in a multilayer inductor that is a multilayer chip component, an electrically insulating magnetic layer and a conductor pattern are alternately laminated, and the conductor patterns of each layer are sequentially connected between the layers, so that the lamination direction in the magnetic body A coil that spirals around is formed while superimposing on the coil. Since such a multilayer inductor is surrounded by a magnetic body made of a ferrite material, the coil is surrounded by a small amount of magnetic leakage to the outside. Suitable for thinning.
積層インダクタは、厚膜技術を用いて磁性層となるペースト状の磁性材料からなるシート上に電極層となる電極パターンが形成されたものを順次積層して得た積層体を焼成し、その焼成によって得られた焼結体の表面に外部電極用ペーストを形成することで製造される。また電極層は、融点が９６２℃のＡｇ（銀）を導電体として用いるのが一般的であることから、磁性層を構成する磁性材料としては、低温での焼成が可能なＮｉ−Ｚｎ（ニッケル―亜鉛）系フェライトがある。 Multilayer inductors fire a laminated body obtained by sequentially laminating a sheet made of a paste-like magnetic material, which becomes a magnetic layer, using a thick film technique, and in which an electrode pattern that becomes an electrode layer is formed. It is manufactured by forming the paste for external electrodes on the surface of the sintered body obtained by the above. Since the electrode layer generally uses Ag (silver) having a melting point of 962 ° C. as a conductor, the magnetic material constituting the magnetic layer is Ni—Zn (nickel) that can be fired at a low temperature. -Zinc) Ferrite.
なお以下の特許文献１などには、本発明に関連する技術として、Ｎｉ−Ｚｎ系フェライトにＣｕ（銅）を添加したＮｉ−Ｚｎ−Ｃｕ系フェライト材料の改良技術について開示されている。また以下の非特許文献１には磁性材料の特性についての基礎的な事項について記載されている。非特許文献２には磁性材料の特性評価方法などが記載されている。
The following Patent Document 1 discloses a technique for improving a Ni—Zn—Cu ferrite material in which Cu (copper) is added to Ni—Zn ferrite as a technique related to the present invention. Non-Patent Document 1 below describes basic matters regarding the characteristics of magnetic materials. Non-Patent
磁性材料としてはＭｎＺｎ系フェライトがよく知られているが、積層チップ部品に用いるためには上述した電極層を構成するＡｇの融点に関わる問題から、Ｎｉを含んだフェライトを用いている。しかしＮｉ―Ｚｎ系フェライトやＮｉ−Ｃｕ−Ｚｎ系フェライトはＭｎＺｎ系フェライトと比較すると損失（コアロス）が大きく直流重畳特性が劣化するという問題を有していた。そのため磁性材料中のＦｅ（鉄）の割合を大きくして飽和磁束密度を高め、直流重畳特性を確保していた。例えば上記特許文献１に記載の磁性材料ではＦｅの割合をＦｅ２Ｏ３換算で４９ｍｏｌ％程度である。 As a magnetic material, MnZn-based ferrite is well known. However, in order to use it for a laminated chip component, ferrite containing Ni is used because of the problem relating to the melting point of Ag constituting the electrode layer described above. However, Ni—Zn based ferrite and Ni—Cu—Zn based ferrite have a problem that the loss (core loss) is large and the DC superposition characteristics are deteriorated as compared with MnZn based ferrite. Therefore, the ratio of Fe (iron) in the magnetic material is increased to increase the saturation magnetic flux density, and the DC superposition characteristics are ensured. For example, in the magnetic material described in Patent Document 1, the proportion of Fe is about 49 mol% in terms of Fe 2 O 3 .
