JP5765250B2 - Ferrite sintered body and electronic parts - Google Patents
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- 229910000859 α-Fe Inorganic materials 0.000 title claims description 47
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 59
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 46
- 239000011787 zinc oxide Substances 0.000 claims description 29
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 21
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 11
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 10
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 6
- 239000005751 Copper oxide Substances 0.000 claims description 5
- 229910000431 copper oxide Inorganic materials 0.000 claims description 5
- 229910052596 spinel Inorganic materials 0.000 claims description 2
- 239000011029 spinel Substances 0.000 claims description 2
- 230000035699 permeability Effects 0.000 description 21
- 239000002994 raw material Substances 0.000 description 21
- 239000000463 material Substances 0.000 description 15
- 235000014692 zinc oxide Nutrition 0.000 description 13
- 238000005259 measurement Methods 0.000 description 11
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- 229910017518 Cu Zn Inorganic materials 0.000 description 2
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- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
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- 150000001875 compounds Chemical class 0.000 description 2
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- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
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- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
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- 230000000052 comparative effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
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- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 150000003891 oxalate salts Chemical class 0.000 description 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
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- 239000007921 spray Substances 0.000 description 1
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- Magnetic Ceramics (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Soft Magnetic Materials (AREA)
Description
本発明は、自動車用トランスポンダ、チョークコイルおよびインダクタなどのフェライトコアの製造に好適なフェライト焼結体と、該焼結体から構成されるフェライトコアのたとえば周囲に巻き線が巻回してあるコイル部品などの電子部品と、に関する。 The present invention relates to a ferrite sintered body suitable for manufacturing a ferrite core such as an automobile transponder, choke coil, and inductor, and a coil component in which a winding is wound around, for example, a ferrite core composed of the sintered body. And so on.
フェライト焼結体で構成されるフェライトコアは、主としてコイル部品、センサ、アンテナ、偏向ヨーク等の部品に用いられており、これらの部品は、各種電子機器に用いられていた。 Ferrite cores composed of ferrite sintered bodies are mainly used for parts such as coil parts, sensors, antennas, deflection yokes, etc., and these parts have been used for various electronic devices.
しかしながら、近年、携帯電話やノート型パソコン等の携帯用機器の急速な普及が進み、たとえばコイル部品が組み込まれた機器には、厳しい使用環境、とりわけ温度変化に耐え得る特性が要求される。具体的には、使用可能な温度域が広範囲に及ぶことや、かつその温度域での初透磁率の変化が小さい、望ましくは全く変化しないことが挙げられる。 However, in recent years, portable devices such as mobile phones and notebook personal computers have rapidly spread. For example, a device incorporating a coil component is required to have a characteristic that can withstand harsh use environments, particularly temperature changes. Specifically, the usable temperature range covers a wide range, and the change in the initial magnetic permeability in the temperature range is small, preferably not changed at all.
さらに近年、特にトランスポンダなどのタイヤ空気圧センサやエンジンルーム内の制御回路等の自動車用部品としても、コイル部品の用途が拡大しており、このような用途には、厳しい使用環境、とりわけ温度変化に耐え得る特性が要求される。 In recent years, coil parts have also been used for automobile parts such as tire pressure sensors such as transponders and control circuits in engine rooms. Characteristics that can be withstood are required.
しかも、コイル部品は、用途に応じて、その初透磁率が特定の範囲内にあるものが選択される。したがって、コイル部品には、初透磁率の温度変化が小さいことに加え、その初透磁率が特定の範囲にあることが求められる。 In addition, a coil component whose initial permeability is in a specific range is selected according to the application. Therefore, the coil component is required to have the initial permeability within a specific range in addition to the small temperature change of the initial permeability.
ところで、特許文献１では、Ｎｉ−Ｃｕ−Ｚｎ系フェライト焼結体において、Ｆｅ２Ｏ３とＺｎＯとの比を特定の範囲とすることで、初透磁率の相対温度係数を良好にできるフェライトが記載されている。 By the way, in Patent Document 1, in a Ni—Cu—Zn-based ferrite sintered body, a ferrite that can improve the relative temperature coefficient of initial permeability by setting the ratio of Fe 2 O 3 and ZnO within a specific range is disclosed. Have been described.
本発明は、このような実状に鑑みてなされ、広い温度範囲（たとえば、−４０〜１２５℃）において、初透磁率μｉの変化率が小さく、しかも初透磁率μｉが特定の範囲（たとえば、３５０〜７００程度）にあるフェライト焼結体と、該フェライト焼結体で構成してあるフェライトコアを有する電子部品とを、提供することを目的とする。 The present invention has been made in view of such a situation, and in a wide temperature range (for example, −40 to 125 ° C.), the change rate of the initial permeability μi is small and the initial permeability μi is in a specific range (for example, 350 It is an object of the present invention to provide a ferrite sintered body at about 700 to an electronic component having a ferrite core composed of the ferrite sintered body.
