CN116323491A - MnZn系铁氧体及其制造方法 - Google Patents

MnZn系铁氧体及其制造方法 Download PDF

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Publication number
CN116323491A
CN116323491A CN202180067034.0A CN202180067034A CN116323491A CN 116323491 A CN116323491 A CN 116323491A CN 202180067034 A CN202180067034 A CN 202180067034A CN 116323491 A CN116323491 A CN 116323491A
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mass
mnzn
pcv
main component
ferrite
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三角彰太
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Tokin Corp
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Tokin Corp
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    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
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Abstract

提供了一种MnZn系铁氧体及其制造方法，其能够抑制高频下损耗的减小和高磁场中磁特性的变化两者。所述MnZn系铁氧体包含作为主成分的Fe2O3、ZnO和MnO，其中，在100mol％的主成分中，Fe2O3为53.2至56.0mol％并且ZnO为3.0至12.0mol％，余量为MnO，相对于100质量％的主成分，MnZn系铁氧体包含作为副成分的0.005至0.060质量％的SiO2、0.010至0.060质量％的CaO、0.10至0.40质量％的Co2O3、和0.05至0.30质量％的TiO2，平均晶体粒径为4μm以下，并且烧结密度为4.8g/cm3以上。

Description

MnZn系铁氧体及其制造方法
技术领域
本发明涉及一种MnZn系铁氧体及其制造方法。
背景技术
MnZn系铁氧体甚至在小磁场中具有诸如高磁导率、高磁通密度和易磁化的特性，并且广泛地用于通信设备应用、电源应用等中。已经对MnZn系铁氧体进行了各种研究，以便根据期望的应用来获得性质(例如，专利文献1和2)。
专利文献1公开了一种MnZn系铁氧体烧结体，该MnZn系铁氧体烧结体包括由特定量的Fe2O3、ZnO和MnO组成的主成分和由特定量的SiO2、CaCO3、Co3O4、ZrO2和Ta2O5组成的副成分，该MnZn系铁氧体烧结体具有3μm以上且小于8μm的平均结晶粒径，并且具有4.65g/cm3以上的烧结体密度，作为在300kHz至500kHz的高频率下在宽温度范围内具有低磁芯损耗、并且在高温环境下具有磁芯损耗的经时变化小的MnZn系铁氧体烧结体。
另外，专利文献2公开了低损耗Mn-Zn铁氧体，该Mn-Zn铁氧体包含作为主成分的Fe、Mn和Zn，作为第一副成分的Co、Ca和Si，以及作为第二副成分的特定量的Va族元素，并且具有小于3.2μm的平均结晶粒径和1Ω·m以上的低体积效率，作为即使在1MHz以上的高频下，在较宽的温度范围和较宽的操作磁通密度下也具有低电力损耗的Mn-Zn铁氧体。
现有技术文献
专利文献
专利文献1：国际专利公开号WO2018/181242
专利文献2：国际专利公开号WO2006/054749
发明内容
本发明要解决的课题
需要一种MnZn系铁氧体以在高频下具有进一步降低的损耗。另一方面，本发明人已经发现，取决于用于减少损耗的方法，在施加高磁场时可以改变磁特性。
本发明解决了上述问题，并且提供了一种MnZn系铁氧体及其制造方法，该MnZn系铁氧体可以抑制高频下损耗的减小和高磁场中磁特性的变化两者。
解决课题的手段
根据本发明的MnZn系铁氧体
