JP2017014047A - Ferrite sintered body, and ferrite core - Google Patents
Ferrite sintered body, and ferrite core Download PDFInfo
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Abstract
Description
本発明は、フェライト焼結体、及びフェライトコアに関する。 The present invention relates to a ferrite sintered body and a ferrite core.
フェライト焼結体は、インダクタ、電源用トランス、電磁フィルタ等の電子部品において広範囲に使用されている。これらの電子部品においてコア（磁心）を形成するフェライト焼結体は、フェライトコアと呼ばれている（特許文献１及び２を参照）。 Ferrite sintered bodies are widely used in electronic parts such as inductors, power transformers, and electromagnetic filters. A ferrite sintered body forming a core (magnetic core) in these electronic components is called a ferrite core (see Patent Documents 1 and 2).
インダクタは高い精度が求められるセンシング機器におけるＬＣ共振回路に使用される。しかしながら、従来のフェライトコアを用いたインダクタでは、外気温の変動に伴ってフェライトコアの磁気特性も変動してしまうため、広い温度領域で精度を保つことが困難であった。 An inductor is used for an LC resonance circuit in a sensing device that requires high accuracy. However, in a conventional inductor using a ferrite core, the magnetic characteristics of the ferrite core also vary with changes in the outside air temperature, so it is difficult to maintain accuracy over a wide temperature range.
本発明は、上述の問題点に鑑み、広い温度領域で透磁率の変動が小さいフェライト焼結体及びフェライトコアを提供することを目的とする。 In view of the above-described problems, an object of the present invention is to provide a ferrite sintered body and a ferrite core having a small variation in magnetic permeability over a wide temperature range.
本発明のフェライト焼結体は、４７〜５２ｍｏｌ％のＦｅ２Ｏ３、１４〜２４ｍｏｌ％のＮｉＯ、２９〜３４ｍｏｌ％のＺｎＯを含み、Ｃの含有量は０．００３質量％以下であり、Ｓの含有量は０．０１５質量％以下であり、Ｆｅ２Ｏ３、ＮｉＯ、及びＺｎＯの合計量が９９．８ｍｏｌ％以上である。 Ferrite sintered body of the present invention, 47~52mol% of Fe 2 O 3, comprises 14～24Mol% of NiO, 29~34mol% of ZnO, the content of C is less 0.003 wt%, S Is 0.015 mass% or less, and the total amount of Fe 2 O 3 , NiO, and ZnO is 99.8 mol% or more.
上記フェライト焼結体が、４９〜５１ｍｏｌ％のＦｅ２Ｏ３、１６〜２０ｍｏｌ％のＮｉＯ、３１〜３３ｍｏｌ％のＺｎＯを含むと好ましい。 The ferrite sintered body, 49~51mol% of Fe 2 O 3, preferably containing 16～20Mol% of NiO, 31~33mol% of ZnO.
本発明のフェライトコアは、４７〜５２ｍｏｌ％のＦｅ２Ｏ３、１４〜２４ｍｏｌ％のＮｉＯ、２９〜３４ｍｏｌ％のＺｎＯを含み、Ｃの含有量は０．００３質量％以下であり、Ｓの含有量は０．０１５質量％以下であり、Ｆｅ２Ｏ３、ＮｉＯ、及びＺｎＯの合計量が９９．８ｍｏｌ％以上である。 Ferrite cores of the present invention, 47～52Mol% of Fe 2 O 3, comprises 14～24Mol% of NiO, 29～34Mol% of ZnO, the content of C is less 0.003 wt%, containing S The amount is 0.015 mass% or less, and the total amount of Fe 2 O 3 , NiO, and ZnO is 99.8 mol% or more.
上記フェライトコアが、４９〜５１ｍｏｌ％のＦｅ２Ｏ３、１６〜２０ｍｏｌ％のＮｉＯ、３１〜３３ｍｏｌ％のＺｎＯを含むと好ましい。 The ferrite core, 49~51mol% of Fe 2 O 3, 16~20mol% of NiO, to include 31～33Mol% of ZnO preferred.
