CN113200741B - 一种5g应用低损耗软磁铁氧体材料及其制备方法 - Google Patents

一种5g应用低损耗软磁铁氧体材料及其制备方法 Download PDF

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CN113200741B
CN113200741B CN202110534300.8A CN202110534300A CN113200741B CN 113200741 B CN113200741 B CN 113200741B CN 202110534300 A CN202110534300 A CN 202110534300A CN 113200741 B CN113200741 B CN 113200741B
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soft magnetic
modified
magnetic ferrite
ferrite material
loss
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CN113200741A (zh
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姚木有
苏荣佳
林正崇
谭福清
郭皓
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Guangdong Zhaoqing Weishuo Electronics Co ltd
Hubei Weishuo New Material Co ltd
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Hubei Weishuo New Material Co ltd
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Abstract

本发明属于铁氧体合成技术领域，一种5g应用低损耗软磁铁氧体材料及其制备方法，原料包括改性Fe2O3、Mn3O4、ZnO的混合物，原料含量改性Fe2O3为36.8mol％～38.5mol％、ZnO为26.4mol％～28.2mol％，余量为Mn3O4，软磁铁氧体材料中还包括添加剂，添加剂包括CaCO3、Nb2O5、Bi2O3、V2O5、Co2O3、MoO3中的至少四种，软磁铁氧体材料中还包括阻畸剂，本发明采用Fe2O3内部包裹SiC纤维的方式进行改性Fe2O3，改性后的原料能够进行从运料混合后的晶体内部的各个方向进行掺杂，掺杂效果更显著，同时阻畸剂在晶体表面形成的阻隔层能够减少空隙的同时还能够使晶格不发生形变，并且该阻畸剂在后续的烧结过程中会挥发，使铁氧体能够在保证较低的介电损耗的同时还能够保持较高的磁导率。

Description

一种5g应用低损耗软磁铁氧体材料及其制备方法
技术领域
本发明属于铁氧体合成技术领域，特别涉及一种5g应用低损耗软磁铁氧体材料及其制备方法。
背景技术
随着电源技术与通信技术的发展，电源的向更节能、更小型化方向发展对材料功率损耗要求更高，现代5G通信设备的户外设施，如电源、中继器、微波接力站、海底电缆、光缆水下设备等，不仅要求耐高温，还要承受严寒，要求设备都能可靠稳定地工作。因而要求材料在-40℃～+140℃，甚至到160℃的宽温范围，这就要求材料从低温到高温都具有很高的磁感应强度和低的功率损耗。
