CN112142457A - 宽频高磁导率高阻抗锰锌铁氧体及其制备方法 - Google Patents

宽频高磁导率高阻抗锰锌铁氧体及其制备方法 Download PDF

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CN112142457A
CN112142457A CN202010993430.3A CN202010993430A CN112142457A CN 112142457 A CN112142457 A CN 112142457A CN 202010993430 A CN202010993430 A CN 202010993430A CN 112142457 A CN112142457 A CN 112142457A
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zinc ferrite
impedance
permeability
manganese
functional components
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孙科
徐士亮
宋兴连
赵齐民
魏秀璐
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Linyi Chunguang Magnetic Industry Co ltd
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Abstract

本发明提供一种宽频高磁导率高阻抗锰锌铁氧体及其制备方法，涉及磁性材料技术领域，用以解决现有技术中1MHZ以上高频锰锌铁氧体电阻率低、介电常数高，无法适用的问题，而在此高频下适用NiZn铁氧体则存在成本高的问题。本发明采用贫铁类配方，通过混合、预烧、研磨、喷雾造粒、压制成型和烧结步骤，得到的环状磁芯，在1‑100MH在有较高的阻抗和较高的磁导率。

Description

宽频高磁导率高阻抗锰锌铁氧体及其制备方法
技术领域
本发明涉及磁性材料技术领域，具体地说，涉及一种宽频高磁导率高阻抗锰锌铁氧体及其制备方法。
背景技术
在电子信息时代，随着通信卫星、移动通信、计算机应用的高速发展，电磁干扰(EMI)在军事和民用电子信息领域的影响越来越严重，对公共环境和人身安全及信息保密造成了很大的危害。解决电磁污染和提高电子设备抗电磁干扰能力的有效办法是采用电磁兼容(EMC)设计，其中需用到大量的抗电磁干扰材料。随着电子设备的小型化、高频化发展，迫切希望能有在高频下具有高磁导率和高阻抗的电子材料。MnZn铁氧体与NiZn铁氧体相比，其电阻率低，介电常数高等原因，很难适应1MHz以上高频使用，所以在1MHz以上频率使用的器件大多是NiZn铁氧体材料。然而NiZn材料制造成本高，低频段磁导率和阻抗低，应用也收到一定限制。贫铁类MnZn铁氧体材料低频段磁导率高，同时电阻率较高，因而高频段阻抗也较高。与NiZn材料相比，其制造成本也低，可以代替部分NiZn材料，应用于制作中高频抗电磁干扰器件。
发明内容
为解决上述问题，本发明提供一种宽频高磁导率高阻抗锰锌铁氧体及其制备方法，其采用贫铁类配方，具有宽频、高磁导率、高阻抗特性。
本发明所述的宽频高磁导率高阻抗锰锌铁氧体，包括功能性组分和辅助性组分，功能性组分及用量为：Fe2O3:46.5-49.5mol％，ZnO:16.5-18.5mol％，余量为MnO，三种功能性组分的摩尔比之和为100％；所述辅助性组分为Co2O3、SiO2、CaCO3、Nb2O5、V2O5、TiO2和SnO2。
所述辅助组分的用量为：0.01-0.02％SiO2，0.03-0.05％CaCO3，0.02-0.04％Nb2O5，0.03-0.05％V2O5，0.1-0.2％TiO2，0.1-0.2％SnO2,0.4-0.7％Co2O3，以上百分数为质量百分数。
本发明的另一个目的在于提供一种宽频高磁导率高阻抗锰锌铁氧体的制备方法，包括以下步骤：(1)将功能性组分进行湿式混合；(2)预烧；(3)加入辅助性组分，研磨；(4)喷雾造粒；(5)压制成型；(6)烧结：以1-3.5℃/min的速度升温到600℃，保温0.3-2h；以0.5-1℃升温速度升温到800℃，将氧分压降低至5-10％；以4-6℃/min，升温到1360-1380℃，升温段氧分压保持在5-10％，保温时间4-8h。
进一步的，步骤(7)保温过程结束后，平衡气氛中以3-6℃/min速度冷却到室温。
进一步的，步骤(1)中湿式混合步骤加水量为功能性组分总重量的50-80％，混合时间为40-60分钟。
进一步的，步骤(2)中混合后的物料经干燥后置于马弗炉中预烧，预烧温度为850-950℃，预烧时间为30-60min，气氛为空气气氛。
进一步的，步骤(3)中研磨之前先将辅助性组分加入到功能性组分中，混合后置于篮式砂磨机中、砂磨介质为水，砂磨50-120分钟后加入0.05-0.1％的PVA，以上占比为质量分数，砂磨总时间为120min。
进一步的，步骤(4)喷雾造粒进口温度350-400℃，出口温度130-150℃，颗粒形貌为规则的球形。
进一步的，步骤(5)喷雾造粒后的颗粒压制成外径37±1mm,内径24±1mm,高度29±1mm的环状毛坯，毛坯密度2.6±0.1g/cm3。
与现有技术相比，本发明的有益效果是：本发明所述的配方，以及制备工艺提供的是贫铁类锰锌铁氧体，其具有较高的磁导率、电阻和高频阻抗特性，较NiZn铁氧体的成本显著降低，可以在1MHz以上高频使用。