さらに上記特許文献１に記載のフェライト材料では２価〜４価の金属を添加することで焼結性やＱ特性（高周波特性）も向上させている。そして当該特許文献１では２価の金属としてはとくにＣｏ（コバルト）が最も好ましいとしており、そのＣｏはＣｏＯのような酸化物として添加していた。しかしＦｅの割合が多くＣｏＯなどを添加したフェライト材料では自ずと透磁率μが大きくなる。確かに磁性材料として透磁率μが大きくなること自体は問題ではないが、積層インダクタを広い周波数範囲で使用する場合、周知のスネーク（Ｓｎｏｅｋ）の限界から透磁率μを大きくしてしまうと高周波領域でコアロスが増大するという問題が発生する。そこでＮｉ―Ｚｎ系フェライトやＮｉ−Ｃｕ−Ｚｎ系フェライトの組成を調整することで透磁率を低くすることが考えられる。具体的にはＺｎに対してＮｉの割合を大きくする。しかしフェライト中でＮｉの割合をＺｎに対して大きくすると磁歪が増加し、透磁率μを低下させることができてもこの磁歪の増加によってやはりコアロスが発生するという背反が生じる。 Furthermore, in the ferrite material described in Patent Document 1, the sinterability and Q characteristics (high frequency characteristics) are improved by adding a bivalent to tetravalent metal. In Patent Document 1, Co (cobalt) is most preferable as the divalent metal, and Co is added as an oxide such as CoO. However, the magnetic permeability μ is naturally increased in a ferrite material having a large proportion of Fe and added with CoO or the like. Certainly, it is not a problem that the magnetic permeability μ increases as a magnetic material, but when the laminated inductor is used in a wide frequency range, if the magnetic permeability μ is increased from the limit of the well-known Snake, the high frequency region This causes a problem that the core loss increases. Therefore, it is conceivable to reduce the magnetic permeability by adjusting the composition of Ni—Zn ferrite or Ni—Cu—Zn ferrite. Specifically, the ratio of Ni to Zn is increased. However, when the proportion of Ni in the ferrite is increased with respect to Zn, the magnetostriction increases, and even though the magnetic permeability μ can be reduced, the increase in magnetostriction still causes a contradiction that core loss occurs.
そこで本発明は、低温焼成が可能で、高周波領域を含む広い周波数範囲でのコアロス特性に優れた磁性材料を提供することを目的としている。 Therefore, an object of the present invention is to provide a magnetic material that can be fired at a low temperature and has excellent core loss characteristics in a wide frequency range including a high frequency region.
上記目的を達成するための本発明は、Ｆｅ２Ｏ３がａｍｏｌ％、ＺｎＯがｂｍｏｌ％、ＣｕＯがｃｍｏｌ％、残部としてＮｉＯがｄｍｏｌ％含まれている主成分に対して添加剤としてｘｗｔ％のＺｒＯ２とｙｗｔ％のＮｂ２Ｏ５とが添加され、
ａ＋ｂ＋ｃ＋ｄ＝１００、４３≦ａ≦４８、２０≦ｂ≦３０、５≦ｃ≦１５であるとともに、０．５≦ｘ≦０．７、０．１＜ｙ≦０．３
であることを特徴とする磁性材料としている。
The present invention for achieving the above object, Fe 2 O 3 is amol%, ZnO is bmol%, CuO is cmol%, NiO as the balance of xwt% as an additive with respect to the main component contained dmol% ZrO 2 and ywt% Nb 2 O 5 are added,
a + b + c + d = 100, 43 ≦ a ≦ 48, 20 ≦ b ≦ 30, 5 ≦ c ≦ 15, 0.5 ≦ x ≦ 0.7, 0.1 <y ≦ 0.3
It is a magnetic material characterized by the above.
前記主成分に対して添加剤としてＣａＣＯ３が０ｗｔ％よりも多く０．０５ｗｔ％以下で添加されている磁性材料とすればより好ましい。また本発明は前記磁性材料を焼結させてなる磁性磁器組成物も含んでいる。 It is more preferable to use a magnetic material in which CaCO 3 is added in an amount of more than 0 wt% and 0.05 wt% or less as an additive to the main component. The present invention also includes a magnetic ceramic composition ing by sintering the magnetic material.
本発明の磁性材料によれば、積層インダクタの磁性層に適用した際に、低温焼成を可能としつつ、広い周波領域においてコアロスを低減させることができる。 According to the magnetic material of the present invention, when applied to the magnetic layer of the multilayer inductor, core loss can be reduced in a wide frequency range while enabling low-temperature firing.
