JP7094361B2 - Ferrite sintered body and noise filter - Google Patents
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Description
本開示は、フェライト焼結体およびノイズフィルタに関する。 The present disclosure relates to ferrite sintered bodies and noise filters.
近年、物流管理やクレジット決済等に、ＩＣチップを実装した非接触ＩＣカードが広く用いられている。この非接触ＩＣカードは、ＩＣチップとこのＩＣチップに接続されたアンテナを備えており、通信機器との間で電磁波を介して通信するようになっている。しかしながら、外部の電気器具などからのノイズの影響を受けやすく、ノイズを抑制するために、Ｆｅ－Ｚｎ－Ｎｉ－Ｃｕ系フェライト材料からなるフェライト焼結体を用いたノイズフィルタが用いられている。 In recent years, non-contact IC cards equipped with IC chips have been widely used for physical distribution management, credit card payments, and the like. This non-contact IC card includes an IC chip and an antenna connected to the IC chip, and communicates with a communication device via electromagnetic waves. However, it is easily affected by noise from external electric appliances and the like, and in order to suppress the noise, a noise filter using a ferrite sintered body made of a Fe—Zn—Ni—Cu based ferrite material is used.
本件出願人は、このようなフェライト焼結体として、特許文献１（特許第５７２６６１７号公報）で、金属元素として少なくともＦｅ、Ｚｎ、ＮｉおよびＭｎを含有する酸化物からなるフェライト焼結体であって、ＺｎをＺｎＯ換算で２５ｍｏｌ％～５０ｍｏｌ％含有するＺｎＯと、残部がＮｉＯとの混合粉末中に埋設して焼成され、ＦｅをＦｅ2Ｏ3換算で４２～５０ｍｏｌ％、ＺｎをＺｎＯ換算で２０～３０ｍｏｌ％、ＮｉをＮｉＯ換算で２０～３０ｍｏｌ％、ＭｎをＭｎＯ換算で０．０１～０．５ｍｏｌ％含有し、さらに、ＣｕをＣｕＯ換算で８ｍｏｌ％以下（０を含まず）含有するフェライト焼結体を提案している。As such a ferrite sintered body, the applicant of the present invention is a ferrite sintered body composed of an oxide containing at least Fe, Zn, Ni and Mn as a metal element in Patent Document 1 (Japanese Patent Laid-Open No. 5726617). Then, Zn is embedded in a mixed powder of ZnO containing 25 mol% to 50 mol% of Zn in terms of ZnO and the balance of NiO and fired, Fe is 42 to 50 mol% in terms of Fe 2 O 3 , and Zn is converted into ZnO. Ferrite containing 20 to 30 mol%, Ni 20 to 30 mol% in terms of NiO, Mn in 0.01 to 0.5 mol% in terms of MnO, and Cu in 8 mol% or less (not including 0) in terms of CuO. We are proposing a sintered body.
特許文献１で提案されたフェライト焼結体は、周波数１００ＫＨｚで透磁率を高くすることを狙ったものであり、ＺｎＯおよびＮｉＯがそれぞれ適正量で含まれていても、ＺｎＯ／ＮｉＯが適正な比率でなければ、非接触型ＩＣカードで使われる周波数１３．５６ＭＨｚ付近で複素透磁率の実数部分の値がスネークの限界則に従って減少するため、ノイズを十分抑制することができなかった。
The ferrite sintered body proposed in
本開示のフェライト焼結体は、金属元素として少なくともＦｅ、Ｚｎ、ＮｉおよびＣｕの酸化物を主成分として含むフェライト焼結体である。各金属元素の含有量は、ＦｅがＦｅ2Ｏ3換算で４９．２モル％～５０．２モル％、ＺｎがＺｎＯ換算で２１．０モル％～２４．０モル％、ＮｉがＮｉＯ換算で２１．０モル％～２３．０モル％、ＣｕがＣｕＯ換算で４モル％～７モル％であり、ＺｎＯ／ＮｉＯのモル比が０．９６より大きく、少なくとも表層部は複数の気孔を有し、複数の前記気孔の円相当径の歪度Ｓｋは、０．５以上２以下である。 The ferrite sintered body of the present disclosure is a ferrite sintered body containing at least an oxide of Fe, Zn, Ni and Cu as a main component as a metal element. The content of each metal element is 49.2 mol% to 50.2 mol% in terms of Fe 2 O 3 , Zn in 21.0 mol% to 24.0 mol% in terms of ZnO, and Ni in terms of NiO. 21.0 mol% to 23.0 mol%, Cu is 4 mol% to 7 mol% in terms of CuO, the molar ratio of ZnO / NiO is larger than 0.96, and at least the surface layer portion has a plurality of pores. However, the strain degree Sk of the equivalent circle diameters of the plurality of pores is 0.5 or more and 2 or less .
以下、図面を参照して、本開示のフェライト焼結体について詳細に説明する。 Hereinafter, the ferrite sintered body of the present disclosure will be described in detail with reference to the drawings.
