CN109626985B - 一种超高频高阻抗MnZn铁氧体材料 - Google Patents

一种超高频高阻抗MnZn铁氧体材料 Download PDF

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CN109626985B
CN109626985B CN201910112419.9A CN201910112419A CN109626985B CN 109626985 B CN109626985 B CN 109626985B CN 201910112419 A CN201910112419 A CN 201910112419A CN 109626985 B CN109626985 B CN 109626985B
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mnzn ferrite
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徐士亮
宋兴连
韩卫东
孔志强
解丽丽
吴士超
辛本奎
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Shandong Chunguang Magnetoelectric Technology Co ltd
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Abstract

本发明提出了一种超高频高阻抗MnZn铁氧体材料，其原料包括主要主料和辅料。一种超高频高阻抗MnZn铁氧体材料的制备方法，包括以下步骤：称取Fe2O3 52‑55mol％，Mn3O4 16‑18mol％，CuO 3‑5mol％，ZnO 22‑29mol％的主料，将主料放入到在篮式砂磨机中进行湿式混合，加水量为原料重量的50％，混合时间40‑60min。该超高频高阻抗MnZn铁氧体材料，具有高磁导率(μi＝3000)，同时具有高于常规高导MnZn铁氧体产品的高频阻抗，25MHz阻抗比常用的5K类MnZn铁氧体高导产品阻抗提高50％，100MHz阻抗比常用的5K类MnZn铁氧体高导产品阻抗高15％，电阻率比常用5K类MnZn铁氧体高导产品提高100倍左右，达到100Ω·m，可以满足电子产品的超高频高阻抗要求。

Description

一种超高频高阻抗MnZn铁氧体材料
技术领域
本发明涉及新型材料技术领域，具体为一种超高频高阻抗MnZn铁氧体材料。
背景技术
随着各种电子设备、电视网络、程控交换机、移动通信机及办公室自动化的日益普及，电磁干扰也日益成为了人们担心的一大环境污染。随着许多有源网络向小型化和高频华方向发展，其危害性越来越大。如在IT领域，高频的数据以有线和无线的方式向我们生存环境中注入新的噪音，主板线路中包括的大量有源器件，如晶体管、MOS管、震荡回路等，各自以其自身的股友震荡频率，通过微电子线路传递给其他器件，产生电磁干扰问题，影响整个系统的工作状态。抑制电磁干扰或者提高电子设备的抗电磁干扰能力最有效的方法是采用电磁兼容性设计，其中需要大量抗电磁干扰材料。铁氧体电感元器件具有优良的抗电磁干扰特性，成为抑制电磁干扰最重要并已获得普遍采用的电磁元件。锰锌铁氧体具有宽频带、高阻抗、较好的频率特性，可解决传导干扰、辐射干扰等问题，是常用的抗电磁干扰材料。常规MnZn铁氧体由于存在Fe2+和Fe3+，电子可以通过在两者之间跃迁，从而传导电流，因而其电阻率较低，高频阻抗特性差。
发明内容
本发明要解决的技术问题是克服现有的MnZn铁氧体高频低阻抗缺陷，开发出一种超高频高阻抗MnZn铁氧体材料，具有高磁导率，同时具有高于常规高导锰锌铁氧体产品的阻抗，25MHz阻抗比常用的5K类MnZn铁氧体高导产品阻抗提高50％，100MHz阻抗比常用的5K类MnZn铁氧体高导产品阻抗提高15％，可以满足电子产品的高频高阻抗要求，电阻率比常用5K类MnZn铁氧体高导产品提高100倍左右，达到100Ω·m，有效解决背景技术中的问题。
