CN114907106B - 高机械强度宽温宽频MnZn功率铁氧体的制备方法 - Google Patents

高机械强度宽温宽频MnZn功率铁氧体的制备方法 Download PDF

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CN114907106B
CN114907106B CN202210324651.0A CN202210324651A CN114907106B CN 114907106 B CN114907106 B CN 114907106B CN 202210324651 A CN202210324651 A CN 202210324651A CN 114907106 B CN114907106 B CN 114907106B
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temperature
ferrite
mnzn
bto
sintering
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CN114907106A (zh
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余忠
易耀华
王东明
邬传健
张凯
孙科
刘培元
兰中文
蒋晓娜
余勇
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Ruyuan Dong Yang Guang Materials Co ltd
University of Electronic Science and Technology of China
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Ruyuan Dong Yang Guang Materials Co ltd
University of Electronic Science and Technology of China
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Abstract

高机械强度宽温宽频MnZn功率铁氧体的制备方法，涉及铁氧体材料制备技术领域。本发明包括以下步骤：(1)BaTiO3(BTO)基PTC介电陶瓷粉体粉体制备；(2)MnZn铁氧体预烧料制备；(3)掺杂处理：以步骤2)获得的MnZn功率铁氧体预烧料为重量参照基准，按预烧料重量百分比加入以下添加剂：0.02～0.08wt％CaCO3、0.01～0.05wt％Nb2O5、0.01～0.05wt％ZrO2、0.3～0.5wt％Co2O3、0.01～0.05wt％MoO3和0.001～0.012wt％BTO基PTC介电陶瓷粉体，将以上粉料二次球磨；(4)样品成型；(5)烧结。采用本发明技术制备的材料具有优异的机械强度，提高了电子系统的可靠性。

Description

高机械强度宽温宽频MnZn功率铁氧体的制备方法
技术领域
本发明涉及铁氧体材料制备技术领域。
背景技术
MnZn功率铁氧体作为一种高Bs、低损耗磁性材料，广泛应用于开关电源中的各种变压器、滤波器、扼流圈等磁性元件，其产量占软磁铁氧体材料总产量的一半以上。它是开关电源模块的核心，主要用于功率的转换和传递，已成为上述电子设备实现小型高效和高可靠性的关键支撑性电子功能材料。2020年以来，电子电力步入GaN时代，开关电源模块的开关频率增加，驱动损耗增大，同时第三代半导体器件的适用工作频率在100-500kHz，模块的开关频率也将宽频可调以适应不同的应用场合。例如5G通信网络对基站设施的数据处理与无线通信能力要求高功率密度电源设计，电源设计装配越来越密集，导致散热条件差。