上記目的を達成するために、本発明に係るフェライト焼結体は、スピネル構造を有し、酸化鉄と、酸化亜鉛と、酸化銅と、酸化ニッケルと、を含む主成分を有するフェライト焼結体である。該フェライト焼結体はＡ相とＢ相とを有している。Ａ相は、酸化鉄のＦｅ２Ｏ３換算での含有割合（モル％）が酸化亜鉛のＺｎＯ換算での含有割合（モル％）よりも大きい領域であり、Ｂ相は、酸化鉄のＦｅ２Ｏ３換算での含有割合（モル％）が酸化亜鉛のＺｎＯ換算での含有割合（モル％）以下の領域である。主成分１００モル％に占める酸化鉄のＦｅ２Ｏ３換算での含有割合をｘ（モル％）とし、Ａ相の面積とＢ相の面積との合計面積に対するＡ相の面積割合をｙ（％）とした場合に、変数（ｘ，ｙ）が、下記の点Ａ〜Ｄを頂点とする四角形に囲まれた領域内（線上を含む）にある。
点Ａ（４６，９７）
点Ｂ（４６，８３）
点Ｃ（４７．９，７０）
点Ｄ（４７．９，８５）
In order to achieve the above object, a ferrite sintered body according to the present invention has a spinel structure and has a main component containing iron oxide, zinc oxide, copper oxide, and nickel oxide. It is. The ferrite sintered body has an A phase and a B phase. The A phase is a region in which the content ratio (mol%) of iron oxide in terms of Fe 2 O 3 is larger than the content ratio (mol%) of zinc oxide in terms of ZnO, and the B phase is Fe 2 of iron oxide. The content ratio (mol%) in terms of O 3 is a region below the zinc oxide content ratio (mol%) in terms of ZnO. The content ratio of iron oxide in 100 mol% of the main component in terms of Fe 2 O 3 is x (mol%), and the area ratio of the A phase to the total area of the area of the A phase and the area of the B phase is y (% ), The variable (x, y) is in an area (including a line) surrounded by a rectangle whose vertices are the following points A to D.
Point A (46,97)
Point B (46, 83)
Point C (47.9, 70)
Point D (47.9, 85)
本発明に係るフェライト焼結体では、主成分中に占める酸化鉄のＦｅ２Ｏ３換算での含有量（モル％）と、上記のＡ相の面積比率（％）と、が特定の範囲にある。このようにすることで、広い温度範囲における初透磁率の変化率を小さくすることができ、しかも、初透磁率を特定の範囲内とすることができる。 In the ferrite sintered body according to the present invention, the content (mol%) of iron oxide in the main component in terms of Fe 2 O 3 and the area ratio (%) of the A phase are within a specific range. is there. By doing in this way, the rate of change of the initial permeability in a wide temperature range can be reduced, and the initial permeability can be set within a specific range.
本発明に係る電子部品は、上記に記載のフェライト焼結体から構成されるフェライトコアを有する電子部品である。 The electronic component which concerns on this invention is an electronic component which has a ferrite core comprised from the ferrite sintered compact as described above.
本発明に係る電子部品は、μｉの温度変化が少なく、しかもμｉが特定の範囲（たとえば、３５０〜７００程度）にあるため、１Ｈｚ〜５ＭＨｚまでの周波数帯における応用製品のコイル部品、トランス部品、磁気ヘッド部品に好適である。コイル部品としては、自動車用トランスポンダ、インダクタやチョークコイル等が挙げられ、トランス部品としては、スイッチング用、インバータ用等の電源トランス等が挙げられる。 Since the electronic component according to the present invention has a small temperature change of μi and μi is in a specific range (for example, about 350 to 700), the coil component, the transformer component, and the application product in the frequency band from 1 Hz to 5 MHz. Suitable for magnetic head components. Examples of the coil component include a transponder for an automobile, an inductor, a choke coil, and the like. Examples of the transformer component include a power transformer for switching and an inverter.
以下、本発明を図面に示す実施形態に基づき説明する。 Hereinafter, the present invention will be described based on embodiments shown in the drawings.