包含作为主成分的Fe2O3、ZnO和MnO，其中
在100mol％的主成分中，Fe2O3为53.2至56.0mol％并且ZnO为3.0至12.0mol％，余量为MnO，
相对于100质量％的主成分，MnZn系铁氧体包含作为副成分的0.005至0.060质量％的SiO2、0.010至0.060质量％的CaO、0.10至0.40质量％的Co2O3、和0.05至0.30质量％的TiO2，
平均结晶粒径为4μm以下，并且
烧结密度为4.8g/cm3以上。
上述MnZn系铁氧体的一实施方案，该MnZn系铁氧体还包含作为副成分的0.010至0.100％质量的ZrO。
上述MnZn系铁氧体的一实施方案，该MnZn系铁氧体在25℃、2MHz和50mT的条件下的单位体积磁芯损耗(Pcv)为1500mW/cm3以下。
上述MnZn系铁氧体的一实施方案，由以下式(1)表示的在25℃、2MHz和50mT的条件下的单位体积磁芯损耗(Pcv)与施加磁场之前的该单位体积磁芯损耗相比的变化率为100％以下：
式(1)：(Pcv-Pcv0)/Pcv0×100
其中，Pcv0是施加磁场之前的单位体积磁芯损耗。
根据本发明的用于制造MnZn系铁氧体的方法是
一种用于制造本发明的MnZn系铁氧体的方法，该方法包括：
将包含各主成分的原料混合，使得在烧结之后、在100mol％的主成分中，Fe2O3为53.2到56.0mol％、ZnO为3.0到12.0mol％、且余量为MnO的步骤；
添加包含各副成分的原料，使得在烧结之后、MnZn系铁氧体相对于100质量％的主成分包含0.005至0.060质量％的SiO2、0.010至0.060质量％的CaO、0.10至0.40质量％的Co2O3、和0.05至0.30质量％的TiO2的步骤；以及
将获得的混合粉末进行破碎直到混合粉末变成具有1.2以下的D90颗粒直径的破碎粉末的步骤。
上述生产方法的一实施方案还包括对破碎粉末进行成型、并且在1050℃至1150℃的温度下对所得的成型品进行热处理的步骤。
发明效果
根据本发明，提供了一种MnZn系铁氧体及其制造方法，其能够抑制高频下损耗的减小和高磁场中磁特性的变化两者。
具体实施方式
在下文中，将描述根据本发明的MnZn系铁氧体及其制造方法。
除非另有说明，否则由使用“至”表示的数值范围包括其下限值和上限值。
[MnZn系铁氧体]
根据本发明的MnZn系铁氧体(在下文中也称为本MnZn系铁氧体)
包含作为主成分的Fe2O3、ZnO和MnO，其中
在100mol％的主成分中，Fe2O3为53.2至56.0mol％并且ZnO为3.0至12.0mol％，余量为MnO，
相对于100质量％的主成分，MnZn系铁氧体包含作为副成分的0.005至0.060质量％的SiO2、0.010至0.060质量％的CaO、0.10至0.40质量％的Co2O3和0.05至0.30质量％的TiO2，
平均结晶粒径为4μm以下，并且
烧结密度为4.8g/cm3以上。
本发明人已经获得了如下发现：通过调节MnZn系铁氧体使得每个金属氧化物包含在如上所述的上述特定比例中、平均结晶粒径为4μm以下且烧结密度为4.8g/cm3以上，能够减小高频(特别是1MHz至3MHz)下的损耗，并且还能够抑制在施加高磁场之后磁性特性中的变化，并且本发明人已经完成了本发明。
本发明人已经获得了如下发现：通过使用具有镍铁钴合金特性(perminvarproperty)的磁滞回线的MnZn系铁氧体能够减小高频下的损耗。对于具有镍铁钴合金特性的MnZn系铁氧体，通过抑制畴壁的位移(钉住)来减小与畴壁位移相关的剩余损耗。然而，当施加高磁场时，畴壁的钉住变得不足，并且畴壁的活动性增加，从而损耗的减少可能变得不足。另一方面，MnZn系铁氧体包含上述特定比例的各成分，并且使结晶粒径减小到4μm以下，从而减少结晶颗粒中的畴壁的数量并减少与畴壁位移相关的剩余损耗。具体地，本MnZn系铁氧体可以将25℃、2MHz和50mT的条件下的单位体积磁芯损耗(Pcv)抑制至1500mW/cm3以下。此外，本MnZn系铁氧体例如可以将由下式(1)表示的在25℃、2MHz和50mT的条件下的单位体积磁芯损耗(Pcv)与施加磁场之前的该单位体积磁芯损耗相比的变化率设定为100％以下：
式(1)：(Pcv-Pcv0)/Pcv0×100
如上所述，本MnZn系铁氧体具有以下特性：即使当施加高磁场时，也可以与不施加高磁场的状态一样降低高频下的损耗。