具体实施方式
下面结合实施例对本发明做进一步解释和说明。
实施例1
本发明所述的宽频高磁导率高阻抗锰锌铁氧体，包括功能性组分和辅助性组分，功能性组分及用量为：Fe2O3:48.5mol％，ZnO:17.5mol％，MnO：34mol％；所述辅助性组分及占功能性组分质量的百分比为：0.01％SiO2、0.03％CaCO3、0.02％Nb2O5、0.03％V2O5、0.2％TiO2、0.2％SnO2和0.4％Co2O3。
其制备方法，步骤如下：
(1)将功能性组分进行湿式混合；湿式混合步骤加水量为功能性组分总重量的50％，混合时间为50分钟。
(2)预烧；混合后的物料经干燥后置于马弗炉中预烧，预烧温度为950℃，预烧时间为30min，气氛为空气气氛。
(3)加入辅助性组分，研磨：研磨之前先将辅助性组分加入到功能性组分中，混合后置于篮式砂磨机中砂磨，砂磨介质为水，砂磨50min后加入0.1％(质量分数)的PVA，继续研磨，砂磨总时间为120min。
(4)喷雾造粒；喷雾造粒进口温度400℃，出口温度130℃，颗粒形貌为规则的球形。
(6)压制成型；压制成外径37mm,内径24mm,高度29mm的环状毛坯，毛坯密度2.6g/cm3。
(7)烧结：以2℃/min的速度升温到600℃，保温1h；以0.8℃升温速度升温到800℃，将氧分压降低至8％；以5℃/min，升温到1370℃，保温时间6h，升温段氧分压保持在8％。保温过程结束后，平衡气氛中以5℃/min速度冷却到室温。
通过本实施例获得产品，在1MHz，0.25V测试条件下经测量阻抗为40Ω，在25MHz，0.25V测试条件下阻抗为120Ω；100MHz,0.25V测试条件下阻抗为160Ω。在1KHz，<0.25mT测试条件下的磁导率4200，表面电阻1.4MΩ。
实施例2
本发明所述的宽频高磁导率高阻抗锰锌铁氧体，包括功能性组分和辅助性组分，功能行组分及用量为：Fe2O3:46.5mol％，ZnO:16.5mol％，余量为MnO，三种功能性组分的摩尔比之和为100％；所述辅助性组分及用量为：0.02％SiO2，0.05％CaCO3，0.04％Nb2O5，0.03％V2O5，0.1％TiO2，0.1％SnO2,0.4％Co2O3，辅助组分用量为质量百分数。
其制备方法，步骤如下：
(1)将功能性组分进行湿式混合；湿式混合步骤加水量为功能性组分总重量的80％，混合时间为60分钟。
(2)预烧；混合后的物料经干燥后置于马弗炉中预烧，预烧温度为900℃，预烧时间为60min，气氛为空气气氛。
(3)加入辅助性组分，研磨；研磨之前先将辅助性组分加入到功能性组分中，混合后置于篮式砂磨机中、砂磨介质为水，砂磨90min后加入0.07％的PVA(质量分数)后继续研磨，砂磨总时间为120min。
(4)喷雾造粒；喷雾造粒进口温度380℃，出口温度150℃，颗粒形貌为规则的球形。
(6)压制成型；压制成外径36mm,内径23mm,高度28mm的环状毛坯，毛坯密度2.71g/cm3。
(7)烧结：以3℃/min的速度升温到600℃，保温0.8h；以0.5℃升温速度升温到800℃，将氧分压降低至5％；以4℃/min，升温到1380℃，保温时间4h，升温段氧分压保持在5％。保温过程结束后，平衡气氛中以3℃/min速度冷却到室温。
本发明产品为Ф36*23*28mm的环状磁芯，在1-100MH在有较高的阻抗：1MHz，0.25V测试条件下阻抗50Ω，25MHz，0.25V测试条件下阻抗124Ω，100MHz,0.25V测试条件下阻抗160Ω。并且还有较高的磁导率，1KHz，<0.25mT测试条件下的磁导率4100，表面电阻在1.2MΩ。
实施例3
本发明所述的宽频高磁导率高阻抗锰锌铁氧体，包括功能性组分和辅助性组分，功能行组分及用量为：，Fe2O3:49.5mol％，ZnO:18.5mol％，余量为MnO，三种功能性组分的摩尔比之和为100％；所述辅助性组分及用量为：0.015％SiO2，0.04％CaCO3，0.03％Nb2O5，0.04％V2O5，0.15％TiO2，0.16％SnO2,0.6％Co2O3，以上百分数为重量百分数。其制备方法，步骤如下：
(1)将功能性组分进行湿式混合；湿式混合步骤加水量为功能性组分总重量的70％，混合时间为50分钟。
(2)预烧；混合后的物料经干燥后置于马弗炉中预烧，预烧温度为850℃，预烧时间为50min，气氛为空气气氛。
(3)加入辅助性组分，研磨；研磨之前先将辅助性组分加入到功能性组分中，混合后置于篮式砂磨机中、砂磨介质为水，砂磨50min后加入0.07％的PVA，砂磨总时间为120min。
(4)喷雾造粒；喷雾造粒进口温度400℃，出口温度130℃，颗粒形貌为规则的球形。
(6)压制成型；压制成外径36mm,内径23mm,高度28mm的环状毛坯，毛坯密度2.5g/cm3。
(7)烧结：以3.5℃/min的速度升温到600℃，保温2h；以1℃升温速度升温到800℃，将氧分压降低至10％；以6℃/min，升温到1380℃，保温时间8h，升温段氧分压保持在10％。保温过程结束后，平衡气氛中以6℃/min速度冷却到室温。
本发明产品为Ф36*23*28mm的环状磁芯，在1-100MH在有较高的阻抗：1MHz，0.25V测试条件下阻抗42Ω，25MHz，0.25V测试条件下阻抗122Ω，100MHz,0.25V测试条件下阻抗165Ω。并且还有较高的磁导率，1KHz，<0.25mT测试条件下的磁导率4100，表面电阻在1.1MΩ。