本発明によれば、広い温度範囲で透磁率の変動が小さいフェライト焼結体及びフェライトコアを提供することができる。 ADVANTAGE OF THE INVENTION According to this invention, the ferrite sintered compact and ferrite core with which the fluctuation | variation of a magnetic permeability is small in a wide temperature range can be provided.
＜フェライト焼結体＞
本実施形態のフェライト焼結体は、４７〜５２ｍｏｌ％のＦｅ２Ｏ３、１４〜２４ｍｏｌ％のＮｉＯ、２９〜３４ｍｏｌ％のＺｎＯを含み、Ｃの含有量は０．００３質量％以下であり、Ｓの含有量は０．０１５質量％以下であり、Ｆｅ２Ｏ３、ＮｉＯ、及びＺｎＯの合計量が９９．８ｍｏｌ％以上である。このようなフェライト焼結体は、広い温度領域での透磁率の変動が小さい。
<Ferrite sintered body>
Ferrite sintered body of the present embodiment, 47～52Mol% of Fe 2 O 3, comprises 14～24Mol% of NiO, 29～34Mol% of ZnO, the content of C is less 0.003 wt%, The S content is 0.015% by mass or less, and the total amount of Fe 2 O 3 , NiO, and ZnO is 99.8 mol% or more. Such a ferrite sintered body has a small variation in magnetic permeability in a wide temperature range.
上記フェライト焼結体において、Ｆｅ２Ｏ３の含有量は、４９〜５１ｍｏｌ％であると好ましい。ＮｉＯの含有量は、１６〜２０ｍｏｌ％であると好ましい。ＺｎＯの含有量は、３１〜３３ｍｏｌ％であると好ましい。また、Ｆｅ２Ｏ３の含有量は、５０．２〜５１ｍｏｌ％、ＮｉＯの含有量は、１８〜１８．８ｍｏｌ％、ＺｎＯの含有量は、３１〜３１．５ｍｏｌ％であるとさらに好ましい。 In the ferrite sintered body, the content of Fe 2 O 3 is preferably 49 to 51 mol%. The content of NiO is preferably 16 to 20 mol%. The content of ZnO is preferably 31 to 33 mol%. Further, the Fe 2 O 3 content is more preferably 50.2 to 51 mol%, the NiO content is 18 to 18.8 mol%, and the ZnO content is 31 to 31.5 mol%.
上記フェライト焼結体において、Ｆｅ２Ｏ３、ＮｉＯ、及びＺｎＯの合計量が９９．８ｍｏｌ％以上である。上記合計量は、９９．９ｍｏｌ％以上であると好ましい。また、上記フェライト焼結体において、Ｃの含有量は、０．００３質量％以下である。上記フェライト焼結体において、Ｃの含有量が０．００１〜０．００２質量％であると好ましく、Ｃを実質的に含まないことがより好ましい。さらに、上記フェライト焼結体において、Ｓの含有量は、０．０１５質量％以下である。上記フェライト焼結体において、Ｓの含有量が０．００５〜０．０１０質量％であると好ましく、Ｓを実質的に含まないことがより好ましい。ここで、本明細書において、実質的に含まないとは、燃焼法による測定における検出限界値未満であることをいう。また、本実施形態のフェライト焼結体は、Ｆｅ２Ｏ３、ＮｉＯ、及びＺｎＯ以外の成分を実質的に含まなくてもよい。 In the ferrite sintered body, the total amount of Fe 2 O 3 , NiO, and ZnO is 99.8 mol% or more. The total amount is preferably 99.9 mol% or more. In the ferrite sintered body, the content of C is 0.003% by mass or less. In the ferrite sintered body, the C content is preferably 0.001 to 0.002% by mass, and more preferably substantially free of C. Furthermore, in the ferrite sintered body, the content of S is 0.015% by mass or less. In the ferrite sintered body, the content of S is preferably 0.005 to 0.010% by mass, and more preferably substantially free of S. Here, in the present specification, “substantially not contained” means that it is less than the detection limit value in the measurement by the combustion method. Further, the ferrite sintered body of the present embodiment may not substantially contain components other than Fe 2 O 3 , NiO, and ZnO.