本MnZn系铁氧体包含作为主成分的Fe2O3、ZnO和MnO。在本MnZn系铁氧体中，在100mol％的主成分中，Fe2O3为53.2至56.0mol％并且ZnO为3.0至12.0mol％，余量为MnO(33.0至43.8mol％)。
通过将Fe2O3设置为53.2mol％以上、优选为53.5mol％以上，能够获得具有高磁通密度的MnZn系铁氧体。另一方面，通过将Fe2O3设置为56.0mol％以下、优选为55.0mol％以下、更优选为54.8mol％以下，其与其它成分的组合抑制了MnZn系铁氧体形成为镍铁钴合金，以使得当施加高磁场时能够降低损耗。
通过将ZnO设置为3mol％以上、优选6mol％以上，其与其他成分的组合能够抑制MnZn系铁氧体形成为镍铁钴合金，并且烧结性优异，并且易于将结晶密度调节至4.8g/cm3以上。另一方面，通过将ZnO设置为12.0mol％以下、优选11.0mol％以下，能够获得具有高磁通密度的MnZn系铁氧体。
此外，本MnZn系铁氧体至少包含作为副成分的SiO2、CaO、Co2O3和TiO2。
通过将SiO2设置为0.005质量％以上、优选0.010质量％以上，能够充分形成具有高比电阻的晶界相、以抑制高频下的涡流的产生。此外，通过含有SiO2，提高了MnZn系铁氧体的机械强度。另一方面，通过将SiO2设置为0.060质量％以下、优选为0.050质量％以下，能够抑制较大化SiO2的产生、并抑制损耗的劣化。
通过将CaO设置为0.010质量％以上、优选为0.030质量％以上，能够充分形成具有高比电阻的晶界相、以抑制高频下的涡流的产生。另一方面，通过将CaO设置为为0.050质量％以下、优选为0.045质量％以下，能够抑制作为杂质残留的CaO，并抑制损耗的劣化。
通过将Co2O3设置为0.10质量％以上、优选0.20质量％以上，能够抑制高温环境中的损耗。另一方面，通过将Co2O3设置为0.40质量％以下、优选0.30质量％以下，抑制镍铁钴合金的形成、从而在施加高磁场时可以降低损耗。
另一方面，通过将TiO2设置为0.05质量％以上、优选为0.10质量％以上，抑制镍铁钴合金的形成、从而在施加高磁场时可以降低损耗。另一方面，通过将TiO2设置为0.30质量％以下、优选为0.25质量％以下，抑制镍铁钴合金的形成、从而在施加高磁场时可以降低损耗。
本MnZn系铁氧体还可以包含其他成分，只要发挥本发明的效果即可。其他成分的实施例还包括必要时添加的其他金属氧化物，以及不可避免地含有的元素。
其他金属氧化物的实施例包括ZrO2、Ta2O5、Nb2O5、Bi2O3和MoO3，并且在这些中ZrO2是优选的。此外，不可避免地含有的元素的实施例包括C(碳原子)、P(磷原子)和B(硼原子)。
通过将ZrO2设置为0.01质量％以上、优选0.04质量％以上，能够充分形成具有高比电阻的晶界相、以抑制高频下的涡流的产生。另一方面，通过将ZrO2设置为0.1质量％以下、优选0.08质量％以下，能够抑制作为杂质残留的ZrO2，并抑制损耗的劣化。
相对于主成分100质量％，除ZrO2以外的其他金属氧化物和元素的总含量优选为0.1质量％以下，更优选为0.01质量％以下。
本MnZn系铁氧体可以适当地用作例如在具有高频(例如，1至3MHz)开关频率的开关电源电路中使用的电感器的芯材。此外，本MnZn系铁氧体即使在施加高磁场时也能够抑制磁特性的变化，并且因此可以适用于例如可能流过大电流的变压器或扼流线圈。
[用于制造MnZn系铁氧体的方法]
接下来，将描述用于制造MnZn系铁氧体的方法的一个实施方案(下文中也称为本制造方法)。
本制造方法可以是能够适当地制造本MnZn系铁氧体的制造方法，该方法至少包括：将含有各主成分的原料混合，使得在烧结之后、在100mol％的主成分中，Fe2O3为53.2至56.0mol％并且ZnO为3.0至12.0mol％，余量为MnO的步骤(混合步骤)；添加包含各副成分的原料，使得在烧结之后、本MnZn系铁氧体相对于100质量％的主成分包含0.005至0.060质量％的SiO2、0.010至0.060质量％的CaO、0.10至0.40质量％的Co2O3、和0.05至0.30质量％的TiO2的步骤(添加步骤)；以及将所获得的混合粉末进行破碎直到混合粉末变成具有1.2μm以下的D90颗粒直径的破碎粉末的步骤(破碎步骤)。本制造方法还可以包括以下步骤：诸如在混合步骤之后、将粘合剂添加到主成分的混合粉末以获得颗粒料(granule)的干燥/造粒步骤；对所获得的颗粒体进行煅烧的煅烧步骤；破碎粉末的干燥/造粒步骤；对破碎粉末或其颗粒料进行成型的成型步骤；或对所得的成型品进行热处理的热处理步骤(烧结步骤)。