尽管5G通信基站电源前景十分可观，但目前5G基站耗电也成为阻碍其发展的绊脚石，电源、器件厂商在迎接机遇的同时，更要跨越功耗大关、耐高温大关等各项考验。业内人士表示，与4G电源相比，5G电源没有风扇，因此选用的器件需满足140℃甚至到160℃耐高温规格。近年来,行业内，为了得到5G应用于通信以及网络设施的高性能功率铁氧体材料技术人员做了大量研究工作，可谓硕果累累，例如东磁公司的专利文献CN 102693807 A公布了一种超宽温低损耗高磁通密度MnZn功率铁氧体及其制备方法，该超宽温低损耗高磁通密度MnZn功率铁氧体在100kHz、200mT的条件下，25℃功耗≤390mW/cm 3，120℃功耗≤ 330mW/cm 3，140℃功耗≤400mW/cm 3，在1194A/m、50Hz的条件下，25℃的饱和磁通密度≥540，此材料具备较好的宽温低损性能，但并未体现出具备在更宽至160℃的范围内具有功率损耗特性。
提供一种高感应强度、宽温低损软磁铁氧体材料，要求宽温下传输损耗小、磁感应强度高抗饱和能力强的变压器中，是当前电源技术与通信技术的关键重要材料。
发明内容
本发明的目的是提供一种5g应用低损耗软磁铁氧体材料及其制备方法，提供了一种高感应强度、宽温低损软磁铁氧体材料。
本发明的上述技术目的是通过以下技术方案得以实现的：一种5g应用低损耗软磁铁氧体材料及其制备方法，其特征在于：原料包括改性Fe2O3、Mn3O4、ZnO的混合物，所述原料含量改性Fe2O3为36.8mol％～38.5mol％、ZnO为26.4mol％～28.2mol％，余量为Mn3O4；
所述软磁铁氧体材料中还包括添加剂，所述添加剂包括CaCO3、Nb2O5、Bi2O3、V2O5、Co2O3、MoO3中的至少四种；
所述软磁铁氧体材料中还包括阻畸剂。
进一步的，所述改性Fe2O3通过一下步骤制备：将Fe2O3与去离子水混合后放入到超声波细胞破碎机中超声5min，之后再采用180nm的过滤膜进行过滤，得到Fe2O3分散液，在Fe2O3分散液加入聚乙烯吡咯烷酮溶液后再放入到超声波细胞破碎机中超声5min，得到Fe2O3喷涂物，再采用超声喷涂机将Fe2O3喷涂物喷涂到SiC纤维表面，得到改性Fe2O3。
进一步的，所述改性Fe2O3表面Fe2O3喷涂物喷涂厚度为35nm-45nm。
进一步的，所述添加剂还包括Re2SnO5。
进一步的，所述Re2SnO5中的Re稀土元素为铈元素、镨元素、镝元素中的一种。
进一步的，阻畸剂包括聚环氧琥珀酸、氨基三甲叉膦酸、乙二胺四甲叉膦酸中的一种。
进一步的，一种5g应用低损耗软磁铁氧体材料及其制备方法，包括以下步骤：
(1)将取一定质量比的改性Fe2O3、Mn3O4、ZnO混合料中加入锆球和液体形成料：球：液比为1：3：2的球磨介质后，放入球磨灌中进行混合球磨形成粉体，球磨时间80min，浆料平均粒径在1.1μm；
(2)将步骤(1)得到的粉体使用天然气回转窑在空气条件下温度为960℃预烧4个小时，进料量2～3kg/h，转速2N/min，得到尖晶石合成度为10～20％的铁氧体粉体。
(3)将步骤(2)所得铁氧体粉体与添加剂按比例混合，并将混合后的物料放入到球磨灌中进行二次球磨，其中：料：球：液比为1：5：1，球磨70min后，再加入少量的阻畸剂继续球磨20min，得到平均粒径在1.1-1.4μm的粉料；
(4)造粒成型，在步骤(3)得到的粉料中加入浓度为8％的聚乙烯醇搅拌15min，混合完全后，使粉料团聚成具有流动性的小颗粒，筛选出40目到200目之间的颗粒填入特定尺寸与形状的磨具中进行单向加压，脱模后形成得到生坯；
(5)烧结，对步骤(3)中形成的生坯进行保温排胶后烧结，在起始温度为50℃，以 2～3℃/min的速度升温，温度达到1380℃后，将氧含量控制在3％～4％之间，持续致密化时间 2～3小时，再将氧含量降低到1-2％之间，保温6-7个小时，在平衡气氛中降温，采用2～3℃/min 的降温速度将温度从1380℃下降到25℃，得到最终软磁铁氧体材料。