新能源汽车用开关电源，不仅需要考虑汽车速度变化导致的负载变化，还要考虑汽车工作时的地域环境和季节温度变化；汽车发动机工作时温度很高，会导致靠近发动机附近的开关电源模块温度急剧升高，应用于其中的MnZn功率铁氧体的损耗也会急剧增大，进而引起开关电源恶性发热甚至烧毁。基于上述情况，这就对电源模块的高温可靠性和力学性能提出了更加苛刻的要求。一方面，需要高性能宽温宽频MnZn功率铁氧体材料以适应特定的应用场合，使电源能耗和发热降到最低；另一方面，需要提高铁氧体的机械性能以适应磁性器件小型化和平面化的需求，提高磁性器件加工过程中的产品合格率，同时提高电源移动/震动过程中的可靠性。因此，研究高机械强度宽温宽频MnZn功率铁氧体材料符合国家保护环境节能减排的发展理念，不仅有利于推动开关电源小型轻量化和高频化发展，保证电源的应用可靠性，而且可以在技术层次上提升国内MnZn铁氧体产业的竞争力。
中国专利公开号为CN 101921105 A，公开的《一种高弯曲强度铁氧体的制备方法》，其主料其包括Fe2O3 55.5～58.5mol％、ZnO 4.5～9.5mol％，其余为MnO；辅料包括0.5～1.5mol％LiO和600～2000ppm的CoO。中国专利公开号为CN 107162580 A，公开的《高机械强度MnZn铁氧体材料》，其主料其包括Fe2O3 50～56mol％、 ZnO 0～16mol％，其余为MnO；添加剂包括500ppm以下的SiO2,1000ppm以下的 CaO,1000ppm以下的V2O5。所制备的铁氧体抗弯强度高且具有高的饱和磁通密度。但其制备的铁氧体未明确25-140℃宽温范围内以及100-300kHz宽频范围的损耗Pcv和始磁导率μi。中国专利公开号为CN 113314289 A，公开的《一种宽温宽频应用锰锌低功率铁氧体材料及制备方法》，其主成分包括Fe2O3 50～60mol％、 ZnO 5～12mol％，其余为MnO；添加剂包括0.01～0.1wt％CaCO3、0.03～0.15wt％V2O5、 0～0.05wt％Nb2O5、0～0.04wt％SiO2、0.02～0.12wt％SnO2、0.02～0.6wt％Co2O3、0.04～0.3wt％TiO2、0～0.1wt％NiO、0～0.05wt％MoO3。其制备的锰锌低功率铁氧体材料在高饱和磁感应强度和宽温、宽频的应用环境下，具有良好的低功率损耗性能，但未说明MoO3对材料机械性能的影响。
中国专利公开号为CN 112979301 A，公开的《高频高温低损耗MnZn功率铁氧体材料及其制备方法》，其主成分包括Fe2O353.5～56.5mol％、MnO32.5～35.5mol％、 ZnO9.0～12.0mol％；添加剂包括0.06～0.12wt％CaCO3、0.01～0.04wt％V2O5、 0.10～0.40wt％TiO2、0.02～0.08wt％SnO2、0.20～0.55wt％Co2O3、0.01～0.06wt％BaTiO3(BTO)、0.1～0.3wt％CaCu3Ti4O12(CCTO)。其利用BTO和CCTO的高电阻特性进行联合掺杂制备的MnZn功率铁氧体应用频率为MHz级。再如中国专利公开号为CN 108530050A，公开的《宽温低损耗高阻抗MnZn软磁铁氧体材料及制备方法》，其主料包括Fe2O3 52.0～55.0mol％、ZnO 9.5～12.5mol％，其余为MnO，辅料为 0.03～0.05wt％CaO；添加剂包括0.001～0.05wt％纳米BaTiO3、0.001～0.05wt％Bi2O3、 0.001～0.035wt％CaO、0.001～0.02wt％Nb2O5、0.003～0.2wt％HfO2、0.08～0.3wt％Co2O3。其仍然仅是利用BTO高电阻率的特性，通过纳米BTO粉体增加与颗粒料的接触，增大MnZn铁氧体晶界电阻率，且制备的材料只有100kHz 200mT的性能，限制了其应用。