＝＝＝本発明に想到する過程＝＝＝
本発明に係る磁性材料はＮｉ−Ｚｎ−Ｃｕ系フェライトを主成分としつつ、その主成分に各種酸化金属を添加したものである。あるいはその磁性材料を焼結させることでＮｉの一部をその添加物に含まれる金属に置換した磁性磁器組成物である。たしかにここまでは従来の磁器材料や磁性磁器組成物と同じである。しかし本発明は、Ｎｉに対してＺｎの割合を大きくすることで磁歪を低減させ、さらにＦｅの割合を小さくすることで透磁率μが大きくなりすぎないように調整して高周波領域でのコアロス特性を改善するという技術思想に基づいて想到したものである。この技術思想は従来の技術思想とは正反対である。すなわち従来はＮｉ−Ｚｎ−Ｃｕ系フェライトにおいてＺｎに対してＮｉの割合を大きくすることで、Ｎｉフェライトに基づく低温焼成を可能としつつ透磁率μを小さくしていた。
=== The process of conceiving the present invention ===
The magnetic material according to the present invention is composed of Ni—Zn—Cu ferrite as a main component and various metal oxides added to the main component. Alternatively, a magnetic ceramic composition in which a part of Ni is replaced with a metal contained in the additive by sintering the magnetic material. It is true that it is the same as conventional porcelain materials and magnetic porcelain compositions so far. However, the present invention reduces the magnetostriction by increasing the ratio of Zn to Ni, and further adjusts the permeability μ so that the magnetic permeability μ does not become too large by decreasing the ratio of Fe. It was conceived based on the technical idea of improving. This technical idea is the opposite of the conventional technical idea. That is, conventionally, by increasing the ratio of Ni to Zn in Ni—Zn—Cu based ferrite, the magnetic permeability μ was reduced while enabling low-temperature firing based on Ni ferrite.
また本発明者が上記の従来とは正反対の技術思想に基づいて本発明に至る過程で上記主成分における各金属の割合について検討したところ、以下に示す知見を得ることができた。焼結体である磁性磁器組成物の状態では、Ｆｅ２Ｏ３換算でのＦｅの割合が４８ｍｏｌ％よりも大きいとコアロスの温度依存性が大きくなり、４３ｍｏｌ％未満では必要な磁気特性（例えば透磁率μが小さすぎる）が得られなかった。Ｚｎの割合についてはＺｎＯ換算で３０ｍｏｌ％よりも大きいと相転移温度（Ｔｃ）が低くなり、２０ｍｏｌ％未満では必要な磁気特性が得られなかった。Ｃｕの割合についてはＣｕＯ換算で５ｍｏｌ％以上１５ｍｏｌ％以下の割合とすることでＡｇの融点以下である９００℃の焼結温度で十分な焼結密度を得ることができ、かつ必要な磁気特性が得られた。そして本発明者は、上述した技術思想の転換や知見を出発点として、Ｎｉ−Ｚｎ−Ｃｕ系フェライトに対して添加する種々の金属酸化物とその添加量につい鋭意研究を重ね、その結果本発明に想到した。 In addition, when the present inventor examined the ratio of each metal in the main component in the process leading to the present invention based on the technical idea opposite to the conventional one, the following knowledge could be obtained. In the state of the magnetic porcelain composition that is a sintered body, the temperature dependence of core loss increases when the proportion of Fe in terms of Fe 2 O 3 is greater than 48 mol%, and the required magnetic properties (for example, permeability) are less than 43 mol%. Magnetic susceptibility μ was too small). When the proportion of Zn is larger than 30 mol% in terms of ZnO, the phase transition temperature (Tc) becomes low, and when it is less than 20 mol%, necessary magnetic properties cannot be obtained. About the ratio of Cu, by making it into the ratio of 5 mol% or more and 15 mol% or less in conversion of CuO, a sufficient sintering density can be obtained at a sintering temperature of 900 ° C. which is not more than the melting point of Ag, and necessary magnetic properties are obtained. Obtained. Then, the present inventor repeated earnest research on various metal oxides added to the Ni—Zn—Cu ferrite and the amount of the addition, starting from the above-mentioned change in the technical idea and knowledge, and as a result, the present invention. I came up with it.
