CN110494408A - MnZn系铁氧体烧结体 - Google Patents

MnZn系铁氧体烧结体 Download PDF

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Publication number
CN110494408A
CN110494408A CN201880021725.5A CN201880021725A CN110494408A CN 110494408 A CN110494408 A CN 110494408A CN 201880021725 A CN201880021725 A CN 201880021725A CN 110494408 A CN110494408 A CN 110494408A
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mass parts
scaled
core loss
sintered body
based ferrite
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CN201880021725.5A
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CN110494408B (zh
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三吉康晴
多田智之
小汤原德和
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Proterial Ltd
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Hitachi Metals Ltd
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Abstract

本发明提供一种MnZn系铁氧体烧结体，所述铁氧体烧结体含有：主成分，其包含以Fe2O3换算为53.30～53.80摩尔％的Fe、以ZnO换算为6.90～9.50摩尔％的Zn以及以MnO换算为其余部分的Mn；和副成分，其相对于所述换算时的所述主成分的合计100质量份，包含以SiO2换算为0.003～0.020质量份的Si、以CaCO3换算大于0质量份且为0.35质量份以下的Ca、以Co3O4换算为0.30～0.50质量份的Co、以ZrO2换算为0.03～0.10质量份的Zr以及以Ta2O5换算为0～0.05质量份的Ta，平均晶体粒径为3μm以上且小于8μm，烧结体密度为4.65g/cm3以上。

Description

MnZn系铁氧体烧结体
技术领域
本发明涉及适于在各种电源装置的变压器、电感器(インダクタ)、电抗器(リアクトル)、扼流线圈(チョークコイル)等电子部件的磁芯中使用的MnZn系铁氧体烧结体。
背景技术
近年来正在迅速普及的EV(Electric Vehicle，电动汽车)、PHEV(Plug-in HybridElectric Vehicle，插电式混合动力汽车)等作为电动运输设备之一的电动汽车设有大输出功率的电动机、充电器等设备，这些设备使用耐受高电压、大电流的电子部件。电子部件以线圈和磁芯作为基本构成，磁芯由MnZn系铁氧体烧结体等磁性材料构成。
在此种用途中，不仅在行驶时对电子部件施加各种各样的机械、电负荷，而且使用时的环境温度也多种多样。通常而言，预期由磁芯损耗造成的发热，利用晶体磁各向异性常数K1调整磁芯损耗达到极小的温度，将该温度设定为略高于电子部件所暴露的环境最高温度，防止铁氧体因热失控而失去磁性。