本開示のフェライト焼結体は、金属元素として少なくともＦｅ、Ｚｎ、ＮｉおよびＣｕの酸化物を主成分として含むフェライト焼結体であって、各金属元素の含有量は、ＦｅがＦｅ2Ｏ3換算で４９．２モル％～５０．２モル％、ＺｎがＺｎＯ換算で２１．０モル％～２４．０モル％、ＮｉがＮｉＯ換算で２１．０モル％～２３．０モル％、ＣｕがＣｕＯ換算で４モル％～７モル％であり、ＺｎＯ／ＮｉＯのモル比が０．９６より大きい。The ferrite sintered body of the present disclosure is a ferrite sintered body containing at least Fe, Zn, Ni and Cu oxides as main components as metal elements, and the content of each metal element is Fe 2 O 3 for Fe. 49.2 mol% to 50.2 mol% in terms of equivalent, Zn in 21.0 mol% to 24.0 mol% in terms of ZnO, Ni in 21.0 mol% to 23.0 mol% in terms of NiO, Cu It is 4 mol% to 7 mol% in terms of CuO, and the molar ratio of ZnO / NiO is larger than 0.96.
このような構成とすることにより、周波数１３．５６ＭＨｚ付近で複素透磁率の実数部分の値が高くなるので、ノイズを十分抑制することができる。 With such a configuration, the value of the real number portion of the complex magnetic permeability becomes high near the frequency of 13.56 MHz, so that noise can be sufficiently suppressed.
ここで、周波数１３．５６ＭＨｚはＦｅｌｉｃａ（登録商標、ソニー(株)製）等の非接触ＩＣカードに割り当てられている周波数であり、ＩＳＯ／ＩＥＣで標準化されている周波数でもある。 Here, the frequency 13.56 MHz is a frequency assigned to a non-contact IC card such as FeliCa (registered trademark, manufactured by Sony Corporation), and is also a frequency standardized by ISO / IEC.
上記組成範囲の算出方法については、ＩＣＰ（Inductively Coupled Plasma）発光分光分析装置または蛍光Ｘ線分析装置を用いて、Ｆｅ、Ｚｎ、Ｎｉ、Ｃｕの含有量を求めて、それぞれＦｅ2Ｏ3、ＺｎＯ、ＮｉＯ、ＣｕＯに換算し、それぞれの分子量からモル値を算出し、合計１００モル％における占有率を算出することにより求められる。Regarding the calculation method of the above composition range, the contents of Fe, Zn, Ni, and Cu are obtained by using an ICP (Inductively Coupled Plasma) emission spectroscopic analyzer or a fluorescent X-ray analyzer, and Fe 2 O 3 and Zn O are obtained, respectively. , NiO, CuO, and the molar value is calculated from the respective molecular weights, and the occupancy rate in a total of 100 mol% is calculated.
また、複素透磁率については、外径が１３ｍｍ、内径が７ｍｍ、厚みが３ｍｍのフェライト焼結体からなるリング状試料の全周にわたって線径が０．２ｍｍの被膜導線を１０回巻き付けた後、インピ－ダンス・アナライザー（キーサイト・テクノロジー社製、Ｅ４９９１Ａ）に電気的に接続して、高周波電流電圧法を用いて周波数１３．３３ＭＨｚにおける複素透磁率（μ）を測定すればよい。
Regarding the complex magnetic permeability, after winding a coated conductor having a wire diameter of 0.2
また、本開示のフェライト焼結体は、前記主成分の含有量の合計１００質量部に対して、ＭｎをＭｎＯ換算で０．３質量部～０．８質量部含んでいてもよい。 Further, the ferrite sintered body of the present disclosure may contain Mn in an amount of 0.3 part by mass to 0.8 part by mass in terms of MnO with respect to 100 parts by mass of the total content of the main component.
ＭｎのＭｎＯ換算での含有量が上記範囲であると、透磁率を高く保持したまま、さらに飽和磁束密度を高くすることができる。 When the content of Mn in terms of MnO is within the above range, the saturation magnetic flux density can be further increased while maintaining a high magnetic permeability.
また、本開示のフェライト焼結体は、前記主成分の含有量の合計１００質量部に対して、ＡｌをＡｌ2Ｏ3換算で０．０３質量部～０．３質量部含んでいてもよい。Further, the ferrite sintered body of the present disclosure may contain 0.03 parts by mass to 0.3 parts by mass of Al in terms of Al 2 O 3 with respect to 100 parts by mass of the total content of the main component. ..
ＡｌのＡｌ2Ｏ3換算での含有量が０．０３質量部以上であると、温度変化に対して複素透磁率の実数部分μ’の変化を小さくすることができる。一方、ＡｌのＡｌ2Ｏ3換算での含有量が０．３質量部以下であると、温度変化に対して複素透磁率の実数部分μ’の変化を小さくすることができるとともに、実数部分μ’を高くすることができる。When the content of Al in terms of Al 2 O 3 is 0.03 parts by mass or more, the change in the real part μ'of the complex magnetic permeability can be reduced with respect to the temperature change. On the other hand, when the content of Al in terms of Al 2 O 3 is 0.3 parts by mass or less, the change in the real part μ'of the complex magnetic permeability can be made small with respect to the temperature change, and the real part μ'can be reduced. 'Can be raised.