中国科学技术大学公开了一种常温居里点陶瓷PTC的方法(宋嘉梁.常温PTC 热控材料及其热控方法研究[D].2016.)，其配方为下式 0.7molBaCO3+0.3molSrCO3+1.01molTiO2+0.001～0.004molY2O3+0.005molAl2O3+0.02 4molSiO2。其制备工艺是：将BaCO3、SrCO3、TiO2和Y2O3按设定的摩尔百分比称量，一磨后在1150℃预烧，获得BaTiO3主晶相；二磨配料按设定的摩尔比将Al2O3、 SiO2加入预烧料中，造粒成型后在1350℃空气烧结，获得居里温度点大于45℃的BaTiO3基陶瓷PTC材料。南京理工大学公开了一种低居里点陶瓷PTC的配方 (张宏亮.正温度系数热敏材料的制备与研究[D].2019.)，配方如下式所示：65mol％BaCO3+35mol％SrCO3+100mol％TiO2+xmol％Nb2O5+ymol％Ce2O3+1mol％ TiO2+0.5mol％Al2O3+2.4mol％SiO2，其中x＝0.2，y＝0.2～0.3。制备了居里温度点在 50～90℃的BaTiO3基PTC陶瓷材料。华中科技大学也公开了一种低温烧结PTC陶瓷的方法(孔明日,姜胜林,涂文芳.BaO-B2O3-SiO2玻璃助剂中SiO2对低温烧结PTCR 陶瓷性能的影响[J].材料导报,2009,23(12):68-70+74.)，其配方如下式所示： (Ba0.75Sr0.25)Ti1.02O3+0.6％(摩尔分数)Y2O3其制备工艺是：主配方将BaCO3、 SrCO3、TiO2和Y2O3按设定的摩尔百分比称量，一磨后在1150℃预烧；二磨配料将3％玻璃助剂BaB2O4加入预烧料中，二磨料烘干造粒成型，在970～1250℃空气烧结，获得居里温度点约为97℃的BaTiO3基陶瓷PTC材料。
现有关于钛酸钡系PTC陶瓷的专利，如中国专利公开号CN 112694325 A公开的《一种PTC热敏电阻陶瓷材料及其制备方法、应用》，以及专利公开号CN 113651612A公开的《钛酸钡系PTC热敏陶瓷材料及其在锂电池中的应用》，其材料配方均由钛酸钡基陶瓷粉料和添加剂构成，主要应用于PTC热敏电阻元件，利用其电阻率随温度上升而急剧增大的PTC效应，有效阻断电子线路发生的热失控，起限流、热保护的作用，提高电子设备的安全可靠性。
综上所述，现有的专利中，BaTiO3(BTO)作为添加剂加入MnZn功率铁氧体中，仅利用了普通BTO的高电阻率特性提高铁氧体的晶界电阻，从而降低高频损耗。通过在BaTiO3主晶相中引入适量的SrCO3和Y2O3等辅料以降低材料的居里温度点可以使BTO具有PTC(电阻率正温度系数)效应，电阻率会随温度升高而急剧增大，因此掺加此类BTO基介电陶瓷后将有利于改善铁氧体高温损耗特性。然而BTO具有明显的抑制晶粒生长作用，带来晶粒尺寸减小且不均匀的问题，导致材料的起始磁导率大幅度降低，低温低频损耗增大。而低熔点的MoO3正好具有促进晶粒生长的作用，可以与BTO联合，改善铁氧体材料的晶粒/晶界特性，调控铁氧体的宽温磁特性，进而改善MnZn功率铁氧体的力学性能。因此本发明提供一种高机械强度宽温宽频MnZn功率铁氧体的制备方法。
发明内容
本发明所要解决的技术问题是，提供一种高机械强度宽温宽频MnZn功率铁氧体的制备方法,突破MnZn铁氧体起始磁导率与高温高频损耗相互制约的关键技术瓶颈，同时改善MnZn功率铁氧体宽温宽频特性及力学性能。
本发明解决所述技术问题采用的技术方案是，高机械强度宽温宽频MnZn功率铁氧体的制备方法，其特征在于，包括以下步骤：
(1)BaTiO3(BTO)基PTC介电陶瓷粉体粉体制备：
通过高温固相法，以BaCO3、SrCO3和TiO2作为原料，按照主成分 xmol％BaCO3：ymol％SrCO3：zmol％TiO2的比例称取原料，其中x＝30～40，y＝10～20，z＝45～55；
一次球磨后在1000～1200℃预烧，得到BaTiO3主晶相；