另外，就家用电子设备中使用的电子部件而言，使用例如以使磁芯损耗(也被称作功率损耗)的极小温度为100℃以下的方式设计的MnZn系铁氧体，要求在宽温度范围内为低磁芯损耗。
MnZn系铁氧体的磁芯损耗具有温度依赖性，且在晶体磁各向异性常数K1为0的温度时磁滞损耗小，相对于温度具有极小值。可以通过主要适当地调整MnZn系铁氧体中构成尖晶石的金属离子当中显示正的晶体磁各向异性常数K1的金属离子和显示负的晶体磁各向异性常数K1的金属离子的量，来改变晶体磁各向异性常数K1为0的温度。构成尖晶石的金属离子有作为显示正的K1的金属离子的Fe2+、Co2+等、和作为显示负的K1的金属离子的Fe3+、Mn2+等。可以通过调整Fe2+、Fe3+、Zn2+及Mn2+等金属离子，而较为容易地改变使磁芯损耗达到极小的温度，然而若仅为该调整，则难以改善磁芯损耗的温度依赖性。因而，引入与Fe2+相比具有足够大的晶体磁各向异性常数的Co2+来改善磁芯损耗的温度依赖性。
此种铁氧体的磁芯损耗Pcv一般由磁滞损耗Ph、涡流损耗Pe以及剩余损耗Pr组成。磁滞损耗Ph因直流磁滞而与频率成比例地增加。涡流损耗Pe因涡流而与频率的平方成比例地增加，所述涡流是因电磁感应作用而产生的电动势产生的。剩余损耗Pr是以磁畴壁共振等为要因的剩下的损耗，在500kHz以上的频率下变得明显。即，磁滞损耗Ph、涡流损耗Pe以及剩余损耗Pr随着频率而变化，另外它们在总的磁芯损耗中所占的比例也随着频带而不同。因此，希望有适于所使用的频率、温度的MnZn系铁氧体。
作为在宽温度范围内磁芯损耗低的铁氧体，例如日本特开平05-198416号公开过如下的MnZn系铁氧体，即，向包含52.0～54.7mol％的Fe2O3、31～40mol％的MnO以及6～15mol％的ZnO的基本组成100重量％中，添加0.001～0.030重量％的SiC以及0.02～0.30重量％的CaO，并且添加选自0.01～0.08重量％的氧化铌、0.05～0.40重量％的氧化钛、0.005～0.08重量％的氧化锑、0.02～0.15重量％的氧化钽、0.005～0.20重量％的氧化钒、0.02～0.15重量％的氧化锆、0.02～0.50重量％的氧化锡、0.01～0.50重量％的氧化铝、0.01～1.0重量％的氧化钴、0.02～0.15重量％的氧化铜、0.05～1.0重量％的氧化铪及0.001～0.030重量％的氧化硅中的至少一种。该MnZn系铁氧体在100kHz的频率、200mT的最大磁通密度及100℃的温度下为低磁芯损耗，然而在更高频率(300～500kHz)下在宽温度范围内磁芯损耗并不足够低。
已知Co对于改善磁芯损耗的温度依赖性有效，然而由于包含Co的MnZn系铁氧体中2价的金属离子(Co2+)易于经由晶格缺陷迁移，因此导致磁各向异性的增大，带来磁芯损耗的增加及磁导率的降低这样的磁特性的经时变化，在高温环境下该经时变化大。因此，对于易于暴露于高温的电子部件中所用的MnZn系铁氧体，要求进一步降低磁芯损耗和抑制磁特性的经时变化。
发明内容
发明所要解决的问题
所以，本发明的目的在于，提供一种MnZn系铁氧体烧结体，其在300～500kHz的高频率下在宽温度范围内磁芯损耗低，并且高温环境下的磁芯损耗的经时变化小。
用于解决问题的方法
本发明的MnZn系铁氧体烧结体的特征在于，
所述铁氧体烧结体含有：
主成分，其包含以Fe2O3换算为53.30～53.80摩尔％的Fe、以ZnO换算为6.90～9.50摩尔％的Zn以及以MnO换算为其余部分的Mn；和
副成分，其相对于所述换算时的所述主成分的合计100质量份，包含以SiO2换算为0.003～0.020质量份的Si、以CaCO3换算大于0质量份且为0.35质量份以下的Ca、以Co3O4换算为0.30～0.50质量份的Co、以ZrO2换算为0.03～0.10质量份的Zr以及以Ta2O5换算为0～0.05质量份的Ta，