为实现上述目的，本发明提出：一种超高频高阻抗MnZn铁氧体材料，其原料包括主要主料和辅料，所述主料按摩尔百分比包括以下组分：Fe2O3 52-55mol％，Mn3O4 16-18mol％，CuO 3-5mol％，ZnO 22-29mol％。
作为本发明的一种优选技术方案：所述辅料按重量百分比包括以下组分： SiO2200-300ppm，CaO 500-800ppm，Nb2O5 300-500ppm，ZrO2 400-600ppm， V2O5 800-1000ppm，TiO2 1000-2000ppm，1000-2000ppmSnO2，Co2O3 500-1000ppm。
本发明还提供一种超高频高阻抗MnZn铁氧体材料的制备方法，包括以下步骤：
1)主料混合：称取Fe2O3 52-55mol％，Mn3O4 16-18mol％，CuO 3-5mol％， ZnO 22-29mol％的主料，将主料放入到在篮式砂磨机中进行湿式混合，加水量为原料重量的50％，混合时间40-60min，然后进行干燥；
2)原料预烧：干燥后的粉料放在乘烧板上，放入马弗炉中预烧，预烧温度950min，预烧时间30min，气氛为空气气氛，得到铁氧体预烧料；
3)添加辅料：称取SiO2 200-300ppm，CaO 500-800ppm，Nb2O5 300-500ppm， ZrO2400-600ppm，V2O5 800-1000ppm，TiO2 1000-2000ppm，1000-2000ppmSnO2， Co2O3 500-1000ppm作为辅料，并将辅料与预烧粉料一起放入篮式砂磨机中，砂磨介质为水，砂磨时间120min，砂磨50min后加入0.1％的PVA溶剂和0.1％的消泡剂；
4)造粒：砂磨后的料浆进行喷雾造粒，造粒进口温度400℃，出口温度 130℃，颗粒形貌呈规则的球形，中心内部无气孔，粒径大小均匀，成型性能较好；
5)颗粒定型：喷雾造粒后的颗粒压制成外径25mm，内径15mm，高度10mm 的环状毛坯，毛坯密度2.6±0.1g/cm3。
6)烧结：压制的毛坯在气氛保护钟罩炉中进行烧结，具体烧结过程为：以1-3.5℃/min的速度升温到600℃，在600℃保温0.3-2h，使毛坯中的有机物充分燃烧、挥发，然后以0.5-1℃升温速度升温到800℃，关闭炉门，向炉膛内充入氮气，将氧分压降低至5-10％，再将升温速度提高至4-6℃/min，升温到1300-1340℃，升温段氧分压保持在5-10％，保温过程氧分压在1-10％，保温时间4-8h，最后在平衡气氛中以3-6℃/min速度冷却到室温。
与现有技术相比，本发明的有益效果是：
1、该超高频高阻抗MnZn铁氧体材料，具有高磁导率(μi＝3000)，同时具有高于常规高导锰锌铁氧体产品的阻抗，0.25V，1Ts测试条件下，25MHz 阻抗比常用的5K类Mn Zn铁氧体高导产品阻抗提高50％，达到60Ω，100MHz 阻抗比常用的5K类高导MnZn铁氧体产品阻抗高15％，达到150Ω，电阻率比常用5K类MnZn铁氧体高导产品提高100倍左右，达到100Ω·m，可以满足电子产品的高频高阻抗要求。
2、本发明提供一种锰锌铁氧体产品的烧结温度和气氛曲线，可以保证产品具有高的磁导率和高的电阻率。
附图说明
图1为本发明一种超高频高阻抗MnZn铁氧体材料的制备流程图。
具体实施方式
下面将结合本发明实施例中的附图，对本发明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一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做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。
请参阅图1，本发明提供以下技术方案：
实施例一：
一种超高频高阻抗电子材料，其原料包括主要主料和辅料，主料按摩尔百分比包括以下组分：Fe2O3 52mol％，Mn3O4 16mol％，CuO 3mol％，ZnO 29mol％，辅料按容积浓度比包括以下组分：SiO2 200ppm，CaO 500ppm，Nb2O5 300ppm， ZrO2 400ppm，V2O5 800ppm，TiO21000ppm，1000ppmSnO2，Co2O3 500ppm。