本実施形態に係るコイル部品用フェライトコアとしては、図１に示したドラム型のほか、ＦＴ型、ＥＴ型、ＥＩ型、ＵＵ型、ＥＥ型、ＥＥＲ型、ＵＩ型、トロイダル型、ポット型、カップ型等を例示することができる。図１では、コイル部品１０は、フェライトコア１２の周囲に巻き線１４を所定巻数だけ巻回することにより得られる。
As a ferrite core for coil parts according to the present embodiment, in addition to the drum type shown in FIG. 1, FT type, ET type, EI type, UU type, EE type, EER type, UI type, toroidal type, pot type, A cup type etc. can be illustrated. In FIG. 1, the
コイル部品１０のフェライトコア１２は、本実施形態に係るフェライト焼結体で構成してある。該フェライト焼結体は、Ｎｉ−Ｃｕ−Ｚｎ系フェライトであり、その主成分は、酸化鉄、酸化銅、酸化亜鉛および酸化ニッケルから構成される。
The
また、本実施形態に係るフェライト焼結体は、主として、Ａ相とＢ相とから構成されている。なお、該フェライト焼結体は、Ａ相およびＢ相以外の相を有していてもよい。 The ferrite sintered body according to the present embodiment is mainly composed of an A phase and a B phase. The sintered ferrite body may have a phase other than the A phase and the B phase.
本実施形態では、Ａ相およびＢ相の両方が、構成成分として、酸化鉄、酸化銅、酸化亜鉛および酸化ニッケルを少なくとも有しており、酸化鉄と酸化亜鉛との含有割合によりＡ相とＢ相とに分けられている。すなわち、Ａ相は、酸化鉄のＦｅ２Ｏ３換算での含有量（モル％）が、酸化亜鉛のＺｎＯ換算での含有量（モル％）よりも大きい領域（相）である。また、Ｂ相は、酸化鉄のＦｅ２Ｏ３換算での含有量（モル％）が、酸化亜鉛のＺｎＯ換算での含有量（モル％）以下である領域（相）である。 In this embodiment, both the A phase and the B phase have at least iron oxide, copper oxide, zinc oxide, and nickel oxide as constituent components, and the A phase and B depend on the content ratio of iron oxide and zinc oxide. It is divided into phases. That is, the A phase is a region (phase) in which the content (mol%) of iron oxide in terms of Fe 2 O 3 is larger than the content (mol%) of zinc oxide in terms of ZnO. The B phase is a region (phase) in which the content (mol%) of iron oxide in terms of Fe 2 O 3 is equal to or less than the content (mol%) of zinc oxide in terms of ZnO.
本実施形態では、主成分１００モル％中の酸化鉄の含有量と、フェライト焼結体におけるＡ相の面積およびＢ相の面積の合計１００％に対するＡ相の面積割合と、を制御している。具体的には、主成分１００モル％中のＦｅ２Ｏ３の含有量を「ｘ」（モル％）とし、Ａ相の面積割合を「ｙ」（％）とした場合、変数（ｘ，ｙ）が、図２に示す点Ａ（４６，９７）、点Ｂ（４６，８３）、点Ｃ（４７．９，７０）および点Ｄ（４７．９，８５）を頂点とする四角形に囲まれる領域内（線上を含む）にある（図２の斜線部）。すなわち、主成分１００モル％中、酸化鉄の含有量は、Ｆｅ２Ｏ３換算で、４６．０〜４７．９モル％である。なお、酸化鉄の含有量は、主成分を１００モル％としたときに、酸化鉄がＦｅ２Ｏ３換算で占める量であり、特定の相における含有量ではない。 In the present embodiment, the content of iron oxide in 100 mol% of the main component and the area ratio of the A phase with respect to 100% of the total area of the A phase and the B phase in the ferrite sintered body are controlled. . Specifically, when the content of Fe 2 O 3 in 100 mol% of the main component is “x” (mol%) and the area ratio of the A phase is “y” (%), the variable (x, y ) Are surrounded by a rectangle having points A (46, 97), B (46, 83), C (47.9, 70) and D (47.9, 85) as vertices shown in FIG. It is within the area (including the line) (shaded area in FIG. 2). That is, in the main component 100 mol%, the content of iron oxide, calculated as Fe 2 O 3 is from 46.0 to 47.9 mol%. The content of iron oxide is the amount that iron oxide occupies in terms of Fe 2 O 3 when the main component is 100 mol%, and is not the content in a specific phase.
フェライト焼結体中において、主成分中の酸化鉄の含有量と、Ａ相の面積割合と、が上記の関係を満足することで、初透磁率を特定の範囲にしつつ、フェライト焼結体の初透磁率の温度特性を良好にすることができる。具体的には、−４０〜８５℃、２５〜８５℃および２５〜１２５℃での各温度範囲において、２５℃における初透磁率に対する変化率（Δμｉ／μｉ２５℃）を−５．０〜＋５．０％とすることができる。 In the ferrite sintered body, the content of the iron oxide in the main component and the area ratio of the A phase satisfy the above relationship, so that the initial permeability is in a specific range, and the ferrite sintered body The temperature characteristics of the initial permeability can be improved. Specifically, in each temperature range of −40 to 85 ° C., 25 to 85 ° C., and 25 to 125 ° C., the change rate (Δμi / μi 25 ° C. ) with respect to the initial permeability at 25 ° C. is −5.0 to +5. 0.0%.