将0.1～0.3mol％Y2O3、0.1～0.3mol％Al2O3和1～5mol％SiO2加入到预烧料中，球磨，造粒成型后在1300～1400℃空气烧结，碾磨获得粒径为0.5～1μm的BTO 基PTC介电陶瓷粉体；
(2)MnZn铁氧体预烧料制备：
以Fe2O3、ZnO和MnO作为原料，按照主成分51.5～54.0mol％Fe2O3和 10.0～12.0mol％ZnO，其余为MnO的比例称取原料；一次球磨，烘干、过筛后，在860～920℃的温度下预烧，获得MnZn功率铁氧体预烧料；
(3)掺杂处理：
以步骤2)获得的MnZn功率铁氧体预烧料为重量参照基准，按预烧料重量百分比加入以下添加剂：0.02～0.08wt％CaCO3、0.01～0.05wt％Nb2O5、0.01～0.05 wt％ZrO2、0.3～0.5wt％Co2O3、0.01～0.05wt％MoO3和0.001～0.012wt％BTO基 PTC介电陶瓷粉体，将以上粉料二次球磨；
(4)样品成型：
将步骤(3)所得的球磨料烘干后，造粒成型；
(5)烧结。
进一步的，所述步骤(5)中，分下述阶段烧结：
(5.1)排胶阶段：从50℃升温到800～950℃，氧分压为21％；
(5.2)致密阶段：继续升温到950～1250℃，氧分压为0.05～1％；
(5.3)保温阶段：首先在烧结温度1250～1320℃保温6～10h，氧分压控制为2～5％；然后在烧结温度基础上增加20～100℃，保温1～3h，氧分压控制为1～4％；
(5.4)降温阶段：控制温度速率为-0～3℃/min，降温氧分压＜1％。
所述步骤(1)中，x＝35，y＝15，z＝50。加入至预烧料中的Y2O3、Al2O3、 SiO2的加入量分别为：
0.25mol％Y2O3、0.25mol％Al2O3、1.2mol％SiO2。
所述步骤(2)中，按照主成分52.5mol％Fe2O3和11.5mol％ZnO，其余为MnO的比例称取原料，预烧时间1～3h。
所述步骤(3)中，按照下述比例加入添加剂：
0.03wt％CaCO3、0.02wt％Nb2O5、0.01wt％ZrO2、0.35wt％Co2O3、0.02～0.03 wt％MoO3和0.003～0.005wt％BTO基PTC介电陶瓷粉体。
“以BaTiO3主晶相预烧料为摩尔比的基准”是指以BaTiO3(简写为BTO) 主晶相预烧料为摩尔比计算的分母，例如BTO主晶相预烧料100mol，加入 Y2O30.1～0.3mol，SiO2 1～5mol，则以BTO主晶相预烧料为摩尔比的基准，Y2O3的比例为0.1～0.3mol％，SiO2为1～5mol％。
“以MnZn功率铁氧体的重量为参照基准”是指以主成分的重量作为分母，添加剂为分子计算，例如，主成分的重量为100g，BTO基PTC介电陶瓷粉体的重量为0.004g，以主成分的重量为计算基准，BTO的比例为0.004wt％。
本发明以“～”表示的范围包括范围的两端的数值，例如“SiO2为1～5mol％”所限定的范围包括1mol％和5mol％。
与现有技术相比，本发明具有如下有益效果：
(1)本发明提供的MnZn功率铁氧体材料，磁导率μi＝2900±15％(25～140℃， f＝10kHz)，Pcv＜320mW/cm3(25℃，f＝100kHz，B＝200mT),Pcv＜200mW/cm3(25℃， f＝300kHz，B＝100mT)。能够满足宽频开关电源的高磁导率和低损耗的要求。
(2)通过调控MoO3助熔和BTO阻晶的交互作用，控制材料的显微结构，具有优异的机械强度，提高了电子系统的可靠性。
附图说明
图1为普通BTO基陶瓷(左)的电阻率温度特性图。
图2为本发明所采用的BTO基介电陶瓷(右)的电阻率温度特性图。
图3为100kHz-200mT下对比例1和实施例1-1与实施例1-2的损耗温度特性图。
图4为200kHz-125mT下对比例1和实施例1-1与实施例1-2的损耗温度特性图。
图5为300kHz-100mT下对比例1和实施例1-1与实施例1-2的损耗温度特性图。
图6为100kHz-200mT下对比例2和实施例2-1与实施例2-2的损耗温度特性图。
