CN114716240A - 高力学性能低损耗MnZn功率铁氧体材料制备方法 - Google Patents

高力学性能低损耗MnZn功率铁氧体材料制备方法 Download PDF

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CN114716240A
CN114716240A CN202210326156.3A CN202210326156A CN114716240A CN 114716240 A CN114716240 A CN 114716240A CN 202210326156 A CN202210326156 A CN 202210326156A CN 114716240 A CN114716240 A CN 114716240A
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mnzn
ferrite
bto
power ferrite
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CN114716240B (zh
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余忠
谢辉杰
王宏
邬传健
窦海之
孙科
杨仕机
兰中文
蒋晓娜
余勇
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Sunshine Electronic Technology Co ltd
University of Electronic Science and Technology of China
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Abstract

高力学性能低损耗MnZn功率铁氧体材料制备方法，涉及铁氧体材料制备技术领域。本发明包括以下步骤：(1)BTO基PTC介电陶瓷粉体制备；(2)MnZn铁氧体预烧料制备；(3)掺杂处理：以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：0.01～0.03wt％V2O5、0.05～0.15wt％TiO2、0.01～0.03wt％Bi2O3、0.1～0.3wt％Co2O3、0.01～0.03wt％NiO和0.02～0.08wt％BTO基PTC介电陶瓷粉体，二次球磨；(4)样品成型；(5)烧结。采用本发明技术制备得到的铁氧体材料在高频、高温下具有低损耗的性能。