上記フェライト焼結体は、−２０℃〜１２０℃での透磁率（比透磁率）の温度係数が２５ｐｐｍ／Ｋ以下であると好ましく、５〜２０ｐｐｍ／Ｋであるとより好ましく、３〜１０ｐｐｍ／Ｋであるとさらに好ましい。−２０℃〜１２０℃での透磁率の温度係数が上記範囲であると、フェライト焼結体を高い精度が求められるセンシング機器で用いた際に外気温の変動の影響を受けにくく、広い温度領域で高精度なセンシング性能が得られる。ここで、透磁率の温度係数とは、ある温度領域での透磁率の最大値と最小値の差を温度変化（２０℃との温度差）で割ったものをいう。また、透磁率は例えば、インピーダンスアナライザにより、周波数１ＭＨｚで測定した値を言う。 The ferrite sintered body preferably has a temperature coefficient of magnetic permeability (relative magnetic permeability) at −20 ° C. to 120 ° C. of 25 ppm / K or less, more preferably 5 to 20 ppm / K, and more preferably 3 to 10 ppm / K. More preferably, it is K. When the temperature coefficient of permeability at −20 ° C. to 120 ° C. is in the above range, the ferrite sintered body is hardly affected by fluctuations in the outside air temperature when used in a sensing device that requires high accuracy, and has a wide temperature range. High-precision sensing performance can be obtained. Here, the temperature coefficient of the permeability means a value obtained by dividing the difference between the maximum value and the minimum value of the magnetic permeability in a certain temperature region by the temperature change (temperature difference from 20 ° C.). Further, the magnetic permeability is a value measured at a frequency of 1 MHz with an impedance analyzer, for example.
上記フェライト焼結体の焼結密度は、５．３〜５．５ｇ／ｃｍ３であることが好ましい。このような密度であると、ボイドの発生率が小さく、外因（温度、湿度、圧力）による透磁率の変動が小となる傾向があるため好ましい。 The sintered density of the ferrite sintered body is preferably 5.3 to 5.5 g / cm 3 . Such a density is preferable because the void generation rate is small and the variation in magnetic permeability due to external factors (temperature, humidity, pressure) tends to be small.
本実施形態のフェライト焼結体は、不可避不純物として、Ｆｅ単体、又はＣｄ、Ｃｏ、Ｃｕ、Ｐｂ、Ｓｉ、若しくはＭｎの酸化物を含んでいてもよい。フェライト焼結体における不可避不純物の合計量は、３００ｍｏｌ ｐｐｍ未満であることが好ましく、これらの不純物を実質的に含まないことが好ましい。 The ferrite sintered body of the present embodiment may contain Fe alone or an oxide of Cd, Co, Cu, Pb, Si, or Mn as an inevitable impurity. The total amount of inevitable impurities in the ferrite sintered body is preferably less than 300 mol ppm, and preferably does not substantially contain these impurities.
＜フェライト焼結体の製造方法＞
本実施形態におけるフェライト焼結体の製造方法について説明する。
まず、Ｆｅ２Ｏ３原料、ＮｉＯ原料、及びＺｎＯ原料を、フェライト焼結体におけるＦｅ２Ｏ３、ＮｉＯ、及びＺｎＯの含有量が上記範囲となるような組成比で混合して原料粉体を得る。Ｆｅ２Ｏ３原料としては、Ｆｅ２Ｏ３粉末、Ｆｅ３Ｏ４粉末等が挙げられる。ＮｉＯ原料としては、ＮｉＯ粉末が挙げられる。ＺｎＯ原料としては、ＺｎＯ粉末が挙げられる。Ｆｅ２Ｏ３原料、ＮｉＯ原料、及びＺｎＯ原料の平均粒径は、０．１〜１０μｍであることが好ましい。また、Ｆｅ２Ｏ３原料、ＮｉＯ原料、及びＺｎＯ原料の純度としては、金属不純物が１００〜１０００質量ｐｐｍであることが好ましい。上記不純物としては、Ｃｄ、Ｃｏ、Ｃｕ、Ｐｂ、Ｓｉ、若しくはＭｎが挙げられる。混合の方法は、湿式であっても乾式であってもよいが、不純物の残留することを防げる観点から、乾式であることが好ましい。
<Method for producing ferrite sintered body>
The manufacturing method of the ferrite sintered compact in this embodiment is demonstrated.
