CN112573913A - 一种宽带高导磁率、高居里温度Mn-Zn铁氧体材料及其制备方法与应用 - Google Patents

一种宽带高导磁率、高居里温度Mn-Zn铁氧体材料及其制备方法与应用 Download PDF

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CN112573913A
CN112573913A CN202011471276.XA CN202011471276A CN112573913A CN 112573913 A CN112573913 A CN 112573913A CN 202011471276 A CN202011471276 A CN 202011471276A CN 112573913 A CN112573913 A CN 112573913A
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钟政霖
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ACME ELECTRONICS (GUANGZHOU) CO LTD
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Abstract

本发明属于磁性材料技术领域，具体公开了一种宽带高导磁率、高居里温度Mn‑Zn铁氧体材料及其制备方法与应用。所述铁氧体材料，包括主成分和辅助成分；所述主成分包括60～74wt％氧化铁、11～29wt％氧化锌、其余为氧化锰；所述辅助成分相对于主成分的含量包括0～500ppm碳酸钙、0～200ppm氧化硅、0～500ppm氧化铋、0～800ppm氧化钼和0～200ppm氧化铌，所述辅助成分的含量均不为0。本发明制得的高导磁率的锰锌铁氧体，相对于现有技术，具有较高的居里温度，较目前业界的水准会高出20℃，使用温度范围提升至145℃，并且频率范围提升至160KHz，可得到更大实际使用范畴。