Ａ相およびＢ相の面積を求める方法については特に制限されないが、本実施形態では、たとえば以下のようにして求めることができる。まず、フェライト焼結体を切断し研磨する。研磨面に対して、電子線マイクロアナライザ（ＥＰＭＡ）を用いて、特定の領域（たとえば１００μｍ×１００μｍの正方形領域）について、面分析を行う。 The method for obtaining the areas of the A phase and the B phase is not particularly limited, but in the present embodiment, for example, it can be obtained as follows. First, the ferrite sintered body is cut and polished. A surface analysis is performed on the polished surface of a specific region (for example, a 100 μm × 100 μm square region) using an electron beam microanalyzer (EPMA).
測定点において得られる各元素の含有割合から、Ｆｅ元素のＦｅ２Ｏ３換算での含有割合がＺｎ元素のＺｎＯ換算での含有割合よりも大きい測定点の集合（領域）をＡ相とし、Ｆｅ元素のＦｅ２Ｏ３換算での含有割合が、Ｚｎ元素のＺｎＯ換算での含有割合以下である測定点の集合（領域）をＢ相とする。 From the content ratio of each element obtained at the measurement point, a set (area) of measurement points in which the content ratio of Fe element in terms of Fe 2 O 3 is larger than the content ratio of Zn element in terms of ZnO is defined as A phase, and Fe A set (region) of measurement points in which the content ratio of the element in terms of Fe 2 O 3 is equal to or less than the content ratio of the Zn element in terms of ZnO is defined as a B phase.
そして、面分析を行った領域のマッピング画像について画像処理等を行うことにより、Ａ相およびＢ相の面積を算出し、これらの値からＡ相の面積割合を算出すればよい。 Then, the area of the A phase and the B phase is calculated by performing image processing or the like on the mapping image of the area subjected to the surface analysis, and the area ratio of the A phase may be calculated from these values.
なお、ＥＰＭＡを用いて面分析を行う領域全体がＡ相およびＢ相から構成されている必要はなく、該領域内に、Ａ相およびＢ相以外の相が存在していてもよい。この場合であっても、上記のＡ相の面積割合は、Ａ相の面積とＢ相の面積との合計１００％に対する割合として算出される。 In addition, the whole area | region which performs surface analysis using EPMA does not need to be comprised from A phase and B phase, and phases other than A phase and B phase may exist in this area | region. Even in this case, the area ratio of the A phase is calculated as a ratio with respect to a total of 100% of the area of the A phase and the area of the B phase.
上述したＡ相およびＢ相の面積比は、後述するが、焼成条件の制御や酸化亜鉛の原料を複数用いることで容易に実現することができる。 The area ratio of the A phase and the B phase described above can be easily realized by controlling firing conditions and using a plurality of zinc oxide raw materials.
フェライト焼結体における他の成分の含有量は、酸化鉄の含有量が上記の範囲であれば特に制限されないが、本実施形態では、以下の範囲にあることが好ましい。 The content of other components in the ferrite sintered body is not particularly limited as long as the content of iron oxide is in the above range, but in the present embodiment, it is preferably in the following range.
主成分１００モル％中、酸化銅の含有量は、ＣｕＯ換算で、好ましくは２．０〜８．０モル％、より好ましくは４．０〜６．０モル％である。 In 100 mol% of the main component, the content of copper oxide is preferably 2.0 to 8.0 mol%, more preferably 4.0 to 6.0 mol% in terms of CuO.
主成分１００モル％中、酸化亜鉛の含有量は、ＺｎＯ換算で、好ましくは２８．０〜３４．０モル％、より好ましくは３０．０〜３２．０モル％である。 In 100 mol% of the main component, the content of zinc oxide is preferably 28.0 to 34.0 mol%, more preferably 30.0 to 32.0 mol% in terms of ZnO.
主成分１００モル％中、酸化ニッケルの含有量は、ＮｉＯ換算で、好ましくは１２．０〜２０．０モル％、より好ましくは１４．０〜１６．０モル％である。 In 100 mol% of the main component, the content of nickel oxide is preferably 12.0 to 20.0 mol%, more preferably 14.0 to 16.0 mol% in terms of NiO.
本実施形態に係るフェライト焼結体は、上記の主成分に加え、該フェライト焼結体が有する効果を低下させない程度であれば、所望の特性を得るために、副成分を含有してもよい。副成分としては、特に制限されないが、たとえば、酸化タングステン、酸化モリブデン、酸化ビスマスなどが挙げられる。 In addition to the above main components, the ferrite sintered body according to the present embodiment may contain subcomponents in order to obtain desired characteristics as long as the effects of the ferrite sintered body are not reduced. . The subcomponent is not particularly limited, and examples thereof include tungsten oxide, molybdenum oxide, bismuth oxide and the like.
また、本実施形態に係るフェライト焼結体には、不可避的不純物元素の酸化物が含まれ得る。 In addition, the ferrite sintered body according to the present embodiment may include oxides of inevitable impurity elements.