＝＝＝第１の実施例＝＝＝
本発明の第１の実施例は広い周波数範囲でのコアロス特性を改善させた磁性材料であり、概略的には上述したＦｅ、Ｚｎ、Ｃｕの割合に関する知見に基づく組成を有するＮｉ−Ｚｎ−Ｃｕ系フェライトを主成分としつつ、その主成分にＺｒＯとＮｂ２Ｏ５が適量添加されたものである。そして第１の実施例に係る磁性材料の特性を評価するために、ＺｒＯとＮｂ２Ｏ５の割合が異なるＮｉ−Ｚｎ−Ｃｕ系フェライトを用いたリング状の焼結体（以下、リングコアとも言う）をサンプルとして作成し、各サンプルのコアロスを測定した。
=== First Embodiment ===
The first embodiment of the present invention is a magnetic material having improved core loss characteristics in a wide frequency range, and is generally a Ni-Zn-Cu having a composition based on the above-described knowledge about the ratio of Fe, Zn, and Cu. The main component is based ferrite, and ZrO and Nb 2 O 5 are added in appropriate amounts to the main component. In order to evaluate the characteristics of the magnetic material according to the first example, a ring-shaped sintered body using Ni—Zn—Cu based ferrite having different ratios of ZrO and Nb 2 O 5 (hereinafter also referred to as a ring core). ) As a sample, and the core loss of each sample was measured.
＜サンプルの作製手順＞
図１にサンプルの作製手順を示す図を示した。まず主成分の原料となるＦｅ２Ｏ３、ＺｎＯ、ＣｕＯ、ＮｉＯを秤量、混合する。秤量に際してはＦｅ２Ｏ３が４３〜４８ｍｏｌ％、ＺｎＯが２０〜３０ｍｏｌ％、ＣｕＯが５〜１５ｍｏｌ％の範囲となるように秤量するとともに残部をＮｉＯとした主成分の原料を用意し、その主成分の原料をボールミルなどを用いて混合する（ｓ１）。そして上記主成分の原料の混合物を７５０℃で仮焼成する（ｓ２）。その仮焼成によって得られた粉体をボールミルにてさらに３０時間粉砕し、その粉砕後の粉体に対し、添加剤としてＺｒＯ２とＮｂ２Ｏ５をサンプルに応じた割合（ｗｔ％）で添加し（ｓ３→ｓ４、ｓ５）、粉砕後の主成分原料に添加剤を添加して得られた粉体にＰＶＡ水溶液などのバインダーを加えた混合して適宜な大きさの粒子径となるように造粒する（ｓ６）。そしてその造粒物を外形２５ｍｍ、内径１５ｍｍ、厚さ５ｍｍのリング状に成形する（ｓ７）た。そして、その成形体をＡｇの融点以下である９００℃で焼成し、サンプルとなるリングコアを得た（ｓ８）。なお比較例に係るサンプルとして添加剤が添加されていない主成分の原料のみからなるリングコア（以下、標準サンプルとも言う）を作成した。標準サンプルについてはボールミルによる粉砕によって得た粉体をリング状に成形して焼結させることで作成した（ｓ３→ｓ６〜ｓ８）。
<Sample preparation procedure>
FIG. 1 is a diagram showing a sample manufacturing procedure. First, Fe 2 O 3 , ZnO, CuO, and NiO as raw materials for the main components are weighed and mixed. In weighing, a raw material of a main component having NiO as the balance and preparing a main component raw material was prepared so that Fe 2 O 3 would be 43 to 48 mol%,
＜コアロスの周波数特性＞
各サンプルにおけるコアロスの特性を評価するのに当たり、上述した手順で作成した各サンプルにおいて主成分の組成が同じものを選出した。例えばＦｅ２Ｏ３が４５ｍｏｌ％、ＺｎＯが２５ｍｏｌ％、ＣｕＯが１０ｍｏｌ％、残部をＮｉＯとしたものを選出した。その上で各サンプルのコアロスを様々な周波数にて測定した。またコアロスの測定に際しては各サンプルを所定の巻線数（例えば巻線数３）のトロイダルリングコアにして、周知のＢＨアナライザを用いた。また測定時の最大磁気飽和密度Ｂｍ＝５０ｍＴとし、１００ｋＨｚ、３００ｋＨｚ、５００ｋＨｚ、７００ｋＨｚ、１０００ｋＨｚの各周波数にてコアロスを測定した。
<Frequency characteristics of core loss>
In evaluating the core loss characteristics of each sample, samples having the same main component composition were selected for each sample prepared by the above-described procedure. For example, one having 45 mol% Fe 2 O 3 , 25 mol% ZnO, 10 mol% CuO, and NiO as the balance was selected. Then, the core loss of each sample was measured at various frequencies. In measuring the core loss, each sample was used as a toroidal ring core having a predetermined number of windings (for example, three windings), and a well-known BH analyzer was used. Further, the core loss was measured at each frequency of 100 kHz, 300 kHz, 500 kHz, 700 kHz, and 1000 kHz with the maximum magnetic saturation density Bm = 50 mT at the time of measurement.
