CN107324793A - 宽温内高μi优直流叠加特性锰锌铁氧体的制备方法 - Google Patents

宽温内高μi优直流叠加特性锰锌铁氧体的制备方法 Download PDF

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CN107324793A
CN107324793A CN201710494854.3A CN201710494854A CN107324793A CN 107324793 A CN107324793 A CN 107324793A CN 201710494854 A CN201710494854 A CN 201710494854A CN 107324793 A CN107324793 A CN 107324793A
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刘�东
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Chongqing Zheng Feng Electronics Co Ltd
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Abstract

本发明涉及一种铁氧磁体的制备方法，具体涉及一种宽温内高μi优直流叠加特性锰锌铁氧体的制备方法；组分包括主料和辅料，主料包括53.0～55.0mol％的Fe2O3，31.0～32.0mol％的MnO，余量为ZnO,辅料包括SiO2、CaCO3、Nb2O5、ZrO2和Co3O4，采用本方案的宽温内高μi优直流叠加特性锰锌铁氧体的制备方法制备出的产品具备高的起始磁导率和较好的直流叠加特性的优点。

Description

宽温内高μi优直流叠加特性锰锌铁氧体的制备方法
技术领域
本发明涉及一种铁氧磁体的制备方法，具体涉及一种宽温内高μi优直流叠加特性锰锌铁氧体的制备方法。
背景技术
PoE(Power over Ethernet)技术由于其易安装、易管理、简便性、安全性、稳定性、可扩展性和利旧原则，在家庭应用、无线建网、安全防护、建筑物管理、零售、娱乐等领域，都具有巨大的应用前景，并推动了相关领域的发展。由于以太网线缆在传递数据的同时供应给设备电力，就需要其中的磁性元件具有耐直流偏置的特性，即要求磁性元件在施加一定直流电(通常是8mA，据IEEE802.3af)的情况下还能保持一定的电感量。
现有技术中通常使用的材料有两种，一种是TDK的H5B2材料，常温时饱和磁通密度为420mT，常起始磁导率为7500±25％；0～130℃的起始磁导率均在6000以上，居里温度Tc为130℃，这种材料H5B2的缺点是直流叠加特性差和居里温度较低，在使用时，对于13A/m的直流叠加要求常常满足不了，对于26A/m的直流叠加要求更是满足不了。
第二种是JFE的MAS05，常温时饱和磁通密度为480mT，起始磁导率为4200±25％；-20～150℃的起始磁导率均在4000以上，居里温度为180℃。这种材料MAS05的缺点是磁导率较低，常温时磁导率仅为4200±25％，在使用时，直流叠加特性优良，但是AL系数较低，满足不了设计要求。
发明内容
本发明意在提供一种有高磁导率的同时具有优良直流叠加特性的锰锌铁氧体的宽温内高μi优直流叠加特性锰锌铁氧体的制备方法，解决了常规的高磁导率锰锌铁氧体直流叠加特性差和一般的直流叠加材料磁导率低的缺点。
本方案中的宽温内高μi优直流叠加特性锰锌铁氧体的制备方法，其组分包括主料和辅料，主料包括53.0～55.0mol％的Fe2O3，31.0～32.0mol％的MnO，余量为ZnO,辅料包括50～150ppm SiO2、100～500ppm CaCO3、60～120ppm Nb2O5、100～250ppm ZrO2和500～1000ppm Co3O4，制备方法包括如下步骤，
(1)、将主料按配比配料后，采用湿法配合得到主料浆，湿法配合的混合时间为100～150分钟，得到主料浆；
(2)、将主料浆于烘箱内120℃干燥后过筛，然后置于高温炉中进行预烧，得到预烧料，预烧温度为850～930℃，预烧时间为150～180分钟；
(3)、将辅料按照一定比例添加到预烧料中后，进行湿法粉碎，得到粉碎料，湿法粉碎的时间为150～200分钟，粉碎料的粒径为1.2～1.6μm；
(4)、向烘干过筛后的粉碎料中添加相当于粉料干重1.2％的聚乙烯醇，采用手工造粒，过60～120目筛，烘干，得到颗粒料；
(5)、用机械式压机将颗粒料压制成生坯，生坯密度为3.2g/cm3左右；
(6)、将生坯置于气氛钟罩炉中烧结，升温速率为3～5℃/分钟，保温段温度控制在1400～1430℃，保温段氧含量控制在12～15％，保温10～12小时，降温速率控制在2～5℃/分钟。