具体的には、Ｂ、Ｃ、Ｓｉ、Ｐ、Ｓ、Ｃｌ、Ａｓ、Ｓｅ、Ｂｒ、Ｔｅ、Ｉや、Ｌｉ、Ｎａ、Ｍｇ、Ａｌ、Ｋ、Ｃａ、Ｇａ、Ｇｅ、Ｓｒ、Ｃｄ、Ｉｎ、Ｓｎ、Ｓｂ、Ｂａ、Ｐｂ等の典型金属元素や、Ｓｃ、Ｔｉ、Ｖ、Ｃｒ、Ｍｎ、Ｃｏ、Ｙ、Ｚｒ、Ｎｂ、Ｐｄ、Ａｇ、Ｈｆ、Ｔａ等の遷移金属元素が挙げられる。 Specifically, B, C, Si, P, S, Cl, As, Se, Br, Te, I, Li, Na, Mg, Al, K, Ca, Ga, Ge, Sr, Cd, In, Typical metal elements such as Sn, Sb, Ba, and Pb, and transition metal elements such as Sc, Ti, V, Cr, Mn, Co, Y, Zr, Nb, Pd, Ag, Hf, and Ta can be given.
次に、本実施形態に係るフェライト焼結体の製造方法の一例を説明する。 Next, an example of a method for manufacturing a ferrite sintered body according to the present embodiment will be described.
まず、出発原料として、主成分の原料を準備する。主成分の原料としては、酸化鉄（α−Ｆｅ２Ｏ３ ）、酸化銅（ＣｕＯ）、酸化亜鉛（ＺｎＯ）、酸化ニッケル（ＮｉＯ）、あるいは複合酸化物などを用いることができる。さらに、その他、焼成により上記した酸化物や複合酸化物となる各種化合物等を用いることができる。焼成により上記した酸化物になるものとしては、たとえば、金属単体、炭酸塩、シュウ酸塩、硝酸塩、水酸化物、ハロゲン化物、有機金属化合物等が挙げられる。 First, a main component material is prepared as a starting material. As a raw material of the main component, iron oxide (α-Fe 2 O 3 ), copper oxide (CuO), zinc oxide (ZnO), nickel oxide (NiO), composite oxide, or the like can be used. In addition, various compounds that become oxides or composite oxides by firing can be used. Examples of the oxide that becomes the above-mentioned oxide upon firing include simple metals, carbonates, oxalates, nitrates, hydroxides, halides, organometallic compounds, and the like.
酸化亜鉛の原料としては、２種類以上の原料を用いることが好ましく、特に、主成分の他の原料（酸化鉄等）と仮焼きを行う原料と、仮焼きを行わない原料と、を用いることが好ましい。 As the raw material for zinc oxide, it is preferable to use two or more kinds of raw materials, and in particular, other raw materials (such as iron oxide) of the main component, a raw material to be calcined, and a raw material not to be calcined Is preferred.
仮焼きを行わない原料としては、金属亜鉛、酸化亜鉛、炭酸亜鉛、塩化亜鉛、亜鉛を含む複合酸化物などを用いることが好ましい。酸化亜鉛の原料として２種類以上の原料を用いることで、焼成後のフェライト焼結体において、上述したＡ相の面積割合を制御することが容易となる。 As a raw material not to be calcined, it is preferable to use metal zinc, zinc oxide, zinc carbonate, zinc chloride, a composite oxide containing zinc, or the like. By using two or more kinds of raw materials as the raw material for zinc oxide, it becomes easy to control the area ratio of the A phase described above in the sintered ferrite body after firing.
フェライト焼結体に副成分が含有される場合には、副成分の原料として、上記と同様に、該成分の酸化物や混合物、複合酸化物を用いることができる。また、その他、焼成により上記した酸化物や複合酸化物となる各種化合物を用いることができる。 When the ferrite sintered body contains a subcomponent, the component oxide, mixture, or composite oxide can be used as a subcomponent material in the same manner as described above. In addition, various compounds that become oxides or composite oxides by firing can be used.
準備した出発原料を、所定の組成比となるように秤量して混合し、原料混合物を得る。混合する方法としては、たとえば、ボールミルを用いて行う湿式混合や、乾式ミキサーを用いて行う乾式混合が挙げられる。なお、仮焼きを行わない原料は、原料混合物には含ませず、後述する原料混合物の仮焼き後に添加することが好ましい。また、平均粒径が０．１〜３μｍの出発原料を用いることが好ましい。 The prepared starting materials are weighed and mixed so as to have a predetermined composition ratio to obtain a raw material mixture. Examples of the mixing method include wet mixing using a ball mill and dry mixing using a dry mixer. In addition, it is preferable not to include the raw material which does not perform calcination in a raw material mixture, but to add after the calcination of the raw material mixture mentioned later. Further, it is preferable to use a starting material having an average particle diameter of 0.1 to 3 μm.