Description

一种宽带高导磁率、高居里温度Mn-Zn铁氧体材料及其制备方 法与应用
技术领域
本发明属于磁性材料技术领域，特别涉及一种宽带高导磁率、高居里温度Mn-Zn铁氧体材料及其制备方法与应用。
背景技术
随着通信、计算器、网络等电子信息产业的高速发展,以及电子组件小型化与轻量化的趋势演进,高磁导率锰锌铁氧体能广泛使用于变压器铁芯、噪音过滤器、局部网隔离变压器和数字网络变压器铁芯等。由于应用朝着小型化发展,因此对锰锌铁氧体的初始磁导率提出了更为严苛之需求，除了初始磁导率要高外，市场还要求其具有良好的频率特性及高居里温度。在锰锌铁氧体中，高导磁率材料主要技术难点在于提升居里温度点和频宽，目前整个行业中，初导磁率在10000及以上铁氧体材料居里温度点在120℃-130℃，频宽为100KHz，但在100KHz后的导磁率会出现明显下降。在目前电子信息时代，外界环境的各种电子组件干扰日益严重，因而更要求前述的应用器件所需的材料具有较强的抗电磁干扰功能，从而要求锰锌铁氧体具有宽带高导磁率与高居里温度的特性。
发明内容
为了克服上述现有技术的缺点与不足，本发明的首要目的在于提供一种宽带高导磁率、高居里温度Mn-Zn铁氧体材料。
本发明另一目的在于提供一种宽带高导磁率、高居里温度Mn-Zn铁氧体材料的制备方法。
本发明再一目的在于提供一种宽带高导磁率、高居里温度Mn-Zn铁氧体材料在制备电子组件中的应用。
本发明的目的通过下述方案实现：
一种宽带高导磁率、高居里温度Mn-Zn铁氧体材料，包括主成分和辅助成分；
所述主成分包括60～74wt％氧化铁、11～29wt％氧化锌、其余为氧化锰；所述辅助成分相对于主成分的含量包括0～500ppm碳酸钙、0～200ppm氧化硅(SiO2)、0～500ppm氧化铋(Bi2O3)、0～800ppm氧化钼(MoO3)和0～200ppm氧化铌(Nb2O5)，所述辅助成分的含量均不为0。
优选地，所述辅助成分相对于主成分的含量包括240～270ppm碳酸钙、20～30ppm氧化硅、300～400ppm氧化铋、0～800ppm氧化钼和0～200ppm氧化铌，所述辅助成分的含量均不为0。
一种制备上述宽带高导磁率、高居里温度Mn-Zn铁氧体材料的方法，包括以下步骤：
(1)按照配方依比例混合，然后煅烧；
(2)煅烧完成后添加辅助成分、水、PVA，制备成铁浆；
(3)将所得铁浆以湿式球磨进行粉末细化；
(4)将所得球磨粉末细化浆料进行喷雾造粒；
(5)将所得粉末以固定生胚密度的方式进行压实成型，得到生胚；
(6)将所得生胚进行烧结；依照烧结过程分为升温段、恒温段、降温段，制得最终产物。
步骤(1)所述煅烧的温度为900～1000℃，优选为920～930℃；煅烧的时间为1～4h，优选为2h。
步骤(2)所述水的用量相对于主成分的重量百分比为40～50wt％；所述PVA的用量相对于主成分的重量百分比为0.8～1.2wt％。
步骤(3)所述湿式球磨的球磨时间为1～2小时，目标粒径为1.0～2.0μm；依照粉末粒径大小调整研磨时间。所述球磨介质为钢珠，大小优选为3/8英寸。
步骤(4)所述喷雾造粒温度条件，进口温度为150～200℃，出口温度为80～100℃条件下进行造粒。
步骤(5)所述固定生胚密度具体为3.4±0.2g/cm3。
步骤(6)所述烧结的条件，升温段为从室温升至1300～1400℃，氧分压为19～21％；恒温段维持1300～1400℃在氧分压19～21％中烧结2～10h；降温段从1300～1400℃降至950～1150℃在平衡氧分压中进行0.5～2h，从950～1150℃降至室温在氧分压0.0005～0.002％中进行2～10h，所述烧结的气氛优选为空气和氮气。
优选地，步骤(6)所述烧结的条件，升温段为从室温升至1360℃，氧分压为20.6％；恒温段维持1360℃在20.6％氧分压中烧结6h；降温段从1360℃降至1000℃在平衡氧分压中进行1h，从1000℃降至室温在氧分压0.001％中进行5h。
所述宽带高导磁率、高居里温度Mn-Zn铁氧体材料在制备电子组件中的应用。
本发明相对于现有技术，具有如下的优点及有益效果：
本发明制得的高导磁率的锰锌铁氧体，相对于现有技术，具有较高的居里温度，较目前业界的水准会高出20℃，使用温度范围提升至145℃，可得到更大实际使用范畴。在高导磁率的技术限制中，可应用的频率范围也是非常重要的参数，而目前行业中在导磁率为10000Hz的锰锌铁氧体中，频率范围会在1KHz-100KHz，现将频率范围提升至160KHz，对于锰锌铁氧体的终端设计会产生更有利。
附图说明
图1为实施例3与对比例1的居里温度的对比图示.
图2为本发明所得实际产品图。
具体实施方式
下面结合实施例和附图对本发明作进一步详细的描述，但本发明的实施方式不限于此。
实施例中所用试剂如无特殊说明均可从市场常规购得。PVA的聚合度为400～1800.
实施例中宽带高导磁率.高居里温度锰-锌铁氧体材料的制备方法如下：
(1)混合：将主成分依照Fe2O3、MnO2和ZnO的摩尔比进行干式混合；
(2)煅烧：混合结束投入煅烧炉以高温930±10度、持温2小时烧结；
(3)粉碎研磨与造粒：添加水、微量元素、PVA(聚乙烯醇),以相对于主成分的重量百分比的1.0wt％PVA与43wt％水制作成铁浆，以湿式球磨进行粉末细化，钢珠选择使用3/8英寸大小，依照粉末粒径大小调整研磨时间，目标粒径大小约1.0～2.0μm，研磨时间坐落于1～2小时之间。添加微量含有0～500ppm的按CaCO3计算的碳酸钙，0～200ppm的按SiO2计算的氧化硅,0～500ppm的按Bi2O3计算的氧化铋，0～800ppm的按MoO3计算的氧化钼,0～200ppm的按Nb2O5计算的氧化铌。
(4)造粒：将研磨完成之浆料进行喷雾造粒。
(5)成型：使用成型机以固定生胚密度的方式进行成型，测试磁环尺寸规格为T25*15*10，目标密度为3.4±0.2g/cm3
(6)烧结：烧结制程采用烧结炉进行烧结，升温段为从室温升至1360℃，氧分压为20.6％；恒温段维持1360℃在20.6％氧分压中烧结6h；降温段从1360℃降至1000℃在平衡氧分压中进行1h；从1000℃降至室温在氧分压0.001％中进行，配合气氛(空气和氮气)烧结成品。
实施例1
一种宽带高导磁率.高居里温度锰-锌铁氧体材料,所述的主原料的组分为含有69.0wt％的按Fe2O3计算的氧化铁,14.2wt％的按ZnO计算的氧化锌,其余为Mn3O4；所述的辅助原料的组分为含有268ppm的按CaCO3计算的碳酸钙，27ppm的按SiO2计算的氧化硅，304ppm的按Bi2O3计算的氧化铋，333ppm的按MoO3计算的氧化钼，6ppm的按Nb2O5计算的氧化铌。
实施例2
一种宽带高导磁率.高居礼温度锰-锌铁氧体材料，所述的主原料的组分为含有69.0wt％的按Fe2O3计算的氧化铁，14.1wt％的按ZnO计算的氧化锌，其余为Mn3O4；所述的辅助原料的组分为含有264ppm的按CaCO3计算的碳酸钙，28ppm的按SiO2计算的氧化硅，312ppm的按Bi2O3计算的氧化铋，344ppm的按MoO3计算的氧化钼，8ppm的按Nb2O5计算的氧化铌。
实施例3
一种宽带高导磁率.高居礼温度锰-锌铁氧体材料,所述的主原料的组分为含有69.0wt％的按Fe2O3计算的氧化铁,14.1wt％的按ZnO计算的氧化锌,其余为Mn3O4；所述的辅助原料的组分为含有264ppm的按CaCO3计算的碳酸钙,32ppm的按SiO2计算的氧化硅,396ppm的按Bi2O3计算的氧化铋,404ppm的按MoO3计算的氧化钼,32ppm的按Nb2O5计算的氧化铌。
实施例4
一种宽带高导磁率.高居礼温度锰-锌铁氧体材料，所述的主原料的组分为含有69.0wt％的按Fe2O3计算的氧化铁，13.9wt％的按ZnO计算的氧化锌，其余为Mn3O4；所述的辅助原料的组分为含有260ppm的按CaCO3计算的碳酸钙,28ppm的按SiO2计算的氧化硅，320ppm的按Bi2O3计算的氧化铋，355ppm的按MoO3计算的氧化钼，10ppm的按Nb2O5计算的氧化铌。
由本发明的实施例1至4得到的宽带高导磁率.高居里温度锰-锌铁氧体材料经测试具有表1所示的技术效果。
表1实施例1-4和对比例1所得产物的性能测试结果
ui 居里温度
磁导率 10KHz 100KHz 160KHz 200KHz Tc
实施例1 10408 10905 10275 9480 143
实施例2 10533 11054 10437 9638 145
实施例3 11046 11730 11054 10191 145
实施例4 10583 11120 10516 9710 147
对比例1 10388 10780 9969 9088 130
注：对比例1为目前行业的性能
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。

