CN107417269A - 二峰温度小于‑20℃的宽温高磁导率锰锌铁氧体的制备方法 - Google Patents
二峰温度小于‑20℃的宽温高磁导率锰锌铁氧体的制备方法 Download PDFInfo
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Abstract
本发明涉及一种铁氧磁体的制备方法,具体涉及一种二峰温度小于‑20℃的宽温高磁导率锰锌铁氧体的制备方法;其组分包括主料和辅料,主料包括Fe2O3,MnO和ZnO,辅料包括CaCO3、Nb2O5、Bi2O3和MoO3,制备方法包括,(1)、将主料按配比配料后,采用湿法配合得到主料浆;(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;(3)、将辅助成份按照比例添加到预烧料中后,进行湿法粉碎,得到粉碎料;(4)、向烘干过筛后的粉碎料中添加相当于粉碎料干重1.2%的聚乙烯醇,采用手工造粒,过筛,烘干,得到颗粒料;(5)、将颗粒料压制成型后置于气氛钟罩炉中烧结;采用本方案一种二峰温度小于‑20℃的宽温高磁导率锰锌铁氧体制备的材料具有居里温度高、适用性强的优点。
Description
技术领域
本发明涉及一种铁氧磁体的制备方法,具体涉及一种二峰温度小于-20℃的宽温高磁导率锰锌铁氧体的制备方法。
背景技术
随着ADSL、Wireless Communication等数字通讯技术的快速发展,通讯设备越来越广泛地用于户外。而且,随着人类活动范围的扩大,对通讯设施的温度稳定性要求也越来越高。现有技术中常用的材料一种是TDK的H5C4材料,其二峰温度在-10℃左右,居里温度Tc为110℃,25℃的磁导率为12000±25%,-20℃磁导率9000左右,但是在-40℃时的磁导率较低,-60℃未给出。这种材料的缺点是1、适用温度范围较窄,对于-20℃以下的低温电磁特性要求,常常满足不了,只能增加绕线圈数,增加设计和制造成本;2、居里温度较低,为110℃。
另一种是Ceramic Magnetics,Inc.的TC6000,二峰温度在-25℃,居里温度104℃。25℃的磁导率为7500,喷涂了派瑞林(parylene)后,在-40~85℃范围内最低磁导率为6000,-60℃未给出。这种材料的缺点(1)适用温度范围较窄,在-40℃~104℃范围内磁导率在7000以上;(2)居里温度较低,仅有104℃,对于-40~105℃、-40~120℃诸如此类的超宽温要求,往往要求居里温度在120℃以上,甚至130℃左右,该材料达不到设计要求。
发明内容
本发明意在提供一种-60~120℃范围内均有高于6000的起始磁导率,非常适于ISDN脉冲变压器、无线通讯基站用变压器等要求在较宽温度范围内保持电磁特性的设备的一种二峰温度小于-20℃的宽温高磁导率锰锌铁氧体的制备方法。
本方案中的一种二峰温度小于-20℃的宽温高磁导率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Fe2O3,22.0~24.0mol%的MnO,余量为ZnO,辅料包括CaCO3、Nb2O5、Bi2O3和MoO3,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;
(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)、将辅助成份按照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碎料干重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)、将颗粒料压制成型后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:本发明涉及的锰锌铁氧体材料由于在-60℃仍有6000以上的磁导率,所以在设计和制造阶段,均可节省成本。而且本发明涉及的锰锌铁氧体材料的居里温度在120℃以上,实测值在125℃到130℃之间,因此对于要求居里温度120℃的器件,可以很好地满足设计要求。图1显示本发明方案产品的磁导率(μi)随温度(T)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(5)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为本发明二峰温度小于-20℃的宽温高磁导率锰锌铁氧体的制备方法产品的磁导率随温度变化曲线。
具体实施方式
实施例1
本发明提供一种二峰温度小于-20℃的宽温高磁导率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Fe2O3,22.0mol%的MnO,余量为ZnO,辅料包括200ppmCaCO3、50ppmNb2O5、300ppmBi2O3和300ppmMoO3,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;
(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)、将辅助成份按照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,粉碎料的粒径为1.2μm;
(4)、向烘干过筛后的粉碎料中添加相当于粉碎料干重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)、将颗粒料压制成型后置于气氛钟罩炉中烧结,升温速率为3℃/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
本发明提供一种二峰温度小于-20℃的宽温高磁导率锰锌铁氧体的制备方法,组分包括主料和辅料,主料包括55.0mol%的Fe2O3,24.0mol%的MnO,余量为ZnO,辅料包括500ppmCaCO3、100ppmNb2O5、500ppmBi2O3和500ppmMoO3,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;
(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)、将辅助成份按照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碎料干重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)、将颗粒料压制成型后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。
实施例3
本发明提供一种二峰温度小于20℃的宽温高磁导率锰锌铁氧体的制备方法,组分包括主料和辅料,主料包括54.0mol%的Fe2O3,23.0mol%的MnO,余量为ZnO,辅料包括450ppmCaCO3、80ppmNb2O5、400ppmBi2O3和400ppmMoO3,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;
(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)、将辅助成份按照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碎料干重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)、将颗粒料压制成型后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。
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)
1.二峰温度小于-20℃的宽温高磁导率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Fe2O3,22.0~24.0mol%的MnO,余量为ZnO,辅料包括200~500ppmCaCO3、50~100ppmNb2O5、300~500ppmBi2O3和300~500ppmMoO3,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;
(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)、将辅助成份按照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碎料干重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)、将颗粒料压制成型后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所述的二峰温度小于-20℃的宽温高磁导率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所述的二峰温度小于-20℃的宽温高磁导率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所述的二峰温度小于-20℃的宽温高磁导率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所述的二峰温度小于-20℃的宽温高磁导率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所述的二峰温度小于-20℃的宽温高磁导率锰锌铁氧体的制备方法,其特征在于:步骤(5)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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