本发明的有益效果是：
1、本发明采用Fe2O3内部包裹SiC纤维的方式进行改性Fe2O3，改性后的原料能够进行从混合后的原料晶体内部的各个方向进行掺杂，而不止是从外部进行掺杂，掺杂效果更显著，同时阻畸剂在晶体表面形成的阻隔层能够减少晶体空隙的同时还能够使晶格不发生形变，并且该阻畸剂在后续的烧结过程中会挥发掉，不影响后续Mn Zn铁氧体材料的使用，使铁氧体能够在保证较低的介电损耗的同时还能够保持较高的磁导率。
2、本发明中通过在SiC纤维表面包裹Fe2O3分散液进而形成改性Fe2O3，一方面，由于单独的碳纤维的抗氧化性差，不适于高温条件下实用，而SiC纤维是一种介电材料，具有耐高温、抗氧化、耐化学腐蚀、微波电磁性能可调等特点，具有良好的吸波效果，但吸波宽度小，而包裹Fe2O3之后，改性Fe2O3对电磁波的吸收能力显著增强，能够具有高磁导率，另一方面，被包裹在SiC纤维能够更好地占据到Fe2O3以及Mn Zn铁氧体中O原子密堆形成的四面体和八面体空隙进而调控Mn Zn铁氧体的电磁性能，降低电导损耗，避免了外加添加剂流动性较强而不易进入到空隙中而掺杂失败的现象发生，此外，控制Fe2O3的厚度不仅能够控制Fe2O3的添加含量，还能够避免Fe2O3厚度较大使SiC无法从Fe2O3覆盖层中透出来。
3、本发明在软磁铁氧体材料添加了能够改变其性能的添加剂，一方面，部分添加剂如 CaCO3和Nb2O5具有较高的电阻率，通过聚集在晶界添加剂不仅能够调控晶粒的生长过程，阻碍晶粒的生长，细化晶粒，还能够通过提高晶界的电阻率从而抑制高频损耗，另一方面，部分添加剂如Bi2O3和V2O5一般具有较高或较低的熔点，在后续烧结过程中影响晶粒的生长过程而影响样品最终的显微结构，部分添加剂如Co2O3中的Co3+半径与空隙半径相近，能够进入到Mn Zn铁氧体的晶格内部而直接影响Mn Zn铁氧体的磁性能，同时，本发明中涉及上的添加剂基本包含了以上全部功能，通过多种添加剂的相互作用，既能够促进晶粒的生长，也能够抑制晶粒的生长，能够细化晶粒并使晶粒变得均匀，同时还能够改善Mn Zn铁氧体的显微结构，使最终Mn Zn铁氧体具有高温下高频损耗较低的效果。
4、本发明制备的软磁铁氧体材料中添加的Re2SnO5，由于稀土元素最外层所屏蔽的未成对的4f电子使其原子或离子具有特殊的电磁性能，铁氧体中的铁离子中的3d电子暴露在晶场作用下，同时受到邻近离子电场的作用，其磁矩接近于轨道冻结状态，而稀土离子的磁矩在离子内部的4f电子层，晶场作用被外部5s和5p电子屏蔽，因此将稀土离子掺杂到铁氧体中，稀土离子中的轨道动量距能够对铁氧体中的磁性能、吸波特性以及高频损耗有较大的改善。
5、本发明添加剂Re2SnO5中的稀土元素为铈元素、镨元素、镝元素中的一种，由于Ce离子的半径与铁氧体晶格空隙相近，同时Ce3+为顺磁性物质，Ce4+为抗磁性物质，两者相互作用，使铁氧体能够一直保持较稳定的磁通率，同时，变价的Ce离子进入到铁氧体晶格取代Fe3+后，通过缺陷结构传递电荷，使得部分Fe3+转化为Fe2+，达到电价平衡，降低介电损耗，而镨和镝元素具有较强的各向异性，能够对铁氧体的磁性能带来较大的改观；Sn元素主要通过分布在晶界处，位于晶界处的Sn元素能够将已取代了的稀土元素离子阻隔在晶格内部，能够避免高温情况下各已经进入到晶格内部的物质会从晶格内脱落出来，造成间隙增大的现象发生，因此Sn元素能够稳定稀土元素作用的稳定性，降低介电损耗。