所述铁氧体烧结体的平均晶体粒径为3μm以上且小于8μm，
所述铁氧体烧结体的烧结体密度为4.65g/cm3以上。
在本发明的MnZn系铁氧体烧结体中，优选Ta含量以Ta2O5换算为0.01质量份以上。
在本发明的MnZn系铁氧体烧结体中，优选Fe含量以Fe2O3换算为53.40～53.70摩尔％，Zn含量以ZnO换算为7.00～9.40摩尔％，Si含量以SiO2换算为0.004～0.015质量份，Co含量以Co3O4换算为0.30～0.45质量份，Zr含量以ZrO2换算为0.05～0.09质量份。
本发明的MnZn系铁氧体烧结体优选(a)在300kHz的频率及100mT的励磁磁通密度下20℃时的磁芯损耗Pcv20为300kW/m3以下，100℃时的磁芯损耗Pcv100为320kW/m3以下，并且(b)在500kHz的频率及100mT的励磁磁通密度下20℃时的磁芯损耗Pcv20为650kW/m3以下，100℃时的磁芯损耗Pcv100为850kW/m3以下。
本发明的MnZn系铁氧体烧结体优选以下述式(1)表示的磁芯损耗的变化率Ps为5％以下：
Ps(％)＝[(Pcv100B－Pcv100A)/Pcv100A]×100···(1)
(其中，Pcv100A为在200℃保持前的100℃时的磁芯损耗，Pcv100B为在200℃保持96小时后的100℃时的磁芯损耗，均为在300kHz的频率及100mT的最大磁通密度下测定的值。)。
发明效果
本发明的MnZn系铁氧体烧结体在300～500kHz的高频率下在宽温度范围内磁芯损耗低，并且高温环境下的磁芯损耗的经时变化小，因此适于暴露于高温下的电子部件中所用的磁芯。
附图说明
图1是示意性地表示用于获得本发明的MnZn系铁氧体烧结体的烧结工序的图表。
具体实施方式
以下详细说明本发明的实施方式，然而本发明并不限定于此，可以在本发明的技术思想的范围内适当地变更。
[1]MnZn系铁氧体烧结体
(A)组成
本发明的MnZn系铁氧体烧结体含有包含Fe、Mn及Zn的主成分和包含Si、Ca、Co以及Zr的副成分。本发明的MnZn系铁氧体烧结体可以还含有Ta作为副成分。主成分是主要构成尖晶石铁氧体的元素，所谓副成分是辅助尖晶石铁氧体的形成的元素。虽然Co构成尖晶石铁氧体，然而在本发明中其含量显著少于主成分，因此设为副成分。
(1)主成分
为降低所期望的温度下的磁芯损耗Pcv，需要适当地调整构成尖晶石的显示正的晶体磁各向异性常数K1的金属离子的量和显示负的晶体磁各向异性常数K1的金属离子的量。但是，由于还需要满足饱和磁通密度Bs、居里温度Tc、初始磁导率μi等磁芯损耗Pcv以外的磁特性的要求，因此组成的选择自由度小。另外，为了在宽温度范围内将磁芯损耗抑制得较小，需要设定磁芯损耗达到极小的温度。因而，为了具有500mT以上的饱和磁通密度Bs、230℃以上的居里温度Tc以及1500以上的初始磁导率μi，以便可以用于在高温下耐受高电压及大电流的使用的电子部件用磁芯，并且为了通过将磁芯损耗的极小温度例如设为100℃以下、优选设为80℃以下而在宽温度范围内为低磁芯损耗，将主成分的组成设为以Fe2O3换算为53.30～53.80摩尔％的Fe、以ZnO换算为6.90～9.50摩尔％的Zn以及以MnO换算为其余部分的Mn。
(a)Fe：53.30～53.80摩尔％(Fe2O3换算)
若Fe含量小于53.30摩尔％，则磁芯损耗的极小温度变高，低温侧的磁芯损耗增大，无法充分地获得20～100℃的温度范围内的磁芯损耗的降低效果。另外，若大于53.80摩尔％，则磁芯损耗的极小温度变低，高温侧的磁芯损耗增大，无法充分地获得20～100℃的温度范围内的磁芯损耗的降低效果。Fe含量的下限优选为53.40摩尔％，更优选为53.45摩尔％。另一方面，Fe含量的上限优选为53.70摩尔％，更优选为53.65摩尔％。