本发明的优点是：本发明制备出的铁氧体在25℃时起始磁导率在8000左右，在0～150℃范围内起始磁导率都大于7000，在叠加磁场为13A/m(T3.50-1.60-1.60,12Ts加偏置电流8mA)时，在25℃的有效磁导率为5000左右，在叠加26A/m，25℃时的有效磁导率为3800左右。在0～85℃范围内均有大于5000的有效磁导率；在叠加磁场为26A/m(T3.05-1.78-2.06,26Ts加偏置电流8mA)时，25℃的有效磁导率为3800左右，在-40～70℃范围内均有大于2000的有效磁导率。图1为本发明制备铁氧体在不同叠加磁场下磁导率随温度的变化曲线。
进一步，步骤(1)中，湿法配合的混合时间为120分钟。
进一步，步骤(2)中，预烧温度为890℃，预烧时间为160分钟。
进一步，步骤(3)中，湿法粉碎的时间为180分钟。
进一步，步骤(4)中，选用的筛为80目。
进一步，步骤(6)中，升温速率为4℃/分钟，保温段温度控制在1420℃，保温段氧含量控制在13％，保温11小时，降温速率控制在4℃/分钟。
附图说明
图1为本发明方法制备出宽温内高μi优直流叠加特性锰锌铁氧体在不同叠加磁场下磁导率随温度的变化曲线。
具体实施方式
实施例1
本发明提供一种宽温内高μi优直流叠加特性锰锌铁氧体的制备方法，组分包括主料和辅料，主料包括53.0mol％的Fe2O3，31.0mol％的MnO，余量为ZnO,辅料包括50ppm SiO2、500ppm CaCO3、60ppm Nb2O5、100ppm ZrO2和500ppm Co3O4，制备方法包括如下步骤，
(1)、将主料按配比配料后，采用湿法配合得到主料浆，湿法配合的混合时间为100分钟，得到主料浆；
(2)、将主料浆于烘箱内120℃干燥后过筛，然后置于高温炉中进行预烧，得到预烧料，预烧温度为850℃，预烧时间为150分钟；
(3)、将辅料按照上述比例添加到预烧料中后，进行湿法粉碎，得到粉碎料，湿法粉碎的时间为150分钟，粉碎料的粒径1.2μm；
(4)、向烘干过筛后的粉碎料中添加相当于粉料干重1.2％的聚乙烯醇，采用手工造粒，过60目筛，烘干，得到颗粒料；
(5)、用机械式压机将颗粒料压制成生坯，生坯密度为3.2g/cm3左右；
(6)、将生坯置于气氛钟罩炉中烧结，升温速率为℃/分钟，保温段温度控制在1400℃，保温段氧含量控制在12％，保温12小时，降温速率控制在2℃/分钟。
实施例2
本发明提供一种宽温内高μi优直流叠加特性锰锌铁氧体的制备方法，其组分包括主料和辅料，主料包括54.0mol％的Fe2O3，31.5mol％的MnO，余量为ZnO,辅料包括120ppmSiO2、200ppm CaCO3、100ppm Nb2O5、150ppm ZrO2和800ppm Co3O4，制备方法包括如下步骤，
(1)、将主料按配比配料后，采用湿法配合得到主料浆，湿法配合的混合时间为120分钟，得到主料浆；
(2)、将主料浆于烘箱内120℃干燥后过筛，然后置于高温炉中进行预烧，得到预烧料，预烧温度为890℃，预烧时间为160分钟；
(3)、将辅料按照上述比例添加到预烧料中后，进行湿法粉碎，得到粉碎料，湿法粉碎的时间为180分钟，粉碎料的粒径为1.4μm；
(4)、向烘干过筛后的粉碎料中添加相当于粉料干重1.2％的聚乙烯醇，采用手工造粒，过80目筛，烘干，得到颗粒料；
(5)、用机械式压机将颗粒料压制成生坯，生坯密度为3.2g/cm3左右；
(6)、将生坯置于气氛钟罩炉中烧结，升温速率为4℃/分钟，保温段温度控制在1420℃，保温段氧含量控制在13％，保温11小时，降温速率控制在4℃/分钟。
实施例3
本发明提供一种宽温内高μi优直流叠加特性锰锌铁氧体的制备方法，其组分包括主料和辅料，主料包括55.0mol％的Fe2O3，32.0mol％的MnO，余量为ZnO,辅料包括150ppmSiO2、500ppm CaCO3、120ppm Nb2O5、250ppm ZrO2和1000ppm Co3O4，制备方法包括如下步骤，
(1)、将主料按配比配料后，采用湿法配合得到主料浆，湿法配合的混合时间为150分钟，得到主料浆；
(2)、将主料浆于烘箱内120℃干燥后过筛，然后置于高温炉中进行预烧，得到预烧料，预烧温度为930℃，预烧时间为180分钟；
(3)、将辅料按照上述比例添加到预烧料中后，进行湿法粉碎，得到粉碎料，湿法粉碎的时间为200分钟，粉碎料的粒径为1.6μm；
(4)、向烘干过筛后的粉碎料中添加相当于粉料干重1.2％的聚乙烯醇，采用手工造粒，过120目筛，烘干，得到颗粒料；
(5)、用机械式压机将颗粒料压制成生坯，生坯密度为3.2g/cm3左右；
(6)、将生坯置于气氛钟罩炉中烧结，升温速率为5℃/分钟，保温段温度控制在1430℃，保温段氧含量控制在15％，保温10小时，降温速率控制在5℃/分钟。
以上所述的仅是本发明的实施例，方案中公知的具体结构及特性等常识在此未作过多描述。应当指出，对于本领域的技术人员来说，在不脱离本发明结构的前提下，还可以作出若干变形和改进，这些也应该视为本发明的保护范围，这些都不会影响本发明实施的效果和专利的实用性。