6、本发明中通过添加的阻畸剂能够降低铁氧体晶格发生畸变的现象，由于各添加剂的引入，部分元素掺杂到晶格空隙中，在改善铁氧体性能的同时，会导致各晶格发生畸变，最终导致铁氧体的介电损耗发生变化，添加微量聚环氧琥珀酸、氨基三甲叉膦酸或乙二胺四甲叉膦酸中的一种，首先，由于较多多余的正电荷，为保持电中性，需要电子补偿正电荷，从而导致漏电导损耗增加，而阻畸剂高温条件下键断裂形成的阴离子能够补偿晶格表面的正电荷，减小了电子的损耗，其次，在阻畸剂能够在晶格表面突出的化学键以及离子形成一层阻隔层，能够避免具有吸附特性的稀土离子使原料中各元素离子大量的聚集到晶格表面，最终导致晶格形态以及体积发生较大的改变的情况发生，最后，形成的阻隔层还能够能够减少空隙的同时还能够使晶格不发生形变，使铁氧体能够在保证较低的介电损耗的同时还能够保持较高的磁导率，并且该阻畸剂在后续的烧结过程中会挥发，并不会影响后续然磁铁氧体材料的使用。
7、本发明制备的软磁铁氧体材料，在球磨过程中，采用锆球作为球磨介质，是为了尽量不引入额外的铁元素而造成成分偏析；此外，氧化锆作为一种高电阻材料，即使引入到粉料中，也会增加Mn Zn铁氧体的电阻率，降低接电损耗。
具体实施方式
下面将对实施例中的技术方案进行清楚、完整地描述。显然，所描述的实施例仅仅是本发明的一部分实施例，而不是全部的实施例。基于本发明的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
一种5g应用低损耗软磁铁氧体材料及其制备方法，包括以下步骤：
(1)取改性36.8mol％改性Fe2O3、36.8mol％Mn3O4、26.4mol％ZnO混合料中加入锆球和液体形成料：球：液比为1：3：2的球磨介质后，放入球磨灌中进行混合球磨形成粉体，球磨时间80min，浆料平均粒径在1.1μm左右。
(2)将步骤(1)得到的粉体使用天然气回转窑在空气条件下温度为960℃预烧4个小时，进料量2kg/h，转速2N/min，得到尖晶石合成度为12％的铁氧体粉体。
(3)将步骤(2)所得铁氧体粉体中添加300ppmCaCO3、100ppmNb2O5、50ppmBi2O3、100ppmCo2O3后混合均匀，并将混合后的物料放入到球磨灌中进行二次球磨，其中：料：球：液比为1：5：1，球磨70min后，得到平均粒径在1.2μm的粉料。
(4)造粒成型，在步骤(3)得到的粉料中加入浓度为8％的聚乙烯醇搅拌15min，混合完全后，使粉料团聚成具有流动性的小颗粒，筛选出40目到200目之间的颗粒填入特定尺寸与形状的磨具中进行单向加压，脱模后形成得到生坯。
(5)烧结，对步骤(4)中形成的生坯进行保温排胶后烧结，在起始温度为50℃，以2～3℃/min的速度升温，温度达到1380℃后，将氧含量控制在3％，持续致密化时间2，再将氧含量降低到1.5％，保温6小时，在平衡气氛中降温，采用2℃/min的降温速度将温度从1380℃下降到25℃，得到最终软磁铁氧体材料。
实施例2
一种5g应用低损耗软磁铁氧体材料及其制备方法，包括以下步骤：
(1)取改性38.5mol％改性Fe2O3、33.3mol％Mn3O4、28.2mol％ZnO混合料中加入锆球和液体形成料：球：液比为1：3：2的球磨介质后，放入球磨灌中进行混合球磨形成粉体，球磨时间80min，浆料平均粒径在1.1μm左右。
(2)将步骤(1)得到的粉体使用天然气回转窑在空气条件下温度为960℃预烧4个小时，进料量2.5kg/h，转速2N/min，得到尖晶石合成度为15％的铁氧体粉体。
(3)将步骤(2)所得铁氧体粉体中添加300ppmCaCO3、100ppmV2O5、50ppmBi2O3、100ppmCo2O3、300Ce2SnO5后混合均匀，并将混合后的物料放入到球磨灌中进行二次球磨，其中：料：球：液比为1：5：1，球磨70min后，得到平均粒径在1.3μm的粉料。
(4)造粒成型，在步骤(3)得到的粉料中加入浓度为8％的聚乙烯醇搅拌15min，混合完全后，使粉料团聚成具有流动性的小颗粒，筛选出40目到200目之间的颗粒填入特定尺寸与形状的磨具中进行单向加压，脱模后形成得到生坯。