First, the Fe 2 O 3 raw material, the NiO raw material, and the ZnO raw material are mixed at a composition ratio such that the content of Fe 2 O 3 , NiO, and ZnO in the ferrite sintered body is in the above range to obtain a raw material powder. obtain. Examples of the Fe 2 O 3 raw material include Fe 2 O 3 powder and Fe 3 O 4 powder. Examples of the NiO raw material include NiO powder. Examples of the ZnO raw material include ZnO powder. The average particle size of the Fe 2 O 3 raw material, NiO raw material, and ZnO raw material is preferably 0.1 to 10 μm. Further, Fe 2 O 3 raw material, the purity of the NiO material, and ZnO starting materials, it is preferred that the metal impurities are 100 to 1000 mass ppm. Examples of the impurities include Cd, Co, Cu, Pb, Si, or Mn. The mixing method may be wet or dry, but is preferably dry from the viewpoint of preventing impurities from remaining.
次に、上記原料紛体を仮焼成して仮焼成物を得る。仮焼成は、空気中で仮焼成温度８００〜１２００℃、仮焼成時間２〜５０時間の条件で行うことが好ましい。仮焼成後、仮焼成物を粉砕する。次いで、粉砕された仮焼成物を成形し、成形体を得る。成形方法としては、特に制限されないが、一軸プレス、静水圧成形等が挙げられる。成形時の圧力としては５０〜５００ＭＰａであると好ましい。仮焼成時の雰囲気は酸素量が１〜５０体積％である（Ｎ２＋Ｏ２）混合ガスでもよい。 Next, the raw powder is calcined to obtain a calcined product. Pre-baking is preferably performed in air under conditions of a pre-baking temperature of 800 to 1200 ° C. and a pre-baking time of 2 to 50 hours. After the calcination, the calcination product is pulverized. Next, the ground calcined product is molded to obtain a molded body. Although it does not restrict | limit especially as a shaping | molding method, Uniaxial press, an isostatic pressing, etc. are mentioned. The pressure during molding is preferably 50 to 500 MPa. The atmosphere at the time of preliminary firing may be a (N 2 + O 2 ) mixed gas having an oxygen content of 1 to 50% by volume.
ここで、成形体はバインダを含まないことが好ましい。成形体がバインダを実質的に含まない場合、後述の本焼成中に成形体中にボイドが発生することを抑制し、透磁率の温度係数をさらに向上させることができる。また、成形体がバインダを含まないことにより、フェライト焼結体におけるＣ及びＳの含有量を上記範囲とすることができる。また、成形体は、ＣｕＯを実質的に含まないほうが好ましい。ＣｕＯを実質的に含まない場合、本焼成中に成形体中にボイドが発生することを抑制し、透磁率の温度係数をさらに向上させることができる。 Here, it is preferable that a molded object does not contain a binder. When a molded object does not contain a binder substantially, it can suppress that a void generate | occur | produces in a molded object during the below-mentioned main baking, and can further improve the temperature coefficient of magnetic permeability. Moreover, when the compact does not contain a binder, the content of C and S in the ferrite sintered body can be within the above range. Moreover, it is preferable that a molded object does not contain CuO substantially. When CuO is not substantially contained, generation of voids in the molded body during the main firing can be suppressed, and the temperature coefficient of permeability can be further improved.