次に、原料混合物の仮焼きを行い、仮焼き材料を得る。仮焼きは、好ましくは８００〜１１００℃の温度で、通常１〜３時間程度行う。仮焼きは、大気（空気）中で行ってもよく、大気中よりも酸素分圧が高い雰囲気や純酸素雰囲気で行っても良い。 Next, the raw material mixture is calcined to obtain a calcined material. The calcining is preferably performed at a temperature of 800 to 1100 ° C., usually for about 1 to 3 hours. The calcination may be performed in the air (air), or may be performed in an atmosphere having a higher oxygen partial pressure or in a pure oxygen atmosphere than in the air.
次に、仮焼き材料の粉砕を行い、粉砕材料を得る。粉砕は、粗粉砕を行ってからさらに微粉砕を行ってもよい。微粉砕は、ボールミルやアトライターなどを用いた湿式粉砕を行うことが好ましい。湿式粉砕は、仮焼き材料の平均粒径が、好ましくは１〜２μｍ程度となるまで行う。仮焼きを行わない原料は、仮焼き材料の粗粉砕前に添加してもよいし、粗粉砕後に添加してもよい。 Next, the calcined material is pulverized to obtain a pulverized material. The pulverization may be performed after coarse pulverization and further fine pulverization. The fine pulverization is preferably performed by wet pulverization using a ball mill or an attritor. The wet pulverization is performed until the average particle diameter of the calcined material is preferably about 1 to 2 μm. The raw material that is not calcined may be added before coarse pulverization of the calcined material, or may be added after coarse pulverization.
次に、粉砕材料の造粒（顆粒）を行い、造粒物を得る。造粒する方法としては、たとえば、加圧造粒法やスプレードライ法などが挙げられる。スプレードライ法は、粉砕材料に、ポリビニルアルコールなどの通常用いられるバインダを加えた後、スプレードライヤー中で霧化し、低温乾燥する方法である。 Next, the pulverized material is granulated (granular) to obtain a granulated product. Examples of the granulation method include a pressure granulation method and a spray drying method. The spray drying method is a method in which a commonly used binder such as polyvinyl alcohol is added to the pulverized material, and then atomized in a spray dryer and dried at a low temperature.
次に、造粒物を所定形状に成形し、成形体を得る。造粒物の成形としては、たとえば、乾式成形、湿式成形、押出成形などが挙げられる。乾式成形法は、造粒物を、金型に充填して圧縮加圧（プレス）することにより行う成形法である。成形体の形状は、特に限定されず、用途に応じて適宜決定すればよいが、本実施形態ではトロイダル型形状とされる。 Next, the granulated product is molded into a predetermined shape to obtain a molded body. Examples of the molding of the granulated product include dry molding, wet molding, and extrusion molding. The dry molding method is a molding method in which a granulated product is filled in a mold and compressed and pressed (pressed). The shape of the molded body is not particularly limited, and may be appropriately determined according to the application. In the present embodiment, the shape is a toroidal shape.
次に、成形体の本焼成を行い、焼結体（本実施形態のフェライト焼結体）を得る。本焼成は、好ましくは９００〜１３００℃の温度で、通常２〜５時間程度行う。本焼成は、大気（空気）中で行ってもよく、大気中よりも酸素分圧が高い雰囲気で行っても良い。 Next, the compact is fired to obtain a sintered body (ferrite sintered body of the present embodiment). The main baking is preferably performed at a temperature of 900 to 1300 ° C., usually for about 2 to 5 hours. The main calcination may be performed in the atmosphere (air) or in an atmosphere having a higher oxygen partial pressure than in the atmosphere.
このような工程を経て、本実施形態に係るフェライト焼結体は製造される。 The ferrite sintered body according to the present embodiment is manufactured through such steps.
以上、本発明の実施形態について説明してきたが、本発明はこうした実施形態に何等限定されるものではなく、本発明の要旨を逸脱しない範囲内において種々なる態様で実施し得ることは勿論である。 As mentioned above, although embodiment of this invention was described, this invention is not limited to such embodiment at all, Of course, in the range which does not deviate from the summary of this invention, it can implement in various aspects. .
たとえば、上述した実施形態では、トロイダル型形状とするために、本焼成前に該形状に成形しているが、本焼成後に該形状に成形（加工）してもよい。 For example, in the above-described embodiment, in order to obtain a toroidal shape, the shape is formed before the main baking, but may be formed (processed) after the main baking.
以下、本発明を、さらに詳細な実施例に基づき説明するが、本発明は、これら実施例に限定されない。 Hereinafter, although this invention is demonstrated based on a more detailed Example, this invention is not limited to these Examples.