图7为200kHz-125mT下对比例2和实施例2-1与实施例2-2的损耗温度特性图。
图8为300kHz-100mT下对比例2和实施例2-1与实施例2-2的损耗温度特性图。
图9为实施例1-1、实施例1-2和对比例1的涡流损耗Pe温度特性图。
图10为实施例2-1、实施例2-2和对比例2的涡流损耗Pe温度特性图。
图11为实施例1-1、实施例1-2和对比例1的磁滞损耗Ph温度特性图。
图12为实施例2-1、实施例2-2和对比例2的磁滞损耗Ph温度特性图。
图13为实施例1-1、实施例1-2和对比例1的起始磁导率和抗弯强度对比曲线图。
图14为实施例2-1、实施例2-2和对比例2的起始磁导率和抗弯强度对比曲线图。
图15为实施例和对比例的SEM显微结构图。
具体实施方式
本发明提供一种高机械强度宽温宽频MnZn功率铁氧体的制备方法，包括以下制备步骤：
(1)BaTiO3基PTC介电陶瓷粉体制备
通过高温固相法，以BaCO3、SrCO3和TiO2作为原料，按照主成分35mol％BaCO3：15mol％SrCO3：50mol％TiO2的比例称取原料；一磨后在1150℃保温0.5h完成预烧，得到BaTiO3主晶相；二磨配料将0.25mol％Y2O3、0.25mol％Al2O3、 1.2mol％SiO2加入到预烧料中，造粒成型后在1350℃空气烧结2h，得到具有 PTC效应的BaTiO3基介电陶瓷。最后将其碾磨获得粒径为0.5～1μm的BaTiO3基PTC介电陶瓷粉体。
(2)MnZn铁氧体预烧料制备
以Fe2O3、ZnO和MnO作为原料，按照主成分52.5mol％Fe2O3和11.5mol％ZnO，其余为MnO的比例称取原料；
将以上粉料在行星式球磨机中进行一次球磨2h(h为小时)；
所得的球磨料烘干、过筛后，在900℃的温度下预烧2h，获得MnZn功率铁氧体预烧料。
(3)掺杂处理
以步骤2)获得的MnZn功率铁氧体预烧料为参照基准，进行实施例，添加剂含量如表1和表2所示：
表1
Figure SMS_1
表2
Figure SMS_2
将预烧料和各组添加剂在行星式球磨机中进行二次球磨3h；
(4)样品成型
将二次球磨所得的球磨料烘干后，按重量百分比加入12wt％的PVA有机粘合剂进行造粒；
根据所需要的样品形状，将获得的造粒料压制成所需的样品生坯，成型压力为6MPa。
(5)样品烧结
将成型后的生坯件置于气氛烧结装置中进行分阶段烧结处理。
第一阶段：排胶阶段。从50℃升温到900℃，氧分压为21％；
第二阶段：致密阶段。继续升温到1250℃，氧分压为0.05％；
第三阶段：保温阶段。首先在烧结温度1250℃保温6h，氧分压控制为3％；
然后在1285℃保温1h，氧分压控制为2.5％；
第四阶段：降温阶段。控制温度速率为-2℃/min，降温氧分压0.05％。
(6)测试
将制备得到的MnZn功率铁氧体样品采用同惠TH2826精密LCR测试仪测试样品的电感L，换算成起始磁导率；样品基本磁性能采用岩崎SY8232 B-H分析仪进行测试；抗弯强度采用MODEL SH-2K机械强度自动试验测试机进行测试。
实验与数据
实施例和对比例样品的基本性能：
表3对比例1与实施例1-1、实施例1-1的性能对比
Figure SMS_3
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Figure SMS_4
表4对比例2与实施例2-1、实施例2-2的性能对比
Figure SMS_5
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Figure SMS_6
图1和图2可见具有PTC效应的BTO介电陶瓷的居里温度约为80℃，超过居里温度后其电阻率以数量级的形式急剧增大，而普通BTO陶瓷的电阻率随温度升高保持同一数量级，超过80℃后逐渐下降。