(b)Zn：6.90～9.50摩尔％(ZnO换算)
若Zn含量小于6.90摩尔％，则磁芯损耗的温度变化变大，因而不优选，另外若大于9.50摩尔％，则难以获得足够的饱和磁通密度。Zn含量的下限优选为7.00摩尔％，更优选为8.00摩尔％，最优选为9.10摩尔％。另一方面，Zn含量的上限优选为9.40摩尔％，更优选为9.30摩尔％。
(c)Mn：其余部分(MnO换算)
Mn含量是从主成分(Fe、Zn及Mn)的总量中减去Fe含量及Zn含量而得的其余部分。
(2)副成分
本发明的MnZn系铁氧体烧结体中，作为副成分至少含有Si、Ca、Co及Zr，任选地含有Ta。副成分的组成以相对于所述换算时的所述主成分的合计100质量份而言的质量份表示。
(a)Si：0.003～0.020质量份(SiO2换算)
Si在晶粒间界处偏析而使晶粒绝缘(提高晶界电阻)，减小相对损耗系数tanδ/μi，使涡流损耗降低。其结果是，MnZn系铁氧体烧结体的高频率区域的磁芯损耗降低。若Si含量过少，则提高晶界电阻的效果小，若Si含量过多，则反而诱发晶体的增大，使磁芯损耗劣化。
若以SiO2换算含有0.003～0.020质量份的Si，则可以利用与其他副成分的组合确保足以降低涡流损耗的晶界电阻，可以在300kHz以上的高频率区域将MnZn系铁氧体烧结体设为低损耗。Si含量的下限以SiO2换算优选为0.004质量份，更优选为0.005质量份。另外，Si含量的上限以SiO2换算优选为0.015质量份，更优选为0.012质量份。
(b)Ca：大于0质量份且为0.35质量份以下(CaCO3换算)
Ca在晶粒间界处偏析而使晶粒绝缘(提高晶界电阻)，减小相对损耗系数tanδ/μi，使涡流损耗降低。其结果是，MnZn系铁氧体烧结体的高频率区域的磁芯损耗降低。若Ca含量过少，则提高晶界电阻的效果小，若Ca含量过多，则反而诱发晶体的增大，使磁芯损耗劣化。
若以CaCO3换算含有大于0质量份且为0.35质量份以下的Ca，则可以利用与其他副成分的组合确保足以降低涡流损耗的晶界电阻，可以在300kHz以上的高频率区域中设为低损耗。Ca含量的下限以CaCO3换算优选为0.05质量份，更优选为0.07质量份。另外，Ca含量的上限以CaCO3换算优选为0.30质量份，更优选为0.20质量份。
(c)Co：0.30～0.50质量份(Co3O4换算)
Co是对于改善磁芯损耗的温度依赖性有效的元素。Co2+与Fe2+一起作为具有正的晶体磁各向异性常数K1的金属离子，具有调整磁芯损耗达到最小的温度的效果。另外，Co使残留磁通密度Br降低，使磁滞损耗Ph降低。另一方面，由于Co2+具有比Fe2+大的晶体磁各向异性常数K1，因此若Co的含量过多，则磁化曲线易于变为Perminber型，另外在低温侧中晶体磁各向异性常数在正的一侧变得过大，低温度范围中的损耗的增加显著，而且磁芯损耗的温度依赖性也恶化。另一方面，若Co含量过少，则改善温度依赖性的效果小。
若以Co3O4换算含有0.30～0.50质量份的Co，则可以利用与其他副成分的组合在实用温度范围内降低磁芯损耗，并且可以改善温度依赖性。Co含量的上限以Co3O4换算优选为0.45质量份，更优选为0.40质量份。
(d)Zr：0.03～0.10质量份(ZrO2换算)
以ZrO2换算为0.03～0.10质量份的Zr与Si及Ca一起主要在晶粒间界层处偏析而提高晶界电阻，由此有助于降低损耗，并且减小磁芯损耗的变化率Ps。若Zr含量过少，则磁芯损耗和磁芯损耗的变化率Ps的降低效果小，若Zr含量过多，则产生粗大晶粒生长，磁芯损耗增大。Zr含量的下限以ZrO2换算优选为0.05质量份，更优选为0.06质量份。另外，Zr含量的上限以ZrO2换算优选为0.09质量份，更优选为0.08质量份。