また、本開示のフェライト焼結体は、前記主成分の含有量の合計１００質量部に対して、ＳｉをＳｉＯ2換算で０．０１～０．２質量部含んでいてもよい。Further, the ferrite sintered body of the present disclosure may contain 0.01 to 0.2 parts by mass of Si in terms of SiO 2 with respect to 100 parts by mass of the total content of the main component.
ＳｉのＳｉＯ2換算での含有量が０．０１質量部以上であると、温度変化に対して複素透磁率の実数部分μ’の変化を小さくすることができる。また、ＳｉのＳｉＯ2換算での含有量が０．２質量部以下であると、温度変化に対して複素透磁率の実数部分μ’の変化を小さくすることができるとともに、実数部分μ’を高くすることができる。When the content of Si in terms of SiO 2 is 0.01 parts by mass or more, the change in the real part μ'of the complex magnetic permeability can be reduced with respect to the temperature change. Further, when the content of Si in terms of SiO 2 is 0.2 parts by mass or less, the change in the real part μ'of the complex magnetic permeability can be reduced with respect to the temperature change, and the real part μ'can be reduced. Can be high.
また、本開示のフェライト焼結体は、前記主成分の含有量の合計１００質量部に対して、ＰをＰ2Ｏ5換算で０．０１質量部～０．１質量部含んでいてもよい。Further, the ferrite sintered body of the present disclosure may contain P in an amount of 0.01 part by mass to 0.1 part by mass in terms of P 2 O 5 with respect to 100 parts by mass in total of the content of the main component. ..
ＰのＰ2Ｏ5換算での含有量が上記範囲であると、焼結助剤として作用し、焼結を促進させ緻密化するために、機械的強度を高くすることができるとともに、ヒステリシス損失を抑制することができる。Ｍｎ、Ａｌ、ＳｉおよびＰの各含有量はＩＣＰ発光分光分析装置または蛍光Ｘ線分析装置を用いて、これら各元素の含有量を求めて、それぞれ酸化物に換算すればよい。When the content of P in terms of P 2 O 5 is in the above range, it acts as a sintering aid, and in order to promote sintering and densify, the mechanical strength can be increased and the hysteresis loss can be increased. Can be suppressed. The contents of Mn, Al, Si and P may be determined by using an ICP emission spectrophotometer or a fluorescent X-ray analyzer to determine the content of each of these elements and convert them into oxides.
また、本開示のフェライト焼結体は、少なくとも表層部が複数の気孔を有し、複数の気孔の円相当径の変動係数ＣＶは２以下であってもよい。 Further, in the ferrite sintered body of the present disclosure, at least the surface layer portion may have a plurality of pores, and the coefficient of variation CV of the circle-equivalent diameter of the plurality of pores may be 2 or less.
気孔の円相当径の変動係数ＣＶがこの範囲であると、気孔の円相当径のばらつきが相対的に小さくなり、異常に大きい気孔がほとんどなくなるので、スライス加工やダイシング加工を用いて、ノイズフィルタ等の電子部品を得る場合、気孔の輪郭や内部から異常に大きな脱粒の発生を抑制することができる。特に、複数の気孔の円相当径の変動係数ＣＶは１．５以下であるとよい。 When the coefficient of variation CV of the equivalent circle diameter of the pores is within this range, the variation of the equivalent circle diameter of the pores becomes relatively small and there are almost no abnormally large pores. When an electronic component such as the above is obtained, it is possible to suppress the occurrence of abnormally large grain removal from the contour of the pores and the inside. In particular, the coefficient of variation CV of the equivalent circle diameters of the plurality of pores is preferably 1.5 or less.
ここで、表層部とは、フェライト焼結体の表面から深さ方向で１ｍｍ以内の領域をいう。そして、気孔の円相当径は、以下のようにして求めることができる。 Here, the surface layer portion refers to a region within 1 mm in the depth direction from the surface of the ferrite sintered body. Then, the diameter equivalent to the circle of the pores can be obtained as follows.
フェライト焼結体の表面から深さ方向に平均粒径Ｄ50が３μｍのダイヤモンド砥粒を用いて銅盤にて研磨する。その後、平均粒径Ｄ50が０．５μｍのダイヤモンド砥粒を用いて錫盤にて研磨する。これらの研磨によって得られる研磨面を観察面とする。 Polishing is performed on a copper plate using diamond abrasive grains having an average particle size D50 of 3 μm in the depth direction from the surface of the ferrite sintered body. Then, it is polished on a tin plate using diamond abrasive grains having an average particle size D50 of 0.5 μm. The polished surface obtained by these polishings is used as an observation surface.