图3～图5可见实施例较对比例MnZn功率铁氧体损耗略有增大，但是MoO3的助熔作用可以增大起始磁导率降低磁滞损耗。
图6～图8可见实施例较对比例MnZn功率铁氧体损耗明显降低，BTO的高电阻特性可以降低涡流损耗，但是起始磁导率略有下降。
图9～图12可见实施例1-1和实施例1-2较对比例1磁滞损耗减小，实施例 2-1和实施例2-2较对比例2涡流损耗降低。
图13～图14可见实施例1-1和实施例1-2较对比例1起始磁导率和抗弯强度均得到提高，而实施例2-1和实施例2-2较对比例2起始磁导率和抗弯强度性能下降。
图15可见实施例1-1和实施例1-2较对比例1更加致密均匀，MoO3的助熔作用可以改善晶体显微结构，增加样品密度，减少气孔率，机械强度得到改善。

Claims (5)

1.高机械强度宽温宽频MnZn功率铁氧体的制备方法，其特征在于，包括以下步骤：
（1）BTO基PTC介电陶瓷粉体制备：
通过高温固相法，以BaCO3、SrCO3和TiO2作为原料，按照主成分xmol%BaCO3：ymol%SrCO3：zmol% TiO2的比例称取原料，其中x=30~40，y=10~20，z=45~55；
一次球磨后在1000~1200℃预烧，得到BaTiO3主晶相；
将0.1~0.3mol%Y2O3、0.1~0.3mol%Al2O3和1~5mol%SiO2加入到预烧料中，球磨，造粒成型后在1300~1400℃空气烧结，碾磨获得粒径为0.5 ~1 μm的BTO基PTC介电陶瓷粉体；
（2）MnZn铁氧体预烧料制备：
以Fe2O3、ZnO和MnO作为原料，按照主成分51.5~54.0mol% Fe2O3和10.0~12.0mol%ZnO，其余为MnO的比例称取原料；一次球磨，烘干、过筛后，在860~920℃的温度下预烧，获得MnZn功率铁氧体预烧料；
（3）掺杂处理：
以步骤（2）获得的MnZn功率铁氧体预烧料为重量参照基准，按预烧料重量百分比加入以下添加剂：0.02~0.08 wt%CaCO3、0.01~0.05wt%Nb2O5、0.01~0.05 wt%ZrO2、0.3~0.5 wt%Co2O3、0.01~0.05 wt%MoO3和0.001~0.012wt%BTO基PTC介电陶瓷粉体，将以上粉料二次球磨；
（4）样品成型：
将步骤（3）所得的球磨料烘干后，造粒成型；
（5）分下述阶段烧结：
（5.1）排胶阶段：从50℃升温到800~950℃，氧分压为21%；
（5.2）致密阶段：继续升温到950~1250℃，氧分压为0.05~1%；
（5.3）保温阶段：首先在烧结温度1250~1320℃保温6~10h，氧分压控制为2~5%；然后在烧结温度基础上增加20~100℃，保温1~3h，氧分压控制为1~4%；
（5.4）降温阶段：控制温度速率为-0~3℃/min，降温氧分压＜1%。
2.如权利要求1所述的高机械强度宽温宽频MnZn功率铁氧体的制备方法，其特征在于，所述步骤（1）中，x=35，y= 15，z=50。
3.如权利要求2所述的高机械强度宽温宽频MnZn功率铁氧体的制备方法，其特征在于，加入至预烧料中的Y2O3、Al2O3、SiO2的加入量分别为：
0.25mol%Y2O3、0.25mol%Al2O3、1.2mol%SiO2。
4.如权利要求3所述的高机械强度宽温宽频MnZn功率铁氧体的制备方法，其特征在于，所述步骤（2）中，按照主成分52.5mol% Fe2O3和11.5mol%ZnO，其余为MnO的比例称取原料，预烧时间1~3h。
5.如权利要求4所述的高机械强度宽温宽频MnZn功率铁氧体的制备方法，其特征在于，所述步骤（3）中，按照下述比例加入添加剂：
0.03wt%CaCO3、0.02wt%Nb2O5、0.01 wt%ZrO2、0.35 wt%Co2O3、0.02~0.03wt%MoO3和0.003~0.005wt% BTO基PTC介电陶瓷粉体。
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