(e)Ta：0～0.05质量份(Ta2O5换算)
由于Ta在晶粒间界层处偏析而提高晶界电阻，因此可以以0.05质量份为上限地含有，也可以为0质量份(不含有)。若Ta含量过多，则Ta侵入晶粒内，使MnZn系铁氧体烧结体的磁芯损耗增大。通过以Ta2O5换算含有0～0.05质量份的Ta，可以确保足以降低涡流损耗的晶界电阻，可以在500KHz以上的高频率区域中，降低特别是高温(100℃)条件下的磁滞损耗及剩余损耗，在高频率区域实现宽温度范围内的低损耗化。在含有Ta的情况下，含量的下限以Ta2O5换算优选为0.01质量份。另外，Ta含量的上限以Ta2O5换算优选为0.04质量份，更优选为0.03质量份。
副成分当中的Si主要在晶粒间界及三相点偏析，而Ca、Zr及Ta具有在烧结工序的途中固溶于尖晶石相、烧结后也有一部分残留于晶粒内的情况。若固溶于尖晶石相的Ca、Zr及Ta变多，则晶粒内的电阻变高，使体积电阻率ρ增加，而晶界的Ca、Zr及Ta的含量减少。为了在提高体积电阻率的同时制成低磁芯损耗的MnZn系铁氧体烧结体，有效的做法是，调整固溶于尖晶石相的Ca、Zr及Ta的比例和在晶粒间界处偏析的Ca、Zr及Ta的比例，提高晶粒内的电阻，并且形成高电阻的晶粒间界。该调整可以利用后述的烧结温度和烧结气氛的控制来进行。
(3)杂质
在构成MnZn系铁氧体烧结体的原料中，有时作为杂质包含硫S、氯Cl、磷P、硼B等。其中S与Ca形成化合物，该化合物在晶粒间界处作为异物偏析，使体积电阻率ρ降低，使涡流损耗增加。根据经验已知，若使这些杂质的含量减少，则可以获得磁芯损耗的降低及磁导率的提高。因此，为了进一步降低磁芯损耗，相对于所述换算时的主成分的合计100质量份，优选将S设为0.03质量份以下，将Cl设为0.01质量份以下，将P设为0.001质量份以下，并且将B设为0.0001质量份以下。
主成分、副成分以及杂质的定量可以利用荧光X射线分析及ICP发光分光分析来进行。预先利用荧光X射线分析进行含有元素的定性分析，然后利用将含有元素与标准样品比较的标准曲线法进行定量。
(B)平均晶体粒径
本发明的MnZn系铁氧体烧结体具有3μ以上且小于8μm的平均晶体粒径。若平均晶体粒径为8μm以上，则涡流损耗及剩余损耗的降低效果不充分，500KHz以下的高频率区域中的磁芯损耗增大。另一方面，若平均晶体粒径小于3μm，则晶界作为磁畴壁的钉扎点(ピンニング点)发挥作用，另外由于退磁场(日文原文：反磁界)的影响而诱发磁导率的降低及磁芯损耗的增加。平均晶体粒径优选为4～7μm。需要说明的是，利用以下的实施例中记载的方法求出平均晶体粒径。
(C)烧结体密度
本发明的MnZn系铁氧体烧结体具有4.65g/cm3以上的密度。若烧结体密度小于4.65g/cm3，则机械强度差，易于产生缺损、破裂。优选的烧结体密度为4.75g/cm3以上。需要说明的是，利用以下的实施例中记载的方法求出烧结体密度。
[2]MnZn系铁氧体烧结体的制造方法
图1表示用于获得本发明的MnZn系铁氧体烧结体的烧结工序的温度条件。所述烧结工序具有升温工序、高温保持工序以及降温工序。通过在烧结工序中调整氧分压，而使Ca、Zr等在晶界处偏析，并且适当地控制固溶于晶粒内的量，使磁芯损耗降低。
(A)升温工序
升温工序当中的从室温直至400～950℃的温度的期间的第1升温工序中，在大气中进行升温，从成形体中除去粘结剂。第1升温工序以后的直至高温保持工序之间的第2升温工序中，优选使气氛中的氧浓度降低为0.01～0.5体积％。在升温工序中，根据脱粘结剂中的碳残留的程度、组成等，适当地选择升温速度。平均升温速度优选为50～200℃/小时的范围内。
(B)高温保持工序