Description

高力学性能低损耗MnZn功率铁氧体材料制备方法
技术领域
本发明涉及铁氧体材料制备技术领域。
背景技术
伴随5G、大数据、云计算、“互联网+”、新能源汽车等新一代信息技术、高端装备战略重点产业蓬勃发展，电源行业迎来了新的增长契机。在开关电源中，磁性材料元件的重量与体积很大，几乎占据整个开关电源电路重量与体积的30％。缩小磁性材料元件的体积与重量，相当于缩小开关电源的体积与重量，从而实现开关电源的高频化、小型化与轻量化。由变压器的工作原理可知，输出电压V＝KfBmAeN，其中K是波形因子，f是开关电源的工作频率，Bm是磁感应强度，Ae是磁芯的有效面积，N是线圈匝数。由该公式可知，在相同的输出电压下，提高工作频率，可以减小开关电源的体积。然而，对于铁氧体磁芯而言，提高工作频率往往会导致磁芯损耗增加。高的磁芯损耗会降低开关电源的效率，严重的情况会导致电子元器件发热甚至烧毁。因此，如何降低MnZn功率铁氧体高温高频下的损耗成为了亟待解决的问题。此外，为防止在绕制线圈或者电源移动/震动过程中，磁芯受外力作用破损开裂，导致电源系统失效，还要求铁氧体磁芯具有高的力学性能。
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，获得居里温度高于30℃的 BTO基陶瓷PTC材料。
华中科技大学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BTO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效应起到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。
有中国专利公告号为CN102696107A，《一种高温低损耗MnZn功率铁氧体及其制备方法》具体涉及一种高温低损耗MnZn功率铁氧体，由主成分和辅助成分组成，其中，主成分及含量以氧化物计算为：Fe2O3为53～53.5mol％、ZnO为8～ 9mol％、MnO余量；按主成分原料总重量计的辅助成分以氧化物计算为：CaCO3、 ZrO2、Nb2O5和Co2O3。其提供上述的一种高温低损耗MnZn功率铁氧体的制备方法。其材料应用的温度范围较高，可以工作在90℃～120℃之间，可广泛应用于开关电源变压器、LCD照明等电子元器件领域，适合长期在100℃或更高温度下工作。但其测试与工作条件仅仅是100kHz 200mT，无法满足开关电源高频化、高效化的需求。
中国专利公开号为CN108530050A，公开的《宽温低损耗高阻抗MnZn软磁铁氧体材料及制备方法》，其主成分包括Fe2O352.0～55.0mol％、ZnO9.5～12.5mol％，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。该专利利用的普通BTO具有较高的电阻率，且通过纳米级普通BTO提高其与颗粒料的接触，以此来提高铁氧体材料的电阻率，降低涡流损耗，并未考虑到高温涡流损耗的控制，同时制备的材料仍只测试100kHz 200mT的性能，依旧无法满足开关电源高频化、高效化的要求。
中国专利公开号为CN112979301A，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、 0.1～0.3wt％CaCu3Ti4O12。其主要利用了BTO和CCTO的高电阻特性进行联合掺杂制备3MHz下具有低损耗的MnZn功率铁氧体，但没有利用BTO的PTC效应对 MnZn功率铁氧体高温高频特性进行改善研究。
中国专利公开号为CN101921105A，公开的《一种高弯曲强度铁氧体的制备方法》，其主成分包括Fe2O355.5～58.5mol％、ZnO4.5～9.5mol％，其余为MnO；添加剂包括0.5～1.5mol％LiO、600-2000ppm的CoO。所制备的铁氧体抗弯强度高且具有高的饱和磁通密度。但制备的铁氧体未测试其在高温高频下的损耗。
综上所述，目前对于BTO基PTC介电陶瓷研究主要对其本身性质(居里温度等)及作为热敏电阻时的应用，很少有将其电阻率随温度上升而迅速上升的特点与MnZn铁氧体NTC效应相联系，从而改善MnZn铁氧体损耗温度特性的应用。对目前的MnZn功率铁氧体材料，在高频高温下难以保持低损耗，仍难以满足开关电源高频化、小型化、轻量化发展的需求。专利中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，没有利用BTO基PTC介电陶瓷对MnZn功率铁氧体高温高频特性进行改善研究。且很少有针对具有BTO基 PTC介电陶瓷掺杂会阻碍晶粒生长，晶粒尺寸减小且不均匀的问题研究进一步降低MnZn功率铁氧体高频高温下损耗的方法。目前对于适用于高频高温下的 MnZn功率铁氧体材料少有关于提高其力学性能的方法。因此本发明提供一种改善MnZn功率铁氧体高温高频损耗及力学性能的方法。
发明内容
本发明所要解决的技术问题是，针对MnZn功率铁氧体在高频高温下难以保持低损耗的问题，提供一种改善MnZn功率铁氧体高温高频损耗及力学性能的制备方法。
本发明解决所述技术问题采用的技术方案是，高力学性能低损耗MnZn功率铁氧体材料制备方法，包括以下步骤：
(1)BTO基PTC介电陶瓷粉体制备：
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，预烧后加入0.2～0.4mol％Al2O3、 1～2mol％SiO2、0.2～0.4mol％Y2O3后进行二次球磨，造粒成型后在1300～1400℃保温1～3h条件下完成空气烧结，碾碎磨粉为粒径0.5～1μm的陶瓷粉体；
(2)MnZn铁氧体预烧料制备
以Fe2O3、ZnO和MnO作为原料，按照主成分54.6～55.6mol％Fe2O3和 8～10mol％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1～3h，获得MnZn功率铁氧体预烧料；
(3)掺杂处理
以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：0.01～0.03wt％V2O5、0.05～0.15wt％TiO2、0.01～0.03wt％Bi2O3、 0.1～0.3wt％Co2O3、0.01～0.03wt％NiO和0.02～0.08wt％BTO基PTC介电陶瓷粉体，二次球磨；
(4)样品成型
将二次球磨后得到的球磨料烘干，然后按重量百分比加入8～15wt％的PVA 有机粘合剂进行造粒，成型；
(5)烧结
将成型的生坯件进行高温烧结。
进一步的，所述步骤1)中，预烧温度为1100～1200℃，保温时间0.5～2h。
所述步骤(5)的烧结温度为1120～1200℃，保温时间6～10h，烧结氧分压控制为2～5％。
所述步骤(1)中，x＝35，y＝15，z＝50，预烧后加入0.25mol％Al2O3、1.2mol％SiO2、0.25mol％Y2O3；
所述步骤(3)中，各添加剂的加入量为：
0.03wt％V2O5、0.06wt％TiO2、0.015wt％Bi2O3、0.3wt％Co2O3、0.03wt％NiO和0.03wt％～0.06wt％BTO基PTC介电陶瓷粉体。
本发明用“～”表示的数值范围包括范围的端值。
采用本发明技术制备得到的铁氧体材料在高频、高温下具有低损耗的性能： 3MHz10mT、120℃下，损耗可低至214kW/m3。本发明能够有效降低开关损耗，满足开关电源高频化、小型化、高效化的发展要求。
附图说明
图1为为普通BTO基介电陶瓷(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为对比例和实施例1、实施例2、实施例3的MnZn功率铁氧体材料SEM 显微结构图。