以下の表１に各サンプルのコアロス特性を示した。 Table 1 below shows the core loss characteristics of each sample.
ここで表１に示した結果について考察すると、まず、積層インダクタなどに用いられる磁性材料では焼結体にしたときに所謂「粒成長」と呼ばれる部分的な結晶成長が発生すると結晶構造に歪みが生じ磁気特性が劣化するという問題がある。第１の実施例に係る磁性材料では主成分にＺｒＯ２とＮｂ２Ｏ５を適量添加しており、ＺｒＯ２に由来するＺｒが焼結体の粒界に析出し、その析出したＺｒが結晶の粒生長を抑制する。その一方でＺｒＯ２は焼結性を低減させて９００℃程度の焼結温度では磁気特性を劣化させる要因にもなり得るもののＮｂ２Ｏ５を適量添加していることでＺｒＯ２によって劣化した焼結性が改善され、結果として、低温での焼結性を維持しつつＺｒＯ２によるコアロス特性の改善効果のみが顕在化したものと思われる。 Considering the results shown in Table 1, when a magnetic material used for a multilayer inductor or the like is first formed into a sintered body, when a partial crystal growth called “grain growth” occurs, the crystal structure is distorted. There arises a problem that the magnetic properties are deteriorated. In the magnetic material according to the first embodiment, ZrO 2 and Nb 2 O 5 are added in appropriate amounts as main components, Zr derived from ZrO 2 is precipitated at the grain boundaries of the sintered body, and the precipitated Zr is crystallized. Suppresses grain growth. On the other hand, ZrO 2 reduces the sinterability and may cause deterioration of magnetic properties at a sintering temperature of about 900 ° C. However, the addition of an appropriate amount of Nb 2 O 5 allows ZrO 2 to deteriorate the sintering property. As a result, it seems that only the improvement effect of the core loss property by ZrO 2 is manifested while maintaining the sinterability at a low temperature.
＝＝＝第２の実施例＝＝＝
ところで焼結した磁性材料は応力よってインダクタンスＬが変化することが知られているが、応力によるインダクタンスＬの変動が大きいとその変動を補正するための制御が難しくなり問題となる。そこで第２の実施例として磁性磁器組成物にしたときに応力よるインダクタンスＬの変動がより小さな磁性材料を挙げる。概略的には第１の実施例に係る磁性材料にＣａをさらに適量添加することで応力に対するインダンクタンスＬの変動を減少させている。
=== Second Embodiment ===
By the way, it is known that the inductance L of the sintered magnetic material changes depending on the stress. However, if the fluctuation of the inductance L due to the stress is large, control for correcting the fluctuation becomes difficult and becomes a problem. Therefore, as a second embodiment, a magnetic material in which the variation of the inductance L due to stress is smaller when a magnetic porcelain composition is used will be mentioned. Schematically, by adding an appropriate amount of Ca to the magnetic material according to the first embodiment, the variation of the inductance L with respect to stress is reduced.
