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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