得られた成形体を本焼成してフェライト焼結体を得る。本焼成は、空気中で本焼成温度１０００〜１５００℃、本焼成時間２〜５０時間の条件で行うことが好ましい。本焼成の雰囲気は酸素量が１〜５０体積％である（Ｎ２＋Ｏ２）混合ガスでもよい。場合によってはＨ２を導入してもよい。 The obtained molded body is subjected to main firing to obtain a ferrite sintered body. The main baking is preferably performed in air under conditions of a main baking temperature of 1000 to 1500 ° C. and a main baking time of 2 to 50 hours. The atmosphere of the main firing may be a (N 2 + O 2 ) mixed gas having an oxygen amount of 1 to 50% by volume. In some cases, H 2 may be introduced.
得られた焼結体を切削又は研磨して、所定の形状を有するフェライトコアを得る。フェライトコアの形状としては、特に限定されないが、棒状、板状等とすることができる。 The obtained sintered body is cut or polished to obtain a ferrite core having a predetermined shape. Although it does not specifically limit as a shape of a ferrite core, It can be set as rod shape, plate shape, etc.
本実施形態のフェライトコアは、広い温度範囲で透磁率の変動が小さい。そのため、高い精度が求められるセンシング機器におけるＬＣ共振回路に好適に使用することができる。 The ferrite core of this embodiment has a small variation in magnetic permeability over a wide temperature range. Therefore, it can be suitably used for an LC resonance circuit in a sensing device that requires high accuracy.
純度９９．９質量％、平均粒径０．５μｍのＦｅ２Ｏ３粉末、ＮｉＯ粉末、ＺｎＯ粉末及びＣｕＯ粉末を表１に示す組成比で混合し、原料粉体を得た。原料粉体を１１００℃で２０時間、仮焼成した。次いで得られた仮焼成体を粉砕し、表１に示す条件（バインダの有無、成形方法）で成形した。ここで、成形方法Ａは、ＣＩＰ（冷間等方圧加圧法）を意味し、成形方法Ｂは、一軸プレスを意味する。得られた成形体を１３５０℃で２０時間、本焼成し、焼結体を得た。得られた焼結体を切削し、外径：１１ｍｍ、内径：６ｍｍ、厚さ：２ｍｍのリング状の透磁率評価用サンプルを得た。 Fe 2 O 3 powder having a purity of 99.9% by mass and an average particle size of 0.5 μm, NiO powder, ZnO powder and CuO powder were mixed at the composition ratio shown in Table 1 to obtain a raw material powder. The raw material powder was calcined at 1100 ° C. for 20 hours. Next, the obtained temporary fired body was pulverized and molded under the conditions shown in Table 1 (presence / absence of binder, molding method). Here, the forming method A means CIP (cold isostatic pressing), and the forming method B means uniaxial press. The obtained molded body was subjected to main firing at 1350 ° C. for 20 hours to obtain a sintered body. The obtained sintered body was cut to obtain a ring-shaped magnetic permeability evaluation sample having an outer diameter of 11 mm, an inner diameter of 6 mm, and a thickness of 2 mm.
＜測定方法＞
上記評価用サンプルについて、燃焼法により、Ｃ及びＳの含有量を測定した。また、金属顕微鏡により、評価用サンプルの表面における５μｍ以上の大きさのボイドの発生量（１ｃｍ２当たり）を測定した。さらに、インピーダンスアナライザを用いて、周波数１ＭＨｚで、室温での透磁率及び−２０〜１２０℃の温度領域での透磁率の温度係数を測定した。測定結果を表１に示す。
<Measurement method>
About the said sample for evaluation, content of C and S was measured by the combustion method. Moreover, the generation amount (per 1 cm 2 ) of voids having a size of 5 μm or more on the surface of the sample for evaluation was measured with a metal microscope. Further, using an impedance analyzer, the magnetic permeability at room temperature and the temperature coefficient of the magnetic permeability in the temperature range of −20 to 120 ° C. were measured at a frequency of 1 MHz. The measurement results are shown in Table 1.