そして、観察面を光学顕微鏡を用いて、倍率を１００倍とし、測定対象の範囲を、例えば、横方向の長さを７２０μｍ、縦方向の長さを５４０μｍとして４か所撮影する。次に、撮影した画像のうち、周辺部を除く領域（面積が２２６８５６μｍ2）を計測範囲とし、画像解析ソフト（例えば、三谷商事(株)製、Ｗｉｎ ＲＯＯＦ）を用いてそれぞれ４か所の計測範囲を解析することによって、気孔の円相当径を得ることができる。Then, using an optical microscope, the observation surface is photographed at four locations with a magnification of 100 times and a measurement target range of, for example, a horizontal length of 720 μm and a vertical length of 540 μm. Next, in the captured image, the area excluding the peripheral part (area: 226856 μm 2 ) is set as the measurement range, and measurement is performed at four locations using image analysis software (for example, Win ROOF manufactured by Mitani Shoji Co., Ltd.). By analyzing the range, the diameter equivalent to the circle of the pores can be obtained.
なお、気孔の円相当径の閾値は、０．８６８μｍとすればよい。 The threshold value of the equivalent circle diameter of the pores may be 0.868 μm.
また、本開示のフェライト焼結体は、少なくとも表層部が複数の気孔を有し、複数の気孔の円相当径の尖度Ｋｕが、０．５以上２以下であってもよい。 Further, in the ferrite sintered body of the present disclosure, at least the surface layer portion may have a plurality of pores, and the kurtosis Ku of the diameter corresponding to the circle of the plurality of pores may be 0.5 or more and 2 or less.
気孔の円相当径の尖度Ｋｕがこの範囲であると、気孔の円相当径の分布が狭く、しかも、異常に大きな円相当径の気孔が少なくなるので、表面から深さ方向に研磨しても、偏摩耗を抑制することができる。特に、尖度Ｋｕは０．７以上１．９以下であるとよい。 If the kurtosis Ku of the equivalent circle diameter of the pores is in this range, the distribution of the equivalent circle diameter of the pores is narrow, and the number of pores with an abnormally large equivalent circle diameter is reduced. However, uneven wear can be suppressed. In particular, the kurtosis Ku is preferably 0.7 or more and 1.9 or less.
ここで、尖度Ｋｕとは、分布のピークと裾が正規分布からどれだけ異なっているかを示す指標（統計量）であり、尖度Ｋｕ＞０である場合、鋭いピークと長く太い裾を有する分布となり、尖度Ｋｕ＝０である場合、正規分布となり、尖度Ｋｕ＜０である場合、分布は丸みがかったピークと短く細い尾を有する分布となる。 Here, kurtosis Ku is an index (statistic) indicating how different the peak and tail of the distribution are from the normal distribution, and when kurtosis Ku> 0, it has a sharp peak and a long thick tail. When the kurtosis is Ku = 0, the distribution is normal, and when the kurtosis is Ku <0, the distribution has a rounded peak and a short and thin tail.
また、本開示のフェライト焼結体は、少なくとも表層部が複数の気孔を有し、複数の気孔の円相当径の歪度Ｓｋが、０．５以上２以下であってもよい。 Further, the ferrite sintered body of the present disclosure may have at least a plurality of pores on the surface layer portion, and the skewness Sk of the diameter corresponding to the circle of the plurality of pores may be 0.5 or more and 2 or less.
気孔の円相当径の歪度Ｓｋがこの範囲であると、気孔の円相当径の平均値が小さく、しかも、異常に大きな円相当径の気孔が少なくなるので、表面から深さ方向に研磨しても、偏摩耗を抑制することができる。特に、歪度Ｓｋは０．７以上１．９以下であるとよい。 When the skewness Sk of the equivalent circle diameter of the pores is in this range, the average value of the equivalent circle diameter of the pores is small, and the number of pores having an abnormally large equivalent circle diameter is reduced. However, uneven wear can be suppressed. In particular, the skewness Sk is preferably 0.7 or more and 1.9 or less.
ここで、歪度Ｓｋとは、分布が正規分布からどれだけ歪んでいるか、即ち、分布の左右対称性を示す指標（統計量）であり、歪度Ｓｋ＞０である場合、分布の裾は右側に向かい、歪度Ｓｋ＝０である場合、分布は左右対称となり、歪度Ｓｋ＜０である場合、分布の裾は左側に向かう。 Here, the skewness Sk is an index (statistic) indicating how much the distribution is distorted from the normal distribution, that is, the left-right symmetry of the distribution. When the skewness Sk> 0, the tail of the distribution is To the right, when the skewness Sk = 0, the distribution is symmetrical, and when the skewness Sk <0, the tail of the distribution goes to the left.
なお、気孔の円相当径の尖度Ｋｕおよび歪度Ｓｋは、Excel（登録商標、Microsoft Corporation）に備えられている関数ＳＫＥＷを用いて求めればよい。 The kurtosis Ku and skewness Sk of the equivalent circle diameter of the pores may be obtained by using the function SKEW provided in Excel (registered trademark, Microsoft Corporation).