本发明还提供一种超高频高阻抗MnZn铁氧体材料的制备方法，包括以下步骤：
1)主料混合：称取Fe2O3 52mol％，Mn3O4 16mol％，CuO 3mol％，ZnO 29mol％的主料，将主料放入到在篮式砂磨机中进行湿式混合，加水量为原料重量的 50％，混合时间40min，然后进行干燥；
2)原料预烧：干燥后的粉料放在乘烧板上，放入马弗炉中预烧，预烧温度950min，预烧时间30min，气氛为空气气氛，得到铁氧体预烧料；
3)添加辅料：称取SiO2 200ppm，CaO 500ppm，Nb2O5 300ppm，ZrO2 400ppm， V2O5800ppm，TiO2 1000ppm，1000ppmSnO2，Co2O3 500ppm作为辅料，并将辅料与预烧粉料一起放入篮式砂磨机中，砂磨介质为水，砂磨时间120min，砂磨50min后加入0.1％的PVA溶剂和0.1％的消泡剂；
4)造粒：砂磨后的料浆进行喷雾造粒，造粒进口温度400℃，出口温度 130℃，颗粒形貌呈规则的球形，中心内部无气孔，粒径大小均匀，成型性能较好；
5)颗粒定型：喷雾造粒后的颗粒压制成外径25mm，内径15mm，高度10mm 的环状毛坯，毛坯密度2.6±0.1g/cm3。
6)烧结：压制的毛坯在气氛保护钟罩炉中进行烧结，具体烧结过程为：以1℃/min的速度升温到600℃，在600℃保温0.3h，使毛坯中的有机物充分燃烧、挥发，然后以0.5℃升温速度升温到800℃，关闭炉门，向炉膛内充入氮气，将氧分压降低至5％，再将升温速度提高至4℃/min，升温到1300℃，升温段氧分压保持在5％，保温过程氧分压在1％，保温时间4h，最后在平衡气氛中以3℃/min速度冷却到室温。
实施例二：
一种超高频高阻抗MnZn铁氧体材料，其原料包括主要主料和辅料，主料按摩尔百分比包括以下组分：Fe2O3 53％，Mn3O4 17mol％，CuO 4mol％，ZnO 26mol％，辅料按容积浓度比包括以下组分：SiO2 230ppm，CaO 600ppm，Nb2O5 360ppm，ZrO2 460ppm，V2O5 860ppm，TiO2 1300ppm，1300ppmSnO2，Co2O3 660ppm。
本发明还提供一种超高频高阻抗电子材料的制备方法，包括以下步骤：
1)主料混合：称取Fe2O3 53％，Mn3O4 17mol％，CuO 4mol％，ZnO 25mol％的主料，将主料放入到在篮式砂磨机中进行湿式混合，加水量为原料重量的 50％，混合时间46min，然后进行干燥；
2)原料预烧：干燥后的粉料放在乘烧板上，放入马弗炉中预烧，预烧温度950min，预烧时间30min，气氛为空气气氛，得到铁氧体预烧料；
3)添加辅料：称取SiO2 230ppm，CaO 600ppm，Nb2O5 360ppm，ZrO2 460ppm， V2O5860ppm，TiO2 1300ppm，SnO2，Co2O3 660ppm作为辅料，并将辅料与预烧粉料一起放入篮式砂磨机中，砂磨介质为水，砂磨时间120min，砂磨50min 后加入0.1％的PVA溶剂和0.1％的消泡剂；
4)造粒：砂磨后的料浆进行喷雾造粒，造粒进口温度400℃，出口温度 130℃，颗粒形貌呈规则的球形，中心内部无气孔，粒径大小均匀，成型性能较好；
5)颗粒定型：喷雾造粒后的颗粒压制成外径25mm，内径15mm，高度10mm 的环状毛坯，毛坯密度2.6±0.1g/cm3。
6)烧结：压制的毛坯在气氛保护钟罩炉中进行烧结，具体烧结过程为：以2℃/min的速度升温到600℃，在600℃保温1h，使毛坯中的有机物充分燃烧、挥发，然后以0.7℃升温速度升温到800℃，关闭炉门，向炉膛内充入氮气，将氧分压降低至7％，再将升温速度提高至5℃/min，升温到1320℃，升温段氧分压保持在7％，保温过程氧分压在4％，保温时间5h，最后在平衡气氛中以3-6℃/min速度冷却到室温。
实施例三：