Claims (10)

1.一种宽带高导磁率、高居里温度Mn-Zn铁氧体材料，其特征在于包括主成分和辅助成分；
所述主成分包括60～74wt％氧化铁、11～29wt％氧化锌、其余为氧化锰；所述辅助成分相对于主成分的含量包括0～500ppm碳酸钙、0～200ppm氧化硅、0～500ppm氧化铋、0～800ppm氧化钼和0～200ppm氧化铌，所述辅助成分的含量均不为0。
2.根据对比文件1所述的宽带高导磁率、高居里温度Mn-Zn铁氧体材料，其特征在于：
所述辅助成分相对于主成分的含量包括240～270ppm碳酸钙、20～30ppm氧化硅、300～400ppm氧化铋、0～800ppm氧化钼和0～200ppm氧化铌，所述辅助成分的含量均不为0。
3.一种制备权利要求1或2所述宽带高导磁率、高居里温度Mn-Zn铁氧体材料的方法，包括以下步骤：
(1)按照配方依比例混合，然后煅烧；
(2)煅烧完成后添加辅助成分、水、PVA，制备成铁浆；
(3)将所得铁浆以湿式球磨进行粉末细化；
(4)将所得球磨粉末细化浆料进行喷雾造粒；
(5)将所得粉末以固定生胚密度的方式进行压实成型，得到生胚；
(6)将所得生胚进行烧结；依照烧结过程分为升温段、恒温段、降温段，制得最终产物。
4.根据权利要求3所述的方法，其特征在于：步骤(1)所述煅烧的温度为900～1000℃，煅烧的时间为1～4h。
5.根据权利要求3所述的方法，其特征在于：步骤(2)所述水的用量相对于主成分的重量百分比为40～50wt％；所述PVA的用量相对于主成分的重量百分比为0.8～1.2wt％。
6.根据权利要求3所述的方法，其特征在于：步骤(3)所述湿式球磨的球磨时间为1～2小时，目标粒径为1.0～2.0μm；
步骤(4)所述喷雾造粒温度条件，进口温度为150～200℃，出口温度为80～100℃条件下进行造粒。
7.根据权利要求3所述的方法，其特征在于：步骤(5)所述固定生胚密度具体为3.4±0.2g/cm3。
8.根据权利要求3所述的方法，其特征在于：步骤(6)所述烧结的条件，升温段为从室温升至1300～1400℃，氧分压为19～21％；恒温段维持1300～1400℃在氧分压19～21％中烧结2～10h；降温段从1300～1400℃降至950～1150℃在平衡氧分压中进行0.5～2h，从950～1150℃降至室温在氧分压0.0005～0.002％中进行2～10h。
9.根据权利要求3所述的方法，其特征在于：步骤(6)所述烧结的条件，升温段为从室温升至1360℃，氧分压为20.6％；恒温段维持1360℃在20.6％氧分压中烧结6h；降温段从1360℃降至1000℃在平衡氧分压中进行1h，从1000℃降至室温在氧分压0.001％中进行5h。
10.根据权利要求1或2所述宽带高导磁率、高居里温度Mn-Zn铁氧体材料在制备电子组件中的应用。
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CN114773047A (zh) * 2022-04-25 2022-07-22 江门安磁电子有限公司 一种宽频高阻抗的锰锌铁氧体材料及其制备方法和应用
CN115295301A (zh) * 2022-10-08 2022-11-04 山东东泰方思电子有限公司 一种锰锌功率铁氧体磁芯材料制备方法
CN115448714A (zh) * 2022-10-12 2022-12-09 上海宝钢磁业有限公司 锰锌铁氧体材料及制备方法和应用

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CN114773047A (zh) * 2022-04-25 2022-07-22 江门安磁电子有限公司 一种宽频高阻抗的锰锌铁氧体材料及其制备方法和应用
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CN115295301A (zh) * 2022-10-08 2022-11-04 山东东泰方思电子有限公司 一种锰锌功率铁氧体磁芯材料制备方法
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