图4为加入Bi2O3后样品晶粒尺寸变化图。
图5为对比例和实施例1、实施例2、实施例3制备所得MnZn功率铁氧体样品高频总损耗PL(3MHz 10mT)的温度特性曲线图。
图6为对比例和实施例1、实施例2、实施例3制备所得MnZn功率铁氧体样品高频涡流损耗Pe(3MHz 10mT)的温度特性曲线图。
图7为对比例和实施例1、实施例2、实施例3制备所得MnZn功率铁氧体样品高频涡流损耗占比(3MHz 10mT)的温度曲线图。
图8为对比例和实施例1、实施例2、实施例3制备所得MnZn功率铁氧体样品高频剩余损耗Pr(3MHz 10mT)的温度特性曲线图。
图9为对比例和实施例1、实施例2、实施例3制备所得MnZn功率铁氧体样品高频剩余损耗占比(3MHz 10mT)的温度曲线图。
图10为对比例和实施例1、实施例2、实施例3制备所得MnZn功率铁氧体样品抗弯强度图。
具体实施方式
本发明中，按预烧料重量百分比加入添加剂是指以预烧料的重量作为分母，添加剂为分子计算，例如，预烧料的重量为100g，TiO2的重量为0.06g，以预烧料的重量为计算基准，TiO2的比例为0.06wt％。
本发明的核心思想是：3MHz下铁氧体损耗主要来源于涡流损耗(Pe)和剩余损耗(Pr)。MnZn铁氧体涡流损耗与电阻率关系密切，而MnZn铁氧体电阻率具有负温度系数(Negitive Temperature Coefficient，NTC)特性，其电阻率随着温度上升而迅速下降，进而导致涡流损耗在高温时显著增大。因此本发明采用BTO 基PTC介电陶瓷进行掺杂，利用BTO基PTC介电陶瓷在高温时电阻率急剧增大来改善铁氧体的电阻率温度特性。在MnZn铁氧体中采用BTO基PTC介电陶瓷进行掺杂有以下优点。一是BTO基PTC介电陶瓷是钙钛矿结构，不能进入尖晶石结构的MnZn铁氧体晶格中，只能聚集在晶界处，且其具有高熔点，能阻碍晶粒生长，起到细化晶粒的作用；二是具有PTC效应的BTO介电陶瓷电阻率高达 104Ω·m，当其富集在晶界处时能提高电阻率；三是完美利用BTO基PTC介电陶瓷的PTC效应，当温度超过其居里温度时，BTO基PTC介电陶瓷的介电常数ε变小，势垒高度变高，电阻率ρ急剧增大，其电阻随着温度的上升而增大，能减缓 MnZn铁氧体电阻率随温度增高而下降的速率。而剩余损耗与显微结构关系密切，采用BTO基PTC介电陶瓷进行掺杂会阻碍晶粒生长，晶粒尺寸减小且不均匀。因此，在此基础上，本发明采用Bi2O3共同掺杂，调控材料的显微结构，控制晶粒尺寸与均匀性，降低材料剩余损耗，同时改善力学性能。
本发明采用的原料包括主成分和添加剂，所述主成分包括 54.6～55.6mol％Fe2O3和8～10mol％ZnO，其余为MnO；所述添加剂以主成分的重量为计算基准，包括：0.01～0.03wt％V2O5、0.05～0.15wt％TiO2、0.1～0.3wt％Co2O3、 0.01～0.03wt％NiO、0.02～0.08wt％BTO基PTC介电陶瓷粉体。
本发明的制备方法包括以下步骤：
(1)BTO基PTC介电陶瓷粉体制备
采用传统陶瓷制备工艺制备具有PTC效应的BTO基介电陶瓷。 xmol％BaCO3：ymol％SrCO3：zmol％TiO2的比例称取原料，其中x＝30～40， y＝10～20，z＝45～55。一磨后在1100～1200℃保温0.5～2h条件下完成预烧。在预烧料中加入0.2～0.4mol％Al2O3、1～2mol％SiO2、0.2～0.4mol％Y2O3后进行二磨。经造粒成型后在1300～1400℃保温1～3h条件下完成空气烧结，得到BTO基PTC介电陶瓷。将得到的样品放入刚玉研钵中碾碎，磨成粉末，获得粒径为0.5～1μm的陶瓷粉体。
(2)MnZn铁氧体预烧料制备
a)以Fe2O3、ZnO和MnO作为原料，按照主成分54.6～55.6mol％Fe2O3和 8～10mol％ZnO，其余为MnO的比例称取原料；
b)将以上粉料在行星式球磨机中进行一次球磨1～3h；
c)所得的球磨料烘干、过筛后，在860～920℃的温度下预烧1～3h，获得 MnZn功率铁氧体预烧料。
(3)掺杂处理
a)以步骤2)获得的MnZn功率铁氧体预烧料为参照基准，同时准备好步骤1)所制备得到的BTO基PTC介电陶瓷粉体，按预烧料重量百分比加入以下添加剂：0.01～0.03wt％V2O5、0.05～0.15wt％TiO2、 0.01～0.03wt％Bi2O3、0.1～0.3wt％Co2O3、0.01～0.03wt％NiO、 0.02～0.08wt％BTO基PTC介电陶瓷粉体；
b)将以上粉料在行星式球磨机中进行二次球磨3～5h；
(4)样品成型
a)将二次球磨后得到的球磨料烘干，然后按重量百分比加入8～15wt％的 PVA有机粘合剂进行造粒；
b)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5～10MPa。
(5)样品烧结
a)将成型的生坯件置于气氛烧结装置中进行高温烧结。烧结温度为 1120～1200℃，保温时间6～10h；烧结氧分压控制为2～5％。
实施例
实施例包括以下制备步骤：
(1)BTO介电陶瓷粉体制备
采用传统陶瓷制备工艺制备具有PTC效应的BTO基介电陶瓷。按主成分 35mol％BaCO3：15mol％SrCO3:50mol％TiO2进行称取原料。一磨后在1150℃保温 1h条件下完成预烧。在预烧料中加入0.25mol％Al2O3、1.2mol％SiO2、0.25mol％Y2O3后进行二磨。经造粒成型后在1350℃保温2h条件下完成空气烧结，得到BTO基 PTC介电陶瓷。将得到的样品放入刚玉研钵中碾碎，磨成粉末，获得粒径为 0.5～1μm的陶瓷粉体。
(2)MnZn铁氧体预烧料制备
以Fe2O3、ZnO和MnO作为原料，按照主成分55.3mol％Fe2O3和9.8mol％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；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，添加剂含量如下表所示：
Figure BDA0003573520280000081
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
将二次球磨后得到的球磨料烘干，然后按重量百分比加入12wt％的PVA有机粘合剂进行手工造粒；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
将成型的生坯件置于气氛烧结装置中进行高温烧结。烧结温度为1180℃，保温时间6h；烧结氧分压控制为4％。
(6)测试
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。采用阿基米德排水法测密度，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1-3和对比例的样品基本性能见下表：
Figure BDA0003573520280000091
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4可见实施例1较对比例晶粒更小，BTO基PTC介电陶瓷具有阻晶作用。
实施例2较对比例更加均匀，Bi2O3可以改善显微结构，减少材料高频下的磁损耗并提高材料机械性能。
图5可见实施例较对比例MnZn功率铁氧体高频损耗明显降低。
图6～图7可见实施例较对比例MnZn功率铁氧体涡流损耗明显降低，涡流损耗比重显著下降，BTO的高电阻特性可以降低涡流损耗。
图8～图9可见实施例较对比例MnZn功率铁氧体剩余损耗明显降低，Bi2O3可以改善显微结构，进一步降低材料剩余损耗及其比重。
图10可见实施例较对比例MnZn功率铁氧体抗弯强度得到提高。