また、本開示のフェライト焼結体は、表層部における気孔の面積率が、例えば、３．２％以下であり、特に、３％以下であるとよい。気孔の面積率は、画像解析ソフト（例えば、三谷商事(株)製、Ｗｉｎ ＲＯＯＦ）を用いて、４か所の上記計測範囲を解析することによって、求めることができる。この場合も気孔の円相当径の閾値は、０．８６８μｍとすればよい。 Further, in the ferrite sintered body of the present disclosure, the area ratio of pores in the surface layer portion is, for example, 3.2% or less, and particularly preferably 3% or less. The area ratio of the pores can be obtained by analyzing the above measurement ranges at four locations using image analysis software (for example, Win ROOF manufactured by Mitani Shoji Co., Ltd.). In this case as well, the threshold value of the equivalent circle diameter of the pores may be 0.868 μm.
図１は、本開示のノイズフィルタの一例を示す斜視図である。 FIG. 1 is a perspective view showing an example of the noise filter of the present disclosure.
図１に示すノイズフィルタ１０は、フェライト焼結体１の両端に外部電極２を備えるものであり、図示していないが、フェライト焼結体１は、フェライトからなる薄い基板の複数枚が積層されたものであり、内部電極を備えるものである。
The
次に、本開示のフェライト焼結体の製造方法の一例について説明する。 Next, an example of the manufacturing method of the ferrite sintered body of the present disclosure will be described.
まず、出発原料として、Ｆｅ、Ｚｎ、ＮｉおよびＣｕの酸化物あるいは焼成によりＦｅ、Ｚｎ、ＮｉおよびＣｕの酸化物を生成する炭酸塩、硝酸塩等（以下、Ｆｅ源粉末、Ｚｎ源粉末、Ｎｉ源粉末、Ｃｕ源粉末と記載することもある。）の金属塩を用意する。このとき平均粒径としては、例えば、Ｆｅが酸化鉄（Ｆｅ2Ｏ3）、Ｚｎが酸化亜鉛（ＺｎＯ）、Ｎｉが酸化ニッケル（ＮｉＯ）およびＣｕが酸化銅（ＣｕＯ）であるとき、それぞれ０．５μｍ以上５μｍ以下とするとよい。First, as a starting material, an oxide of Fe, Zn, Ni and Cu or a carbonate, a nitrate or the like that produces an oxide of Fe, Zn, Ni and Cu by firing (hereinafter, Fe source powder, Zn source powder, Ni source) It may be described as powder or Cu source powder.) Prepare a metal salt. At this time, the average particle size is, for example, 0 when Fe is iron oxide (Fe 2 O 3 ), Zn is zinc oxide (ZnO), Ni is nickel oxide (NiO), and Cu is copper oxide (CuO). It is preferable that the thickness is 5 μm or more and 5 μm or less.
次に、Ｆｅ、Ｚｎ、ＮｉおよびＣｕを酸化物換算した合計１００モル％における組成範囲が、ＦｅがＦｅ2Ｏ3換算で４９．２モル％～５０．２モル％、ＺｎがＺｎＯ換算で２１．０モル％～２４．０モル％、ＮｉがＮｉＯ換算で２１．０モル％～２３．０モル％、ＣｕがＣｕＯ換算で４モル％～７モル％とした上で、ＺｎＯ／ＮｉＯのモル比が０．９６より大きくなるように、Ｆｅ源粉末、Ｚｎ源粉末、Ｎｉ源粉末およびＣｕ源粉末を上記組成となるように秤量する。Next, the composition range in a total of 100 mol% of Fe, Zn, Ni and Cu converted into oxides is 49.2 mol% to 50.2 mol% in terms of Fe 2 O 3 and 21 in terms of Zn O. 0.0 mol% to 24.0 mol%, Ni is 21.0 mol% to 23.0 mol% in terms of NiO, Cu is 4 mol% to 7 mol% in terms of CuO, and then ZnO / NiO mol. The Fe source powder, Zn source powder, Ni source powder and Cu source powder are weighed so as to have the above composition so that the ratio becomes larger than 0.96.
そして、秤量した粉末を、ボールミルや振動ミル等で粉砕混合した後、６００℃以上８００℃以下の温度で２時間以上仮焼することにより、合成された仮焼体（Ａ）を得る。あるいは、秤量した粉末を、ボールミルや振動ミル等で粉砕混合した後、６００℃の温度で２時間以上仮焼することにより仮焼体（Ｂ）を、また、８００℃の温度で２時間以上仮焼することにより仮焼体（Ｃ）をそれぞれ得て、仮焼体（Ｂ）および仮焼体（Ｃ）を質量比率で１：１となるように混合粉体（Ｄ）を得る。 Then, the weighed powder is pulverized and mixed by a ball mill, a vibration mill or the like, and then calcined at a temperature of 600 ° C. or higher and 800 ° C. or lower for 2 hours or longer to obtain a synthesized calcined body (A). Alternatively, the weighed powder is pulverized and mixed with a ball mill, a vibration mill, or the like, and then calcined at a temperature of 600 ° C. for 2 hours or more to prepare the calcined body (B), or at a temperature of 800 ° C. for 2 hours or more. By baking, a calcined body (C) is obtained, and a mixed powder (D) is obtained so that the calcined body (B) and the calcined body (C) have a mass ratio of 1: 1.