在上述混合步骤中，混合主成分使得烧结后的主成分具有本MnZn系铁氧体的组成。在混合之前的主成分的形式没有特别限制，并且优选为粉末形式，因为粉末易于处理并且可以均匀地混合。将各主成分的原料粉末混合并破碎(如果必要)以获得混合粉末。混合和破碎的方法可以从已知的方法中适当地选择。其具体实施例包括磨碎机和珠磨机。混合粉末的颗粒直径不受特别限制，并且考虑到均匀性等方面，优选将中值直径D50调节为0.5μm至1.5μm。稍后描述的颗粒直径D50和D90是颗粒直径(D50)分别为当测量目标颗粒的粒度分布时，累积颗粒直径频率(cumulative particle diameter frequency)为50％的颗粒直径(D50)和累积颗粒直径频率为90％的颗粒直径(D90)。混合粉末的粒度分布可以通过使用粒度分布测量装置来测量。
干燥/造粒步骤可以应用于上述主成分的混合粉末。在干燥/造粒步骤中，例如，当混合粉末的总质量为100质量份时，可以通过将0.5～1质量份的粘合剂(诸如，聚乙烯醇)添加至混合步骤中得到的混合粉末、并通过使用喷雾干燥器等对所获得的混合物进行喷雾来得到颗粒料。
接下来，所获得的颗粒料可以在空气气氛中、在750℃下煅烧约1小时以获得煅烧品(煅烧步骤)。
接下来，将副成分添加到煅烧品中，使得烧结之后的副成分具有本MnZn系铁氧体的组成。添加之前，副成分的形式没有特别限制，并且优选为颗粒的形式，因为颗粒易于处理并且可以均匀地混合。
在添加副成分之后，将所得的混合粉末破碎以获得破碎粉末。可以适当地调节破碎，使得获得的MnZn系铁氧体的平均结晶粒径为4μm以下。其方法的实施例包括涉及使煅烧品破碎、直到破碎后的颗粒直径D90变成1.2μm以下的方法。
在干燥/造粒步骤中，当破碎粉末的总质量为100质量份时，通过将0.5至1.0质量份的粘合剂(例如聚乙烯醇)添加至破碎步骤中获得的破碎粉末中，并且通过使用喷雾干燥器等对所得混合物进行喷雾来获得颗粒料。此时，颗粒料的中值直径D50理想地为40μm以上且200μm以下。
在成型步骤中，将在干燥/造粒步骤中获得的颗粒料成型为预定形状。可以根据应用等来设计预定形状。例如，颗粒料被成型为具有19mm的外径、13mm的内径和11mm的高度的环型芯。
对成型之后的颗粒料进行热处理以获得烧结体(本MnZn系铁氧体)。热处理(烧结)条件优选为在1050℃至1150℃的温度下加热几个小时。通过在1050℃以上进行热处理，容易实现4.8g/cm3以上的烧结密度。另一方面，通过在1150℃以下进行热处理，容易实现4μm以下的平均结晶粒径变得。
根据以上制造方法，优选地制造了具有4μm以下的平均结晶粒径和4.8g/cm3以上的烧结密度的MnZn系铁氧体。
实施例
在下文中，将参照实施例和比较例具体描述本发明。本发明不受实施例的描述的限制。
[实施例1]
对每种原料粉末进行称重并混合，使得在烧结之后，Fe2O3含量为54.0mol％，ZnO含量为10.0mol％，并且MnO含量为36.0mol％，以使总量为100mol％。相对于混合物总量的100质量份，向上述混合物中加入相当于0.5质量份的聚乙烯醇，并且通过使用喷雾干燥器对所得的混合物进行喷雾、以获得颗粒料。接下来，将颗粒料在空气气氛中、在750℃下煅烧1小时以获得煅烧品。接下来，添加各副成分的原料粉末，使得相对于100质量％的主成分，SiO2为0.03质量％、CaO为0.04质量％、Co2O3为0.2质量％、TiO2为0.2质量％且ZrO2为0.08质量％。
接下来，作为破碎步骤，煅烧品和添加剂的混合物通过破碎机来进行破碎，使得破碎之后的颗粒直径D90为1.2μm以下，以获得破碎粉末。接下来，作为干燥/造粒步骤，当破碎粉末的总质量为100质量份时，将1质量份的聚乙烯醇添加到破碎粉末中，并且通过使用喷雾干燥器对所得混合物进行喷雾、以获得颗粒料。接下来，作为成型步骤和烧结步骤，将颗粒料成型为成具有16mm的外径、10mm的内径和5mm的高度的环型芯，并且在1100℃下烧结以获得烧结体(MnZn系铁氧体)。
[实施例2至16]
以与实施例1相同的方式获得实施例2至实施例16的MnZn系铁氧体，除了在实施例1中，混合并添加原料使得烧结后的主成分和副成分的含量比例如表1所示。
[比较例1]
以与实施例1相同的方式获得比较例1的MnZn系铁氧体，除了在实施例1中，缩短破碎时间并且破碎之后粉末的颗粒直径D90为4.82μm。