Claims (4)
Ｃの含有量は０．００３質量％以下であり、Ｓの含有量は０．０１５質量％以下であり、
Ｆｅ２Ｏ３、ＮｉＯ、及びＺｎＯの合計量が９９．８ｍｏｌ％以上である、フェライト焼結体。 47～52Mol% of Fe 2 O 3, a ferrite sintered body comprising 14～24Mol% of NiO, and 29～34Mol% of ZnO,
The content of C is 0.003% by mass or less, the content of S is 0.015% by mass or less,
Fe 2 O 3, NiO, and the total amount of ZnO is more than 99.8 mol%, the ferrite sintered body.
Ｃの含有量は０．００３質量％以下であり、Ｓの含有量は０．０１５質量％以下であり、
Ｆｅ２Ｏ３、ＮｉＯ、及びＺｎＯの合計量が９９．８ｍｏｌ％以上である、フェライトコア。 47～52Mol% of Fe 2 O 3, a ferrite core comprising 14～24Mol% of NiO, and 29～34Mol% of ZnO,
The content of C is 0.003% by mass or less, the content of S is 0.015% by mass or less,
Fe 2 O 3, NiO, and the total amount of ZnO is 99.8 mol% or more, the ferrite core.
4. The ferrite core according to claim 3, comprising 49 to 51 mol% Fe 2 O 3 , 16 to 20 mol% NiO, and 31 to 33 mol% ZnO.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH01305503A (en) * | 1988-06-02 | 1989-12-08 | Sumitomo Special Metals Co Ltd | Radio wave absorbing material |
| JPH06251926A (en) * | 1993-02-24 | 1994-09-09 | Sony Corp | Manufacture of nickel-zinc ferrite |
| JPH07142225A (en) * | 1993-11-17 | 1995-06-02 | Kawasaki Steel Corp | Magnetic oxide particles |
| JPH07307212A (en) * | 1994-03-16 | 1995-11-21 | Hitachi Ferrite Ltd | Ni ferrite sintered body and power source core |
| JPH0817617A (en) * | 1994-07-04 | 1996-01-19 | Hitachi Ferrite Ltd | Ni based ferrite core of high permeability and high saturation magnetic flux density and its manufacture |
| JP2002198213A (en) * | 2000-12-25 | 2002-07-12 | Tdk Corp | Low-temperature baked high-performance ferrite material and ferrite part |
| JP2005255489A (en) * | 2004-03-12 | 2005-09-22 | Kyocera Corp | Ferrite sintered compact, method for manufacturing the same, and ferrite core and ferrite coil using the same |
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2015
- 2015-06-30 JP JP2015131249A patent/JP2017014047A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01305503A (en) * | 1988-06-02 | 1989-12-08 | Sumitomo Special Metals Co Ltd | Radio wave absorbing material |
| JPH06251926A (en) * | 1993-02-24 | 1994-09-09 | Sony Corp | Manufacture of nickel-zinc ferrite |
| JPH07142225A (en) * | 1993-11-17 | 1995-06-02 | Kawasaki Steel Corp | Magnetic oxide particles |
| JPH07307212A (en) * | 1994-03-16 | 1995-11-21 | Hitachi Ferrite Ltd | Ni ferrite sintered body and power source core |
| JPH0817617A (en) * | 1994-07-04 | 1996-01-19 | Hitachi Ferrite Ltd | Ni based ferrite core of high permeability and high saturation magnetic flux density and its manufacture |
| JP2002198213A (en) * | 2000-12-25 | 2002-07-12 | Tdk Corp | Low-temperature baked high-performance ferrite material and ferrite part |
| JP2005255489A (en) * | 2004-03-12 | 2005-09-22 | Kyocera Corp | Ferrite sintered compact, method for manufacturing the same, and ferrite core and ferrite coil using the same |
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