次に、Ｍｎ、Ａｌ、ＳｉおよびＰの酸化物粉末の少なくともいずれかを仮焼体（Ａ）または混合粉体（Ｄ）に添加する。Ｍｎの酸化物粉末を添加する場合、フェライト焼結体における主成分の合計１００質量部に対する含有量が、ＭｎＯ換算で０．２質量部～０．８質量部となるように秤量する。 Next, at least one of the oxide powders of Mn, Al, Si and P is added to the calcined product (A) or the mixed powder (D). When the oxide powder of Mn is added, the weight is measured so that the content of the main component in the ferrite sintered body with respect to 100 parts by mass in total is 0.2 parts by mass to 0.8 parts by mass in terms of MnO.
Ａｌの酸化物粉末を添加する場合、フェライト焼結体における主成分の合計１００質量部に対する含有量が、Ａｌ2Ｏ3換算で０．０３質量部～０．３質量部となるように秤量する。When the oxide powder of Al is added, the content is weighed so that the content of the main component in the ferrite sintered body with respect to 100 parts by mass in total is 0.03 part by mass to 0.3 part by mass in terms of Al 2 O 3 . ..
Ｓｉの酸化物粉末を添加する場合、フェライト焼結体における主成分の合計１００質量部に対する含有量が、ＳｉＯ2換算で０．０１質量部～０．２質量部となるように秤量する。When the oxide powder of Si is added, the weight is measured so that the content of the main component in the ferrite sintered body with respect to 100 parts by mass in total is 0.01 part by mass to 0.2 part by mass in terms of SiO 2 .
Ｐの酸化物粉末を添加する場合、フェライト焼結体における主成分の合計１００質量部に対する含有量が、Ｐ2Ｏ5換算で０．０１質量部～０．１質量部となるように秤量する。When the oxide powder of P is added, the content is weighed so that the content of the main component in the ferrite sintered body with respect to a total of 100 parts by mass is 0.01 part by mass to 0.1 part by mass in terms of P 2 O 5 . ..
そして、平均粒径が２μｍ以下となるまで粉砕した後、所定量のバインダを加えてスラリーとし、噴霧造粒装置（スプレードライヤ）を用いて噴霧して造粒することにより球状の顆粒を得る。 Then, after pulverizing until the average particle size becomes 2 μm or less, a predetermined amount of binder is added to form a slurry, which is sprayed and granulated using a spray granulator (spray dryer) to obtain spherical granules.
そして、得られた球状の顆粒を用いてプレス成形して所定形状の成形体を得る。その後、成形体を４００～８００℃の範囲の温度で脱脂処理して脱脂体とした後、これを１０００～１２００℃の最高温度で２～５時間保持して焼成することにより本開示のフェライト焼結体を得ることができる。 Then, the obtained spherical granules are press-molded to obtain a molded product having a predetermined shape. Then, the molded body is degreased at a temperature in the range of 400 to 800 ° C. to obtain a degreased body, which is then held at a maximum temperature of 1000 to 1200 ° C. for 2 to 5 hours and fired to obtain the ferrite firing of the present disclosure. You can get a unity.
気孔の円相当径の変動係数ＣＶが２以下であるフェライト焼結体を得るには、混合粉体（Ｄ）から得られる顆粒を用い、プレス成形における成形圧を、例えば、２００ＭＰａ以上とすればよい。 In order to obtain a ferrite sintered body having a coefficient of variation CV of 2 or less in the equivalent circle diameter of the pores, granules obtained from the mixed powder (D) are used, and the molding pressure in press molding is, for example, 200 MPa or more. good.
気孔の円相当径の尖度Ｋｕは、０．５以上２以下であるフェライト焼結体を得るには、混合粉体（Ｄ）から得られる成形体の脱脂処理における温度を４００～６００°とすればよい。 In order to obtain a ferrite sintered body having a kurtosis of 0.5 or more and 2 or less with a diameter equivalent to a circle of pores, the temperature in the degreasing treatment of the molded body obtained from the mixed powder (D) is set to 400 to 600 °. do it.
気孔の円相当径の歪度Ｓｋは、０．５以上２以下であるフェライト焼結体を得るには、混合粉体（Ｄ）から得られる顆粒を用い、プレス成形における成形圧を２００ＭＰａ以上とした上で、脱脂処理における温度を４００～６００°とすればよい。 In order to obtain a ferrite sintered body having a skewness Sk of the equivalent circle diameter of the pores of 0.5 or more and 2 or less, granules obtained from the mixed powder (D) are used, and the molding pressure in press molding is 200 MPa or more. After that, the temperature in the degreasing treatment may be set to 400 to 600 °.