[比较例2至12]
以与实施例1相同的方式获得比较例2至比较例12的MnZn系铁氧体，除了在实施例1中，混合并添加原料使得在烧结之后主成分和副成分的含量比例如表1所示。
<评估>
破碎颗粒(Disintegration particle)直径D90是利用湿式粒度分布测定装置测量在上述各实施例及比较例的制造过程中得到的破碎粉末的浆料而确定的。
平均结晶粒径使通过对各实施例和比较例中得到的MnZn系铁氧体进行镜面抛光、通过蚀刻溶解晶界相、随后用显微镜观察而获得的图像进行图像分析来计算的。对于每个，在100个晶粒上执行测量。
通过阿基米德方法测量烧结密度。
此外，通过使用BH分析仪测量MnZn系铁氧体的Pcv和Pcv0，并且通过上式(1)计算Pcv变化率。其结果示于表1中。
[表1]
Figure BDA0004152162560000091
[结果总结]
示出了实施例1至实施例16的MnZn系铁氧体25℃、2MHz、50mT的单位体积磁芯损耗(Pcv)为1500mW/cm3以下，并且Pcv与在施加磁场之前的Pcv的变化率为100％以下，其中在100mol％的主成分中，Fe2O3为53.2至56.0mol％，ZnO为3.0至12.0mol％，余量为MnO；相对于100％质量的主成分，MnZn系铁氧体包含作为副成分的0.005至0.060质量％的SiO2，0.010至0.060质量％的CaO，0.10至0.40质量％的Co2O3，和0.05至0.30质量％的TiO2；平均结晶粒径为4μm以下；并且烧结密度为4.8g/cm3以上。由以上可知，已经清楚的是，本MnZn系铁氧体可以抑制在高频下损耗的减小和在高磁场中磁特性的变化。
本申请要求基于2020年10月2日提交的日本专利申请号2010-167723的优先权，该日本专利的公开内容通过引用整体并入本文。

Claims (6)

1.一种MnZn系铁氧体，所述MnZn系铁氧体包含作为主成分的Fe2O3、ZnO和MnO，其中，
在100mol％的所述主成分中，Fe2O3为53.2至56.0mol％、ZnO为3.0至12.0mol％、且余量为MnO，
相对于100质量％的所述主成分，所述MnZn系铁氧体包含作为副成分的0.005至0.060质量％的SiO2、0.010至0.060质量％的CaO、0.10至0.40质量％的Co2O3、和0.05至0.30质量％的TiO2，
平均结晶粒径为4μm以下，并且
烧结密度为4.8g/cm3以上。
2.根据权利要求1所述的MnZn系铁氧体，其中，所述MnZn系铁氧体还包含作为副成分的0.010至0.100质量％的ZrO。
3.根据权利要求1或2所述的MnZn系铁氧体，其中，在25℃、2MHz和50mT的条件下的单位体积磁芯损耗(Pcv)为1500mW/cm3以下。
4.根据权利要求1至3中任一项所述的MnZn系铁氧体，其中，由下式(1)表示的在25℃、2MHz和50mT的条件下的单位体积磁芯损耗(Pcv)与施加磁场之前的该单位体积磁芯损耗相比的变化率为100％以下。
式(1)：(Pcv-Pcv0)/Pcv0×100
其中，Pcv0是施加磁场之前的单位体积磁芯损耗。
5.一种用于制造根据权利要求1至4中任一项所述的MnZn系铁氧体的方法，所述方法包括：
将包含各所述主成分的原料混合，使得在烧结之后，在100mol％的所述主成分中Fe2O3为53.2至56.0mol％、ZnO为3.0至12.0mol％、且余量为MnO的步骤；
添加包含各所述副成分的原料，使得在烧结之后，所述MnZn系铁氧体相对于100质量％的所述主成分包含0.005至0.060质量％的SiO2、0.010至0.060质量％的CaO、0.10至0.40质量％的Co2O3、和0.05至0.30质量％的TiO2的步骤；以及
将获得的混合粉末进行破碎直到所述混合粉末变成具有1.2以下的D90粒径的破碎粉末的步骤。
6.根据权利要求5所述的用于制造MnZn系铁氧体的方法，其中，所述方法还包括对所述破碎粉末进行成型、并在1050℃至1150℃的温度下对所得的成型品进行热处理的步骤。
CN202180067034.0A 2020-10-02 2021-08-16 MnZn系铁氧体及其制造方法 Pending CN116323491A (zh)

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