まず、フェライト焼結体の原料として、Ｆｅ２Ｏ３、ＮｉＯ、ＣｕＯ、ＺｎＯおよび表１に示す原料を準備した。 First, as raw materials for the ferrite sintered body, Fe 2 O 3 , NiO, CuO, ZnO and raw materials shown in Table 1 were prepared.
次に、Ｆｅ２Ｏ３、ＮｉＯ、ＣｕＯ、ＺｎＯの各粉末を秤量した後、ボールミルで５時間湿式混合して原料混合物を得た。 Next, each powder of Fe 2 O 3 , NiO, CuO, and ZnO was weighed and then wet-mixed with a ball mill for 5 hours to obtain a raw material mixture.
次に、得られた原料混合物を、空気中において９００℃で２時間仮焼きして仮焼き材料を得た。この仮焼き材料に対し、表１に示す原料を、仮焼き材料１００重量％に表１に示す割合の範囲内で添加し、ボールミルで比表面積が３ｍ２／ｇとなるまで湿式粉砕して粉砕材料を得た。なお、表１に示すＺｎＯは、平均粒径５μｍの粉体と、平均粒径１μｍの粉体と、を１：１の割合で混合した粉体である。 Next, the obtained raw material mixture was calcined in the air at 900 ° C. for 2 hours to obtain a calcined material. To this calcined material, the raw materials shown in Table 1 are added to 100% by weight of the calcined material within the range shown in Table 1, and wet pulverized with a ball mill until the specific surface area becomes 3 m 2 / g. Obtained material. ZnO shown in Table 1 is a powder obtained by mixing a powder having an average particle diameter of 5 μm and a powder having an average particle diameter of 1 μm at a ratio of 1: 1.
次に、この粉砕材料を乾燥した後、該粉砕材料１００重量％に、バインダとしてのポリビニルアルコール（３重量％水溶液）を１０重量％添加して造粒し、２０メッシュの篩で整粒して顆粒とした。この顆粒を、１００ｋＰａの圧力で加圧成形して、トロイダル形状の成形体を得た。 Next, after drying this pulverized material, 10% by weight of polyvinyl alcohol (3% by weight aqueous solution) as a binder was added to 100% by weight of the pulverized material, granulated, and sized with a 20 mesh sieve. Granules were used. This granule was press-molded at a pressure of 100 kPa to obtain a toroidal shaped compact.
次に、これら各成形体を、空気中において、１１５０℃で２時間焼成して、焼結体としてのトロイダルコアサンプル（外径１８ｍｍ×内径１０ｍｍ×高さ５ｍｍ）を得た。得られたサンプルについて、蛍光Ｘ線分析を行い、フェライトコアの組成を測定した。また、フェライトコアに対し以下の特性評価を行った。
Next, each of these molded bodies was fired in air at 1150 ° C. for 2 hours to obtain a toroidal core sample (outer diameter 18 mm ×
（Ａ相およびＢ相の面積比の測定）
得られたサンプルを切断し、樹脂に埋め込んだ後、研磨し、その研磨面に対しＥＰＭＡ分析を行った。電子線マイクロアナライザ（島津製作所製ＥＰＭＡ−１６００）を用いて、１００μｍ×１００μｍの正方形領域に対し、加速電圧１５ｋＶ、照射電流０．３μＡ、計数時間６０秒の条件でマッピング分析を行った。
(Measurement of area ratio of A phase and B phase)
The obtained sample was cut, embedded in resin, polished, and EPMA analysis was performed on the polished surface. Using an electron beam microanalyzer (EPMA-1600 manufactured by Shimadzu Corporation), mapping analysis was performed on a 100 μm × 100 μm square region under conditions of an acceleration voltage of 15 kV, an irradiation current of 0.3 μA, and a counting time of 60 seconds.
得られたマッピング分析における各測定点でのＦｅ元素およびＺｎ元素の含有割合の大小から、測定領域においてＡ相とＢ相とに分け、その面積比率を求めた。結果を表２および図３に示す。 From the magnitude of the content ratio of Fe element and Zn element at each measurement point in the obtained mapping analysis, the area ratio was obtained by dividing into the A phase and the B phase in the measurement region. The results are shown in Table 2 and FIG.
（初透磁率（μｉ））
得られたトロイダルコアサンプルに、巻線を２０回巻回した後、ＬＣＲメータ（アジレント社製４２８４Ａ）を用いて、初透磁率μｉを測定した。測定条件は、測定周波数１ｋＨｚ、測定温度２５℃、測定レベル０．４ｍＡとした。本実施例では、２５℃における初透磁率が３５０〜７００の範囲内にある試料を良好とした。
(Initial permeability (μi))
After winding the winding around the obtained toroidal core sample 20 times, the initial permeability μi was measured using an LCR meter (4284A manufactured by Agilent). The measurement conditions were a measurement frequency of 1 kHz, a measurement temperature of 25 ° C., and a measurement level of 0.4 mA. In this example, a sample having an initial permeability in the range of 350 to 700 at 25 ° C. was considered good.