このようにして得られた本開示のフェライト焼結体をコアとし、コア単独、または、このコアに金属線を巻き付けたコイル部品として、例えば、絶縁や変圧を目的としたインダクタ、変圧器、安定器および電磁石に使用したり、ノイズ除去などを目的とした、バラントランス付ノイズフィルタ等のノイズフィルタに使用したりすることができる。 The ferrite sintered body of the present disclosure thus obtained is used as a core, and the core alone or a coil component in which a metal wire is wound around the core, for example, an inductor, a transformer, or a ballast for the purpose of insulation or transformation. It can be used for instruments and electromagnets, or for noise filters such as noise filters with balun transformers for the purpose of noise removal.
また、図１に示すノイズフィルタを得るには、スライサー等を使用してフェライト焼結体から厚みの薄い基板を切り出すスライス加工を施した後、内部電極となる配線を形成し、ダイサー等を使用してダイシング加工を施してチップ化し、その後、積層し、外部電極を形成すればよい。 Further, in order to obtain the noise filter shown in FIG. 1, a slicer or the like is used to cut out a thin substrate from the ferrite sintered body, and then a wiring to be an internal electrode is formed and a dicer or the like is used. Then, it may be diced to form chips, and then laminated to form an external electrode.
以下、本発明の実施例を具体的に説明するが、本発明はこれらの実施例に限定されるものではない。 Hereinafter, examples of the present invention will be specifically described, but the present invention is not limited to these examples.
Ｆｅ、Ｚｎ、ＮｉおよびＣｕを酸化物換算した合計１００モル％における組成範囲およびＺｎＯ／ＮｉＯのモル比が表１に示す値となるように、Ｆｅ源粉末、Ｚｎ源粉末、Ｎｉ源粉末およびＣｕ源粉末を秤量した。 Fe source powder, Zn source powder, Ni source powder and Cu so that the composition range and the ZnO / NiO molar ratio in a total of 100 mol% in terms of Fe, Zn, Ni and Cu as oxides are the values shown in Table 1. The source powder was weighed.
そして、秤量した粉末を、振動ミルで粉砕混合した後、温度７００℃で２時間仮焼することにより、合成された仮焼体を得た。 Then, the weighed powder was pulverized and mixed with a vibration mill, and then calcined at a temperature of 700 ° C. for 2 hours to obtain a synthesized calcined body.
そして、フェライト焼結体における主成分の合計１００質量部に対するＭｎの含有量がＭｎＯ換算で０．５質量部、Ａｌの含有量がＡｌ2Ｏ3換算で０．１７質量部、Ｓｉの含有量がＳｉＯ2換算で０．１質量部となるようにそれぞれ秤量した。The content of Mn in the ferrite sintered body is 0.5 parts by mass in terms of MnO, the content of Al is 0.17 parts by mass in terms of Al 2 O 3 , and the content of Si is 100 parts by mass in total. Weighed to be 0.1 part by mass in terms of SiO 2 .
そして、平均粒径が２μｍ以下となるまで粉砕した後、所定量のバインダを加えてスラリーとし、噴霧造粒装置（スプレードライヤ）を用いて噴霧して造粒することにより球状の顆粒を得た。 Then, after pulverizing until the average particle size became 2 μm or less, a predetermined amount of binder was added to form a slurry, which was sprayed using a spray granulator (spray dryer) to granulate to obtain spherical granules. ..
そして、得られた球状の顆粒を用いてプレス成形して成形体を得る。その後、成形体を温度６００℃で脱脂処理して脱脂体とした後、これを１１００℃の最高温度で３．５時間保持して焼成することにより、外径が１３ｍｍ、内径が７ｍｍ、厚みが３ｍｍのリング状のフェライト焼結体からなる試料を得た。 Then, the obtained spherical granules are used for press molding to obtain a molded product. Then, the molded body is degreased at a temperature of 600 ° C. to obtain a degreased body, which is then held at a maximum temperature of 1100 ° C. for 3.5 hours and fired to increase the outer diameter to 13 mm, the inner diameter to 7 mm, and the thickness. A sample made of a 3 mm ring-shaped ferrite sintered body was obtained.
各試料の主成分の含有量は、蛍光Ｘ線分析装置を用いて、Ｆｅ、Ｚｎ、Ｎｉ、Ｃｕの含有量を求めて、それぞれＦｅ2Ｏ3、ＺｎＯ、ＮｉＯ、ＣｕＯに換算し、それぞれの分子量からモル値を算出し、合計１００モル％における占有率を算出することにより求め、その値を表１に示した。The content of the main component of each sample was determined by using a fluorescent X-ray analyzer to determine the content of Fe, Zn, Ni, and Cu, and converted to Fe 2O 3 , ZnO, NiO, and CuO, respectively. The molar value was calculated from the molecular weight, and the occupancy rate in a total of 100 mol% was calculated, and the value is shown in Table 1.