一种超高频高阻抗MnZn材料，其原料包括主要主料和辅料，主料按摩尔百分比包括以下组分：Fe2O3 54mol％，Mn3O4 17mol％，CuO 4mol％，ZnO 25mol％，辅料按容积浓度比包括以下组分：SiO2 260ppm，CaO 700ppm，Nb2O5 420ppm， ZrO2 520ppm，V2O5 920ppm，TiO21600ppm，SnO2，Co2O3 800ppm。
本发明还提供一种超高频高阻抗电子材料的制备方法，包括以下步骤：
1)主料混合：称取Fe2O3 54mol％，Mn3O4 17mol％，CuO 4mol％，ZnO 25mol％的主料，将主料放入到在篮式砂磨机中进行湿式混合，加水量为原料重量的 50％，混合时间53min，然后进行干燥；
2)原料预烧：干燥后的粉料放在乘烧板上，放入马弗炉中预烧，预烧温度950min，预烧时间30min，气氛为空气气氛，得到铁氧体预烧料；
3)添加辅料：称取SiO2 260ppm，CaO 700ppm，Nb2O5 420ppm，ZrO2 520ppm， V2O5920ppm，TiO2 1600ppm，1600ppmSnO2，Co2O3 800ppm作为辅料，并将辅料与预烧粉料一起放入篮式砂磨机中，砂磨介质为水，砂磨时间120min，砂磨50min后加入0.1％的PVA溶剂和0.1％的消泡剂；
4)造粒：砂磨后的料浆进行喷雾造粒，造粒进口温度400℃，出口温度 130℃，颗粒形貌呈规则的球形，中心内部无气孔，粒径大小均匀，成型性能较好；
5)颗粒定型：喷雾造粒后的颗粒压制成外径25mm，内径15mm，高度10mm 的环状毛坯，毛坯密度2.6±0.1g/cm3。
6)烧结：压制的毛坯在气氛保护钟罩炉中进行烧结，具体烧结过程为：以2.5℃/min的速度升温到600℃，在600℃保温1.5h，使毛坯中的有机物充分燃烧、挥发，然后以0.8℃升温速度升温到800℃，关闭炉门，向炉膛内充入氮气，将氧分压降低至8％，再将升温速度提高至5℃/min，升温到1330℃，升温段氧分压保持在8％，保温过程氧分压在8％，保温时间7h，最后在平衡气氛中以5℃/min速度冷却到室温。
实施例四：
一种超高频高阻抗MnZn铁氧体材料，其原料包括主要主料和辅料，主料按摩尔百分比包括以下组分：Fe2O3 55mol％，Mn3O4 18mol％，CuO 5mol％，ZnO 22mol％，辅料按容积浓度比包括以下组分：SiO2 300ppm，CaO 800ppm，Nb2O5 500ppm，ZrO2 600ppm，V2O51000ppm，TiO2 2000ppm，2000ppmSnO2，Co2O3 1000ppm。
本发明还提供一种超高频高阻抗MnZn铁氧体材料的制备方法，包括以下步骤：
1)主料混合：称取Fe2O3 55mol％，Mn3O4 18mol％，CuO 5mol％，ZnO 22mol％的主料，将主料放入到在篮式砂磨机中进行湿式混合，加水量为原料重量的 50％，混合时间60min，然后进行干燥；
2)原料预烧：干燥后的粉料放在承烧板上，放入马弗炉中预烧，预烧温度950min，预烧时间30min，气氛为空气气氛，得到铁氧体预烧料；
3)添加辅料：称取SiO2 300ppm，CaO 800ppm，Nb2O5 500ppm，ZrO2 600ppm， V2O51000ppm，TiO2 2000ppm，2000ppmSnO2，Co2O3 1000ppm作为辅料，并将辅料与预烧粉料一起放入篮式砂磨机中，砂磨介质为水，砂磨时间120min，砂磨50min后加入0.1％的PVA溶剂和0.1％的消泡剂；
4)造粒：砂磨后的料浆进行喷雾造粒，造粒进口温度400℃，出口温度 130℃，颗粒形貌呈规则的球形，中心内部无气孔，粒径大小均匀，成型性能较好；
5)颗粒定型：喷雾造粒后的颗粒压制成外径25mm，内径15mm，高度10mm 的环状毛坯，毛坯密度2.6±0.1g/cm3。
6)烧结：压制的毛坯在气氛保护钟罩炉中进行烧结，具体烧结过程为：以3.5℃/min的速度升温到600℃，在600℃保温2h，使毛坯中的有机物充分燃烧、挥发，然后以1℃升温速度升温到800℃，关闭炉门，向炉膛内充入氮气，将氧分压降低至10％，再将升温速度提高至6℃/min，升温到1340℃，升温段氧分压保持在10％，保温过程氧分压在10％，保温时间8h，最后在平衡气氛中以6℃/min速度冷却到室温。