高温保持工序优选将气氛中的氧浓度调整为0.1～0.5体积％，在1150～1250℃的温度进行。高温保持工序的气氛中的氧浓度优选设定为高于第2升温工序的氧浓度。
(C)降温工序
若在降温工序中氧浓度过高，则烧结体的氧化推进，从尖晶石中析出赤铁矿(ヘマタイト)。另一方面，若氧浓度过低，则析出方铁矿(ウスタイト)，产生晶体畸变而使磁芯损耗增加。优选以不引起赤铁矿及方铁矿的析出的方式，控制降温工序的氧浓度。具体而言，优选以使氧浓度PO2(体积率)和温度T(℃)满足下述式(2)的方式，控制降温工序的氧浓度：
log PO2＝a－b/(T+273)···(2)
(其中，a为3.1～12.8的常数，b为6000～20000的常数。)
a由高温保持工序的温度和氧浓度规定。若b小于6000，则即使温度下降，氧浓度也高，氧化推进，有从尖晶石析出赤铁矿的情况。另一方面，若b大于20000，则氧浓度降低而析出方铁矿，晶粒及晶界层均未被充分地氧化，电阻变小。a更优选为6.4～11.5，b更优选为10000～18000。
利用上述烧结工序得到的MnZn系铁氧体烧结体在室温下具有5Ω·m以上的体积电阻率。此外为了降低涡流损耗Pe，体积电阻率优选设为10Ω·m以上。
利用实施例对本发明进一步详细说明，然而本发明并不限定于它们。
实施例1～50以及比较例1～8
作为主成分将Fe2O3粉末、ZnO粉末及Mn3O4粉末以表1所示的配合比湿式混合后，干燥，在900℃煅烧3小时。需要说明的是，表1中将Mn3O4粉末的添加量以MnO换算表示。相对于所得的各煅烧粉100质量份，在球磨机内以表1所示的配合比添加SiO2粉末、CaCO3粉末、Co3O4粉末、ZrO2粉末以及Ta2O5粉末，以表2所示的时间粉碎、混合，直至平均粉碎粒径约为1.2～1.4μm为止。向所得的各混合物中作为粘结剂加入聚乙烯醇并用乳钵进行颗粒化后，加压成形而得到环状的成形体。
对于各成形体，利用由从室温升温到表2所示的保持温度的升温工序、在保持温度保持5小时的高温保持工序以及从保持温度冷却到室温的降温工序组成的烧结工序进行烧结。升温工序中，对于升温速度，直至400℃为止设为50℃/小时，从400℃到保持温度为止设为100℃/小时，对于烧成气氛中的氧浓度，从室温到700℃为止设为21体积％(使用大气)，在到达700℃以后设为0.1体积％。将高温保持工序中的氧浓度表示于表2中。降温工序中，对于冷却速度，从保持温度到900℃为止设为100℃/小时，以后设为150℃/小时。降温工序中，直至1000℃为止以达到平衡氧分压的方式调节氧浓度(体积％)。900℃以后在N2气流中冷却，使最终的氧浓度降低至约0.003体积％。如此所述地操作，得到外径25mm×内径15mm×厚5mm的圆环状的MnZn系铁氧体烧结体(磁芯)。
对于各MnZn系铁氧体烧结体，利用下述的方法测定出密度、体积电阻率ρ、平均晶体粒径、饱和磁通密度Bs、初始磁导率μi以及磁芯损耗Pcv。
(1)烧结体密度
根据各MnZn系铁氧体烧结体的尺寸及重量，利用体积重量法算出密度。将结果表示于表3中。
(2)体积电阻率ρ
从各MnZn系铁氧体烧结体中切出平板状的试样，在相面对的两个平面设置银浆电极，使用日置电机株式会社制milliohm high tester 3224测定出电阻R(Ω)。根据电极形成面的面积A(m2)和厚度t(m)，利用下式(3)算出体积电阻率ρ(Ω·m)。将结果表示于表3中。
ρ(Ω·m)＝R×(A/t)···(3)
(3)平均晶体粒径
对各MnZn系铁氧体烧结体的镜面研磨面的晶粒间界进行热蚀刻(1100℃、1hr、N2中处理)后利用光学显微镜(400倍)拍摄照片，在显微镜照片的100μm×100μm的正方形区域中作为基于求积法的当量圆直径求出平均晶体粒径。将结果表示于表3中。
(4)饱和磁通密度Bs