また、リング状の試料の全周にわたって線径が０．２ｍｍの被膜導線を１０回巻き付けた後、インピ－ダンス・アナライザー（キーサイト・テクノロジー社製、Ｅ４９９１Ａ）に電気的に接続して、高周波電流電圧法を用いて周波数が１ＭＨｚ～１００ＭＨｚにおける複素透磁率を測定し、その実数部分μ’の値を図２に示した。
Further, after winding a coated conductor having a wire diameter of 0.2
また、参考値として周波数１３．３３ＭＨｚにおける複素透磁率μの実数部分μ’の値を表１に示した。 As a reference value, Table 1 shows the value of the real part μ'of the complex magnetic permeability μ at a frequency of 13.33 MHz.
表１に示すように、試料Ｎｏ２、３はＦｅがＦｅ2Ｏ3換算で４９．２モル％～５０．２モル％、ＺｎがＺｎＯ換算で２１．０モル％～２４．０モル％、ＮｉがＮｉＯ換算で２１．０モル％～２３．０モル％、ＣｕがＣｕＯ換算で４モル％～７モル％であり、ＺｎＯ／ＮｉＯのモル比が０．９６より大きいことから、図２に示すように周波数１３．３３ＭＨｚに近い１３．５６ＭＨｚにおける複素透磁率の実数部分μ’が高く、ノイズを十分抑制することが可能であると言える。As shown in Table 1, in Samples No. 2 and 3, Fe is 49.2 mol% to 50.2 mol% in terms of Fe 2 O 3 , Zn is 21.0 mol% to 24.0 mol% in terms of ZnO, and Ni. Is 21.0 mol% to 23.0 mol% in terms of NiO, Cu is 4 mol% to 7 mol% in terms of CuO, and the molar ratio of ZnO / NiO is larger than 0.96, which is shown in FIG. As described above, the real part μ'of the complex magnetic permeability at 13.56 MHz, which is close to the frequency of 13.33 MHz, is high, and it can be said that noise can be sufficiently suppressed.
１ ：フェライト焼結体
２ ：外部電極1: Ferrite sintered body 2: External electrode
Claims (7)
少なくとも表層部は複数の気孔を有し、
該気孔の円相当径の閾値である円相当径の最小値が０．８６８μｍであり、
前記表層部の気孔の面積率が３．２％以下であり、
複数の前記気孔の円相当径の変動係数ＣＶは２以下であり、
複数の前記気孔の円相当径の歪度Ｓｋは、０．５以上２以下である、フェライト焼結体。 It is a ferrite sintered body containing at least Fe, Zn, Ni and Cu oxides as main components as metal elements, and the content of each metal element is 49.2 mol% to 50 in terms of Fe 2 O 3 . .2 mol%, Zn is 21.0 mol% to 24.0 mol% in terms of ZnO, Ni is 21.0 mol% to 23.0 mol% in terms of NiO, and Cu is 4 mol% to 7 mol in terms of CuO. %, And the molar ratio of ZnO / NiO is larger than 0.96.
At least the surface layer has multiple pores,
The minimum value of the circle equivalent diameter, which is the threshold value of the circle equivalent diameter of the pores, is 0.868 μm.
The area ratio of the pores in the surface layer portion is 3.2% or less, and the area ratio is 3.2% or less.
The coefficient of variation CV of the equivalent circle diameters of the plurality of pores is 2 or less.
A ferrite sintered body having a skewness Sk of a plurality of pores having a diameter equivalent to a circle of 0.5 or more and 2 or less.
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| JP2006143530A (en) | 2004-11-19 | 2006-06-08 | Sumida Corporation | Ni-Zn ferrite composition and magnetic element |
| JP2006273610A (en) | 2005-03-28 | 2006-10-12 | Hitachi Metals Ltd | Ferrite sintered compact |
| JP2010150053A (en) | 2008-12-24 | 2010-07-08 | Nec Tokin Corp | SINTERED COMPACT OF SPINEL TYPE Ni-Cu-Zn-BASED FERRITE |
| JP2011097524A (en) | 2009-11-02 | 2011-05-12 | Tdk Corp | Ferrite composition, magnetic member for antenna element, and antenna element |
| JP2011246343A (en) | 2010-04-27 | 2011-12-08 | Kyocera Corp | Ferrite sintered compact and noise filter equipped with the same |
| JP2012148931A (en) | 2011-01-19 | 2012-08-09 | Tdk Corp | Ferrite sintered body and electronic component |
| JP2016037445A (en) | 2014-08-05 | 2016-03-22 | スカイワークス ソリューションズ, インコーポレイテッドSkyworks Solutions, Inc. | Composition, RF device, modified nickel zinc ferrite composition, and method for fine-tuning nickel zinc ferrite material |
| WO2016196709A1 (en) | 2015-06-02 | 2016-12-08 | Scientific Design Company, Inc. | Porous bodies with enhanced pore architecture |
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| WO2019225699A1 (en) | 2019-11-28 |
| JPWO2019225699A1 (en) | 2021-04-30 |
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