该锰锌铁氧体材料在1-100MH在有较高的阻抗，以外径25mm，内径15mm，高10mm的圆环毛坯来测试，1MHz，0.25V测试条件下阻抗15Ω，25MHz，0.25V 测试条件下阻抗60Ω，100MHz，0.25V测试条件下阻抗150Ω。并且还有较高的磁导率，1KHz，＜0.25mT测试条件下的磁导率3000左右，电阻率在100Ω·m 以上。
本发明所制备的锰锌铁氧体产品为Φ25*15*10的圆环，磁芯无开裂与结晶现象。磁环的居里温度Tc＞92℃。1KHz，Bm＜0.25mT测试条件下，产品初始磁导率达到3000-4000。0.25V，单匝测试条件下，1MHz阻抗15Ω，25MHz阻抗60Ω，100MHz阻抗150Ω，电阻率在100Ω·m以上。
本发明好处：该超高频高阻抗MnZn铁氧体材料，具有高磁导率，同时具有高于常规高导锰锌铁氧体产品的阻抗，25MHz阻抗比常用的5K类MnZn铁氧体高导产品阻抗提高50％，100MHz阻抗比常用的5K类高导MnZn铁氧体产品阻抗高15％，电阻率比5K类MnZn高导铁氧体产品提高100倍，可以满足电子产品的超高频高阻抗要求。
尽管已经示出和描述了本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由所附权利要求及其等同物限定。

Claims (1)

1.一种超高频高阻抗MnZn铁氧体材料的制备方法，其特征在于：其原料包括主料和辅料 ，所述主料按摩尔百分比包括以下组分：Fe2O352-55mol％，Mn3O416-18mol％，CuO 3-5mol％，ZnO 22-29mol％；所述辅料按重量百分比包括以下组分：SiO2200-300ppm，CaO500-800pm，Nb2O5300-500ppmp，ZrO2400-600ppm，V2O5800-1000ppm，TiO21000-2000ppm，SnO21000-2000ppm，Co2O3500-1000ppm；
所述超高频高阻抗MnZn铁氧体材料的制备方法包括以下步骤：
1)主料混合：称取Fe2O352-55mol％，Mn3O416-18mol％，CuO 3-5mol％，ZnO 22-29mol％的主料，将主料放入到在篮式砂磨机中进行湿式混合，加水量为原料重量的50％，混合时间40-60min，然后进行干燥；
2)原料预烧：干燥后的粉料放在承烧板 上，放入马弗炉中预烧，预烧温度950℃，预烧时间30min，气氛为空气气氛，得到铁氧体预烧料；
3)添加辅料：称取SiO2200-300ppm，CaO 500-800ppm，Nb2O5300-500ppm，ZrO2400-600ppm，V2O5800-1000ppm，TiO21000-2000ppm，SnO21000-2000ppm，Co2O3500-1000ppm作为辅料，并将辅料与预烧粉料一起放入篮式砂磨机中，砂磨介质为水，砂磨时间120min，砂磨50min后加入0.1％的PVA溶剂和0.1％的消泡剂；
4)造粒：砂磨后的料浆进行喷雾造粒，造粒进口温度400℃，出口温度130℃，颗粒形貌呈规则的球形，中心内部无气孔，粒径大小均匀，成型性能较好；
5)颗粒定型：喷雾造粒后的颗粒压制成外径25mm，内径15mm ，高度10mm的环状毛坯，毛坯密度2.6±0.1g/cm3；
6)烧结：压制的毛坯在气氛保护钟罩炉中进行烧结，具体烧结过程为：以1-3.5℃/min的速度升温到600℃，在600℃保温0.3-2h，使毛坯中的有机物充分燃烧、挥发，然后以0.5-1℃/min升温速度升温到800℃，关闭炉门，向炉膛内充入氮气，将氧分压降低至5-10％，再将升温速度提高至4-6℃/min，升温到1300-1340℃，升温段氧分压保持在5-10％，保温过程氧分压在1-10％，保温时间4-8h，最后在平衡气氛中以3-6℃/min速度冷却到室温。
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