Claims (4)

1.高力学性能低损耗MnZn功率铁氧体材料制备方法，其特征在于，包括以下步骤：
(1)BTO基PTC介电陶瓷粉体制备：
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，预烧后加入0.2～0.4mol％Al2O3、1～2mol％SiO2、0.2～0.4mol％Y2O3后进行二次球磨，造粒成型后在1300～1400℃保温1～3h条件下完成空气烧结，碾碎磨粉为粒径0.5～1μm的陶瓷粉体；
(2)MnZn铁氧体预烧料制备
以Fe2O3、ZnO和MnO作为原料，按照主成分54.6～55.6mol％Fe2O3和8～10mol％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1～3h，获得MnZn功率铁氧体预烧料；
(3)掺杂处理
以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：0.01～0.03wt％V2O5、0.05～0.15wt％TiO2、0.01～0.03wt％Bi2O3、0.1～0.3wt％Co2O3、0.01～0.03wt％NiO和0.02～0.08wt％BTO基PTC介电陶瓷粉体，二次球磨；
(4)样品成型
将二次球磨后得到的球磨料烘干，然后按重量百分比加入8～15wt％的PVA有机粘合剂进行造粒，成型；
(5)烧结
将成型的生坯件进行高温烧结。
2.如权利要求1所述的高力学性能低损耗MnZn功率铁氧体材料制备方法，其特征在于，所述步骤1)中，预烧温度为1100～1200℃，保温时间0.5～2h。
3.如权利要求1所述的高力学性能低损耗MnZn功率铁氧体材料制备方法，其特征在于，所述步骤(5)的烧结温度为1120～1200℃，保温时间6～10h，烧结氧分压控制为2～5％。
4.如权利要求1所述的高力学性能低损耗MnZn功率铁氧体材料制备方法，其特征在于，所述步骤(1)中，x＝35，y＝15，z＝50，预烧后加入0.25mol％Al2O3、1.2mol％SiO2、0.25mol％Y2O3；
所述步骤(3)中，各添加剂的加入量为：
0.03wt％V2O5、0.06wt％TiO2、0.015wt％Bi2O3、0.3wt％Co2O3、0.03wt％NiO和0.03wt％～0.06wt％BTO基PTC介电陶瓷粉体。
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