(5)烧结，对步骤(4)中形成的生坯进行保温排胶后烧结，在起始温度为50℃，以3℃/min 的速度升温，温度达到1380℃后，将氧含量控制在4％，持续致密化时间2小时，再将氧含量降低到1％，保温7个小时，在平衡气氛中降温，采用3℃/min的降温速度将温度从1380℃下降到25℃，得到最终软磁铁氧体材料。
实施例3
一种5g应用低损耗软磁铁氧体材料及其制备方法，包括以下步骤：
(1)取改性37.6mol％改性Fe2O3、34.9mol％Mn3O4、27.5mol％ZnO混合料中加入锆球和液体形成料：球：液比为1：3：2的球磨介质后，放入球磨灌中进行混合球磨形成粉体，球磨时间80min，浆料平均粒径在1.1μm左右。
(2)将步骤(1)得到的粉体使用天然气回转窑在空气条件下温度为960℃预烧4个小时，进料量2.7kg/h，转速2N/min，得到尖晶石合成度为18％的铁氧体粉体。
(3)将步骤(2)所得铁氧体粉体中添加200ppmCaCO3、100ppmV2O5、50ppmBi2O3、100ppmMoO3、300Pr2SnO5后混合均匀，并将混合后的物料放入到球磨灌中进行二次球磨，其中：料：球：液比为1：5：1，球磨70min后，再加入0.02mol％聚环氧琥珀酸继续球磨 20min，得到平均粒径在1.3μm的粉料。
(4)造粒成型，在步骤(3)得到的粉料中加入浓度为8％的聚乙烯醇搅拌15min，混合完全后，使粉料团聚成具有流动性的小颗粒，筛选出40目到200目之间的颗粒填入特定尺寸与形状的磨具中进行单向加压，脱模后形成得到生坯。
(5)烧结，对步骤(4)中形成的生坯进行保温排胶后烧结，在起始温度为50℃，以 2～3℃/min的速度升温，温度达到1380℃后，将氧含量控制在3.7％之间，持续致密化时间2.6 小时，再将氧含量降低到1.8％之间，保温6.6个小时，在平衡气氛中降温，采用3℃/min的降温速度将温度从1380℃下降到25℃，得到最终软磁铁氧体材料。
实施例4
一种5g应用低损耗软磁铁氧体材料及其制备方法，包括以下步骤：
(1)取改性37.6mol％改性Fe2O3、35.9mol％Mn3O4、26.5mol％ZnO混合料中加入锆球和液体形成料：球：液比为1：3：2的球磨介质后，放入球磨灌中进行混合球磨形成粉体，球磨时间80min，浆料平均粒径在1.1μm左右。
(2)将步骤(1)得到的粉体使用天然气回转窑在空气条件下温度为960℃预烧4个小时，进料量2.8kg/h，转速2N/min，得到尖晶石合成度为18％的铁氧体粉体。
(3)将步骤(2)所得铁氧体粉体中添加100ppmNb2O5、100ppmV2O5、50ppmBi2O3、100ppmMoO3、200Dy2SnO5后混合均匀，并将混合后的物料放入到球磨灌中进行二次球磨，其中：料：球：液比为1：5：1，球磨70min后，再加入0.015mol％氨基三甲叉膦酸继续球磨20min，得到平均粒径在1.3μm的粉料。
(4)造粒成型，在步骤(3)得到的粉料中加入浓度为8％的聚乙烯醇搅拌15min，混合完全后，使粉料团聚成具有流动性的小颗粒，筛选出40目到200目之间的颗粒填入特定尺寸与形状的磨具中进行单向加压，脱模后形成得到生坯。
(5)烧结，对步骤(4)中形成的生坯进行保温排胶后烧结，在起始温度为50℃，以3℃/min 的速度升温，温度达到1380℃后，将氧含量控制在4％之间，持续致密化时间2小时，再将氧含量降低到2％之间，保温6个小时，在平衡气氛中降温，采用2℃/min的降温速度将温度从 1380℃下降到25℃，得到最终软磁铁氧体材料。
实施例5
一种5g应用低损耗软磁铁氧体材料及其制备方法，包括以下步骤：