Claims (9)

1.一种宽频高磁导率高阻抗锰锌铁氧体，其特征在于，包括功能性组分和辅助性组分，功能性组分及用量为：Fe2O3:46.5-49.5mol％，ZnO:16.5-18.5mol％，余量为MnO，三种功能性组分的摩尔比之和为100％；所述辅助性组分为Co2O3,SiO2，CaCO3，Nb2O5，V2O5，TiO2，SnO2。
2.根据权利要求1所述的宽频高磁导率高阻抗锰锌铁氧体，其特征在于，辅助性组分的用量为：0.01-0.02％SiO2，0.03-0.05％CaCO3，0.02-0.04％Nb2O5，0.03-0.05％V2O5，0.1-0.2％TiO2，0.1-0.2％SnO2,0.4-0.7％Co2O3，以上百分数为质量百分数。
3.一种权利要求1或2所述的宽频高磁导率高阻抗锰锌铁氧体的制备方法，其特征在于，包括以下步骤：(1)将功能性组分进行湿式混合；(2)预烧；(3)加入辅助性组分，研磨；(4)喷雾造粒；(5)压制成型；(6)烧结：以1-3.5℃/min的速度升温到600℃，保温0.3-2h；以0.5-1℃升温速度升温到800℃，将氧分压降低至5-10％；以4-6℃/min，升温到1360-1380℃，升温段氧分压保持在5-10％，保温时间4-8h。
4.根据权利要求3所述的宽频高磁导率高阻抗锰锌铁氧体的制备方法，其特征在于，步骤(7)保温过程结束后，平衡气氛中以3-6℃/min速度冷却到室温。
5.根据权利要求3所述的宽频高磁导率高阻抗锰锌铁氧体的制备方法，其特征在于，步骤(1)中湿式混合步骤加水量为功能性组分总重量的50-80％，混合时间为40-60分钟。
6.根据权利要求3所述的宽频高磁导率高阻抗锰锌铁氧体的制备方法，其特征在于，步骤(2)中混合后的物料经干燥后置于马弗炉中预烧，预烧温度为850-950℃，预烧时间为30-60min，气氛为空气气氛。
7.根据权利要求3所述的宽频高磁导率高阻抗锰锌铁氧体的制备方法，其特征在于，步骤(3)中研磨之前先将辅助性组分加入到功能性组分中，混合后置于篮式砂磨机中、砂磨介质为水，砂磨50-120分钟后加入0.05-0.1％的PVA，以上占比为质量分数，砂磨总时间为120min。
8.根据权利要求3所述的宽频高磁导率高阻抗锰锌铁氧体的制备方法，其特征在于，步骤(4)喷雾造粒进口温度350-400℃，出口温度130-150℃，颗粒形貌为规则的球形。
9.根据权利要求3所述的宽频高磁导率高阻抗锰锌铁氧体的制备方法，其特征在于，步骤(5)喷雾造粒后的颗粒压制成外径37±1mm,内径24±1mm,高度29±1mm的环状毛坯，毛坯密度2.6±0.1g/cm3。
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