以各MnZn系铁氧体烧结体作为磁芯，将一次侧绕组(一次側巻線)及二次侧绕组(二次側巻線)分别卷绕40圈后施加1.2kA/m的磁场，使用直流磁化测定试验装置(Metron技研株式会社制SK-110型)在23℃测定出饱和磁通密度Bs。将结果表示于表3中。
(5)初始磁导率μi
以各MnZn系铁氧体烧结体作为磁芯，将绕组卷绕10圈后施加0.4A/m的磁场，使用惠普制HP-4285A，在23℃、100kHz的条件下测定出初始磁导率μi。将结果表示于表3中。
(6)磁芯损耗Pcv
以各MnZn系铁氧体烧结体作为磁芯，将一次侧绕组及二次侧绕组分别卷绕4圈，使用岩崎通信机株式会社制的B-H分析仪(SY-8232)，在300kHz及500kHz的各频率及100mT的励磁磁通密度的条件下，测定出20℃、40℃、60℃、80℃、100℃、120℃及140℃时的磁芯损耗Pcv。将结果表示于表4及表5中。
[表1-1]
[表1-2]
[表1-3]
[表2-1]
注：(1)高温保持工序的气氛中的氧浓度(体积％)。
[表2-2]
注：(1)高温保持工序的气氛中的氧浓度(体积％)。
[表2-3]
注：(1)高温保持工序的气氛中的氧浓度(体积％)。
[表3-1]
注：(1)烧结体密度。
(2)体积电阻率。
(3)平均晶体粒径。
(4)饱和磁通密度。
(5)100kHz及0.4A/m时的初始磁导率。
[表3-2]
注：(1)烧结体密度。
(2)体积电阻率。
(3)平均晶体粒径。
(4)饱和磁通密度。
(5)100kHz及0.4A/m时的初始磁导率。
[表3-3]
注：(1)烧结体密度。
(2)体积电阻率。
(3)平均晶体粒径。
(4)饱和磁通密度。
(5)100kHz及0.4A/m时的初始磁导率。
[表4-1]
[表4-2]
[表4-3]
[表5-1]
[表5-2]
[表5-3]
从表3～表5可以清楚地看到，实施例1～50的MnZn系铁氧体烧结体的初始磁导率μi均为1800以上，在300kHz及500kHz的任意频率下，都在宽温度范围内为低磁芯损耗。与之不同，比较例1～8的MnZn系铁氧体烧结体在300KHz或500KHz下磁芯损耗高。根据以上结果可知，利用本发明可以得到从低温(20℃)到高温(100℃)为低磁芯损耗的MnZn系铁氧体烧结体。
实施例51～53以及比较例9～11
除了设为表6所示的组成及表7所示的制造条件以外，与实施例1同样地制作出MnZn系铁氧体烧结体。对于各MnZn系铁氧体烧结体，与实施例1同样地测定出密度、体积电阻率ρ、平均晶体粒径、初始磁导率μi、磁芯损耗Pcv。需要说明的是，磁芯损耗Pcv的评价在300kHz的频率及100mT的励磁磁通密度的条件下进行。将结果表示于表8～表10中。
继而，在将各MnZn系铁氧体烧结体的磁芯在高温槽内在200℃保持96小时后，从高温槽中取出并将磁芯的温度降低至室温，在与上述相同的条件下在20℃、40℃、60℃、80℃、100℃、120℃及140℃测定磁芯损耗，根据高温环境(200℃)放置前后的磁芯损耗利用下式(1)算出磁芯损耗的变化率Ps。
Ps(％)＝[(PcvB－PcvA)/PcvA]×100···(1)
(其中，PcvA为在高温(200℃)保持前的磁芯的磁芯损耗，PcvB为在高温(200℃)保持后的磁芯的磁芯损耗。)
例如，在求由高温环境(200℃)放置造成的100℃时的磁芯损耗的变化率Ps的情况下，作为PcvA使用在高温(200℃)保持前在100℃、300kHz的频率及100mT的励磁磁通密度的条件下测定的磁芯的磁芯损耗(Pcv100A)，作为PcvB使用在高温(200℃)保持后在100℃、300kHz的频率及100mT的励磁磁通密度的条件下测定的磁芯的磁芯损耗(Pcv100B)。
在高温保持前的磁芯损耗的测定中，以10～15分钟左右将磁芯放置在140℃的气氛的恒温槽内直至温度稳定为止，但实质上没有产生磁特性的经时变化。