Claims (6)

1.宽温内高μi优直流叠加特性锰锌铁氧体的制备方法，其特征在于：其组分包括主料和辅料，主料包括53.0～55.0mol％的Fe2O3，31.0～32.0mol％的MnO，余量为ZnO,辅料包括50～150ppm SiO2、100～500ppm CaCO3、60～120ppm Nb2O5、100～250ppm ZrO2和500～1000ppm Co3O4，制备方法包括如下步骤，
(1)、将主料按配比配料后，采用湿法配合得到主料浆，湿法配合的混合时间为100～150分钟，得到主料浆；
(2)、将主料浆于烘箱内120℃干燥后过筛，然后置于高温炉中进行预烧，得到预烧料，预烧温度为850～930℃，预烧时间为150～180分钟；
(3)、将辅料按照一定比例添加到预烧料中后，进行湿法粉碎，得到粉碎料，湿法粉碎的时间为150～200分钟，粉碎料的粒径为1.2～1.6μm；
(4)、向烘干过筛后的粉碎料中添加相当于粉料干重1.2％的聚乙烯醇，采用手工造粒，过60～120目筛，烘干，得到颗粒料；
(5)、用机械式压机将颗粒料压制成生坯，生坯密度为3.2g/cm3左右；
(6)、将生坯置于气氛钟罩炉中烧结，升温速率为3～5℃/分钟，保温段温度控制在1400～1430℃，保温段氧含量控制在12～15％，保温10～12小时，降温速率控制在2～5℃/分钟。
2.根据权利要求1所述的宽温内高μi优直流叠加特性锰锌铁氧体的制备方法，其特征在于：步骤(1)中，湿法配合的混合时间为120分钟。
3.根据权利要求1所述的宽温内高μi优直流叠加特性锰锌铁氧体的制备方法，其特征在于：步骤(2)中，预烧温度为890℃，预烧时间为160分钟。
4.根据权利要求2所述的宽温内高μi优直流叠加特性锰锌铁氧体的制备方法，其特征在于：步骤(3)中，湿法粉碎的时间为180分钟。
5.根据权利要求1所述的宽温内高μi优直流叠加特性锰锌铁氧体的制备方法，其特征在于：步骤(4)中，选用的筛为80目。
6.根据权利要求1所述的宽温内高μi优直流叠加特性锰锌铁氧体的制备方法，其特征在于：步骤(6)中，升温速率为4℃/分钟，保温段温度控制在1420℃，保温段氧含量控制在13％，保温11小时，降温速率控制在4℃/分钟。
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