（初透磁率の温度特性）
続いて、上記の測定条件において、−４０〜１２５℃における初透磁率（μｉ）を測定した。得られた初透磁率から、２５℃における初透磁率に対する変化率（Δμｉ／μｉ）を算出した。本実施例では、−４０〜２５℃におけるΔμｉ／μｉ（２５℃）（＝μｉ−４０℃−μｉ２５℃／μｉ２５℃）は−５〜＋５％を良好とし、２５〜８５℃におけるΔμｉ／μｉ（８５℃）（＝μｉ８５℃−μｉ２５℃／μｉ２５℃）は−５〜＋５％を良好とし、２５〜１２５℃におけるΔμｉ／μｉ（１２５℃）（＝μｉ１２５℃−μｉ２５℃／μｉ２５℃）は−５〜＋５％を良好とした。結果を表２に示す。
(Temperature characteristics of initial permeability)
Subsequently, the initial permeability (μi) at −40 to 125 ° C. was measured under the above measurement conditions. From the obtained initial permeability, the rate of change (Δμi / μi) relative to the initial permeability at 25 ° C. was calculated. In this example, Δμi / μi (−25 ° C.) at −40 to 25 ° C. (= μi− 40 ° C. −μi 25 ° C./μi 25 ° C. ) is good from −5 to + 5%, and Δμi / at 25 to 85 ° C. μi (85 ° C.) (= μi 85 ° C. −μi 25 ° C./μi 25 ° C. ) is preferably −5 to + 5%, and Δμi / μi (125 ° C.) at 25 to 125 ° C. (= μi 125 ° C. −μi 25 ° C. / Μi 25 ° C. ) made -5 to + 5% good. The results are shown in Table 2.
表２より、ｘ（Ｆｅ２Ｏ３含有量）と、ｙ（Ａ相面積比率）とが、上述した範囲内である場合には（実施例１〜２０）、幅広い温度範囲において、初透磁率の温度変化を小さくでき、しかも、初透磁率が特定の範囲内（３５０〜７００）にあることが確認できた。また、図３より、実施例１〜２０は、上述した点Ａ〜点Ｄを頂点とする四角形に囲まれた領域内にあることが視覚的に確認できた。 From Table 2, when x (Fe 2 O 3 content) and y (A phase area ratio) are within the above-described ranges (Examples 1 to 20), the initial magnetic permeability in a wide temperature range. Further, it was confirmed that the temperature change of the initial magnetic permeability was in a specific range (350 to 700). Further, from FIG. 3, it was visually confirmed that Examples 1 to 20 were in an area surrounded by a quadrangle having the above points A to D as vertices.
Claims (2)
前記フェライト焼結体が、Ａ相とＢ相とを有し、
前記Ａ相は、前記酸化鉄のＦｅ２Ｏ３換算での含有割合（モル％）が前記酸化亜鉛のＺｎＯ換算での含有割合（モル％）よりも大きい領域であり、前記Ｂ相は、前記酸化鉄のＦｅ２Ｏ３換算での含有割合（モル％）が前記酸化亜鉛のＺｎＯ換算での含有割合（モル％）以下の領域であり、
前記主成分１００モル％に占める前記酸化鉄のＦｅ２Ｏ３換算での含有割合をｘ（モル％）とし、前記Ａ相の面積と前記Ｂ相の面積との合計面積に対する前記Ａ相の面積割合をｙ（％）とした場合に、変数（ｘ，ｙ）が、下記の点Ａ〜Ｄを頂点とする四角形に囲まれた領域内（線上を含む）にあることを特徴とするフェライト焼結体。
点Ａ（４６，９７）
点Ｂ（４６，８３）
点Ｃ（４７．９，７０）
点Ｄ（４７．９，８５） A ferrite sintered body having a spinel structure and having a main component including iron oxide, zinc oxide, copper oxide, and nickel oxide,
The ferrite sintered body has an A phase and a B phase,
The A phase is a region in which the content ratio (mol%) of the iron oxide in terms of Fe 2 O 3 is larger than the content ratio (mol%) of the zinc oxide in terms of ZnO, and the B phase is The content ratio (mol%) of iron oxide in terms of Fe 2 O 3 is a region below the content ratio (mol%) of zinc oxide in terms of ZnO,
The content ratio of the iron oxide in 100 mol% of the main component in terms of Fe 2 O 3 is x (mol%), and the area of the A phase with respect to the total area of the area of the A phase and the area of the B phase When the ratio is y (%), the variable (x, y) is in the region (including the line) surrounded by a quadrangle having the following points A to D as vertices. Union.
Point A (46,97)
Point B (46, 83)
Point C (47.9, 70)
Point D (47.9, 85)
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