(1)取改性38.6mol％改性Fe2O3、33.9mol％Mn3O4、27.5mol％ZnO混合料中加入锆球和液体形成料：球：液比为1：3：2的球磨介质后，放入球磨灌中进行混合球磨形成粉体，球磨时间80min，浆料平均粒径在1.1μm左右。
(2)将步骤(1)得到的粉体使用天然气回转窑在空气条件下温度为960℃预烧4个小时，进料量2～3kg/h，转速2N/min，得到尖晶石合成度为10～20％的铁氧体粉体。
(3)将步骤(2)所得铁氧体粉体中添加100ppmNb2O5、100ppmV2O5、50ppmBi2O3、100ppmMoO3、200Dy2SnO5后混合均匀，并将混合后的物料放入到球磨灌中进行二次球磨，其中：料：球：液比为1：5：1，球磨70min后，再加入0.015mol％乙二胺四甲叉膦酸继续球磨20min，得到平均粒径在1.4μm的粉料。
(4)造粒成型，在步骤(3)得到的粉料中加入浓度为8％的聚乙烯醇搅拌15min，混合完全后，使粉料团聚成具有流动性的小颗粒，筛选出40目到200目之间的颗粒填入特定尺寸与形状的磨具中进行单向加压，脱模后形成得到生坯。
(5)烧结，对步骤(4)中形成的生坯进行保温排胶后烧结，在起始温度为50℃，以 2～3℃/min的速度升温，温度达到1380℃后，将氧含量控制在3％之间，持续致密化时间3小时，再将氧含量降低到2％之间，保温6个小时，在平衡气氛中降温，采用3℃/min的降温速度将温度从1380℃下降到25℃，得到最终软磁铁氧体材料。
表1原料添加比例及实施例性能测试结果
Figure GDA0003118971740000071
Figure GDA0003118971740000081
由上述表1结果可知，本发明的一种5g应用低损耗软磁铁氧体材料经测试，起始磁导率在 10kHz，50mV的条件下，达到了3200H/m，饱和磁通密度25℃达到了550以上，并且实施例2- 实施例5相比于实施例1的功率损耗大大降低，具备高磁导率的同时兼顾低损耗的性能。

Claims (5)

1.一种5g应用低损耗的软磁铁氧体材料，其特征在于：原料包括改性Fe2O3、Mn3O4、ZnO的混合物，所述原料含量改性Fe2O3为36.8 mol%～38.5mol%、ZnO为26.4mol%～28.2mol%，余量为Mn3O4；
所述软磁铁氧体材料中还包括添加剂，所述添加剂包括CaCO3、Nb2O5、Bi2O3、V2O5、Co2O3、MoO3中的至少四种；
所述改性Fe2O3通过在SiC纤维表面包裹Fe2O3分散液形成；
所述软磁铁氧体材料中还包括阻畸剂；
所述阻畸剂包括聚环氧琥珀酸、氨基三甲叉膦酸、乙二胺四甲叉膦酸中的一种。
2.根据权利要求1所述的一种5g应用低损耗的软磁铁氧体材料，其特征在于：所述改性Fe2O3通过以下步骤制备：将Fe2O3与去离子水混合后放入到超声波细胞破碎机中超声5min，之后再采用180nm的过滤膜进行过滤，得到Fe2O3分散液，在Fe2O3分散液加入聚乙烯吡咯烷酮溶液后再放入到超声波细胞破碎机中超声5min，得到Fe2O3喷涂物，再采用超声喷涂机将Fe2O3喷涂物喷涂到SiC纤维表面，得到改性Fe2O3。
3.根据权利要求2所述的一种5g应用低损耗的软磁铁氧体材料，其特征在于：所述改性Fe2O3表面Fe2O3喷涂物喷涂厚度为35nm-45nm。
4.根据权利要求1所述的一种5g应用低损耗的软磁铁氧体材料，其特征在于：所述添加剂还包括Re2SnO5。
5.根据权利要求4所述的一种5g应用低损耗的软磁铁氧体材料，其特征在于：所述Re2SnO5中的Re稀土元素为铈元素、镨元素、镝元素中的一种。
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