＜応力依存特性＞
まず第１の実施例において作製したサンプル２に対してＮｉの一部をＣａに置換したサンプルを作製した。具体的には図１において添加剤を秤量して混合するステップｓ５で、表１に示したサンプル３と同じ量のＺｒＯ２とＮｂ２Ｏ５を添加するとともに、ＣａＣＯ３をサンプルに応じた量だけ添加してステップｓ６〜ｓ８を実行することで主成分中のＮｉの一部がＣａに置換された磁性磁器組成物からなるリングコアをサンプルとして作製した。そして図２に示したように、リングコア１に巻線２を巻いたトロイダルリングコア１０に対し径方向に加重Ｆ（ｋｇｆ）を掛ける。そしてそのときの巻線の両端ａ−ａ’間のインピーダンスＬを周知のインピーダンスアナライザを用いて測定する。
<Stress dependence characteristics>
First, a sample was prepared by replacing part of Ni with Ca for
＜コアロス特性＞
表２に各サンプルにおけるＣａＣＯ３換算でのＣａの割合を示した。
<Core loss characteristics>
Table 2 shows the ratio of Ca in terms of CaCO 3 in each sample.
＜コアロスの周波数特性＞
上述したように第１の実施例に係る磁性材料に対しさらにＣａＣＯ３を添加した磁性材料を焼結してＮｉの一部をＣａに置換した磁性磁器組成物では、応力に対するインダクタンスＬの変動を減少させることができた。しかしＮｉの一部をＣａに置換させたことでコアロスが大きくなってしまっては本末転倒となる。そこで標準サンプルと表２に示したサンプル３、８〜１０におけるコアロスの周波数特性を調べた。
<Frequency characteristics of core loss>
As described above, in the magnetic porcelain composition in which the magnetic material according to the first embodiment is further sintered with the magnetic material added with CaCO 3 and a part of Ni is replaced with Ca, the fluctuation of the inductance L with respect to the stress is changed. It was possible to decrease. However, if a part of Ni is replaced by Ca and the core loss becomes large, the tip falls. Therefore, the frequency characteristics of the core loss in the standard sample and the samples 3 and 8 to 10 shown in Table 2 were examined.
表３に各サンプル１、３、８〜１０におけるコアロスの周波数特性を示した。 Table 3 shows the frequency characteristics of the core loss in each sample 1, 3, 8-10.
１ 磁器磁性組成物（焼結体、リングコア）、ｓ１ 主成分原料秤量・混合工程、
ｓ２ 仮焼成工程、ｓ３ 添加剤秤量・混合工程、ｓ６ 造粒工程、ｓ７ 成形工程、
ｓ８ 焼成工程
1 porcelain magnetic composition (sintered body, ring core), s1 main component raw material weighing and mixing step,
s2 preliminary firing step, s3 additive weighing / mixing step, s6 granulation step, s7 molding step,
s8 Firing process
Claims (3)
ａ＋ｂ＋ｃ＋ｄ＝１００、４３≦ａ≦４８、２０≦ｂ≦３０、５≦ｃ≦１５であるとともに、０．５≦ｘ≦０．７、０．１＜ｙ≦０．３
であることを特徴とする磁性材料。 Fe 2 O 3 is amol%, ZnO is bmol%, CuO is cmol%, NiO as the balance and xwt% of ZrO 2 and Ywt% of Nb 2 O 5 as an additive with respect to the main component contained dmol% Is added,
a + b + c + d = 100, 43 ≦ a ≦ 48, 20 ≦ b ≦ 30, 5 ≦ c ≦ 15, 0.5 ≦ x ≦ 0.7, 0.1 <y ≦ 0.3
A magnetic material characterized by
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