[表6]
注：*为了比较，显示出比较例3的数据。
[表7]
注：*为了比较，显示出比较例3的数据。
(1)高温保持工序的气氛中的氧浓度(体积％)。
[表8]
注：*为了比较，显示出比较例3的数据。
(1)烧结体密度。
(2)体积电阻率。
(3)平均晶体粒径。
(4)100kHz及0.4A/m时的初始磁导率。
[表9]
注：*为了比较，显示出比较例3的数据。
[表10]
注：*为了比较，显示出比较例3的数据。
[表11]
注:*为了比较，显示出比较例3的数据。
从表8～表11可以清楚地看到，实施例51～53的MnZn系铁氧体烧结体均为高初始磁导率μi及高体积电阻率，因此在宽温度范围内为低磁芯损耗，并且磁芯损耗的变化率Ps小。与之不同，比较例9的MnZn系铁氧体烧结体虽然初始磁导率μi高，然而体积电阻率低，因此磁芯损耗高，磁芯损耗的变化率Ps也大。比较例10的MnZn系铁氧体烧结体虽然体积电阻率高，然而初始磁导率μi也高，因此磁芯损耗高，磁芯损耗的变化率Ps也大。另外，比较例3及11的MnZn系铁氧体烧结体由于体积电阻率及初始磁导率μi低，因此磁芯损耗的变化率Ps小，然而磁芯损耗高。根据以上结果可知，利用本发明可以得到从低温(20℃)到高温(100℃)为低磁芯损耗的MnZn系铁氧体烧结体。

Claims (5)

1.一种MnZn系铁氧体烧结体，其特征在于，
所述铁氧体烧结体含有：
主成分，其包含以Fe2O3换算为53.30摩尔％～53.80摩尔％的Fe、以ZnO换算为6.90摩尔％～9.50摩尔％的Zn以及以MnO换算为其余部分的Mn；和
副成分，其相对于所述换算时的所述主成分的合计100质量份，包含以SiO2换算为0.003质量份～0.020质量份的Si、以CaCO3换算大于0质量份且为0.35质量份以下的Ca、以Co3O4换算为0.30质量份～0.50质量份的Co、以ZrO2换算为0.03质量份～0.10质量份的Zr以及以Ta2O5换算为0质量份～0.05质量份的Ta，
所述铁氧体烧结体的平均晶体粒径为3μm以上且小于8μm，
所述铁氧体烧结体的烧结体密度为4.65g/cm3以上。
2.根据权利要求1所述的MnZn系铁氧体烧结体，其特征在于，
Ta含量以Ta2O5换算为0.01质量份以上。
3.根据权利要求1或2所述的MnZn系铁氧体烧结体，其特征在于，
Fe含量以Fe2O3换算为53.40摩尔％～53.70摩尔％，Zn含量以ZnO换算为7.00摩尔％～9.40摩尔％，Si含量以SiO2换算为0.004质量份～0.015质量份，Co含量以Co3O4换算为0.30质量份～0.45质量份，Zr含量以ZrO2换算为0.05质量份～0.09质量份。
4.根据权利要求1～3中任一项所述的MnZn系铁氧体烧结体，其特征在于，
300kHz的频率及100mT的励磁磁通密度下的20℃时的磁芯损耗Pcv20为300kW/m3以下，100℃时的磁芯损耗Pcv100为320kW/m3以下，
并且500kHz的频率及100mT的励磁磁通密度下的20℃时的磁芯损耗Pcv20为650kW/m3以下，100℃时的磁芯损耗Pcv100为850kW/m3以下。
5.根据权利要求1～4中任一项所述的MnZn系铁氧体烧结体，其特征在于，
以下述式(1)表示的磁芯损耗的变化率Ps为5％以下：
Ps＝[(Pcv100B－Pcv100A)/Pcv100A]×100···(1)
其中，Pcv100A为在200℃保持前的100℃时的磁芯损耗，Pcv100B为在200℃保持96小时后的100℃时的磁芯损耗，均为在300kHz的频率及100mT的最大磁通密度下测定的值，Ps以％计。
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