CN105481359A - 一种高性能大功率软磁铁氧体磁芯材料的制备方法 - Google Patents

一种高性能大功率软磁铁氧体磁芯材料的制备方法 Download PDF

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CN105481359A
CN105481359A CN201510839838.4A CN201510839838A CN105481359A CN 105481359 A CN105481359 A CN 105481359A CN 201510839838 A CN201510839838 A CN 201510839838A CN 105481359 A CN105481359 A CN 105481359A
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王军松
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QUANJIAO JUNHONG SOFT MAGNETIC MATERIALS CO Ltd
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Abstract

本发明公开了一种高性能大功率软磁铁氧体磁芯材料的制备方法，该软磁铁氧体磁芯材料由Fe2O3、NiO、ZnO、CuO、Co2O3、Mn3O4、GeO2、Eu2O3、GaAs、CaB2O4、Mo2O3、PbO、Bi2O3、V2O3、LaFeO3、SrCO3等原料组成；本发明材料通过一次配料、一次球磨、一次烧结、二次配料、二次球磨、压制成型、二次烧结等步骤制成。本发明制得的高性能大功率软磁铁氧体磁芯材料综合性能优异，具有高磁导率、高饱和磁感应强度、高居里温度、高电阻率和低损耗因数等特点，完全满足软磁铁氧体磁芯材料在大功率应用状态下的性能要求。

Description

一种高性能大功率软磁铁氧体磁芯材料的制备方法
技术领域
本发明涉及一种高性能大功率软磁铁氧体磁芯材料的制备方法，属于磁性材料技术领域。
背景技术
随着科学技术的进步,软磁铁氧体材料作为一种重要的基础功能材料,广泛
用于通讯、传感、音像设备、滤波器、变压器等电子工业中,为软磁铁氧体的应
用打开了广阔的市场；同时,由于通讯、计算机网络等电子信息产业的快速发展,对大功率状态下应用的软磁铁氧体材料需求也越来越多，如跟踪接收机、电视接收机、质子同步加速器、程控交换机、雷达电源、高频焊机以及舰载、机载和车载电子装备和用于几兆赫工作频率的开关电源等，都需要高性能大功率软磁铁氧体材料，为适应大功率应用，要求此类铁氧体材料具有高磁导率、高饱和磁感应强度、高居里温度、高电阻率、低损耗等特性。因此开发一种高性能大功率软磁铁氧体磁芯材料有很强的实际意义。
发明内容
本发明的目的在于提供一种高性能大功率软磁铁氧体磁芯材料的制备方法。
为实现上述目的，本发明采用的技术方案如下：
一种高性能大功率软磁铁氧体磁芯材料的制备方法，包括以下步骤：
（1）一次配料
以摩尔份计称取以下原料进行配料：50.2-54.6molFe2O3、17.3-20.7molNiO、28.4-31.2molZnO、1.6-3.8molCuO、0.8-1.6molCo2O3、12.5-16.1molMn3O4、0.3-0.8molGeO2、0.2-0.4molEu2O3、0.16-0.33molGaAs、0.08-0.19molCaB2O4；
（2）一次球磨
将步骤（1）称取得到的原料混合均匀，加入相当于混合粉末1-3wt%的十八胺聚氧乙烯醚、0.5-1.5wt%的十聚甘油单硬脂酸酯和0.4-0.8wt%的硫代硫酸钠，7000-8000rpm高速球磨15-20min，烘干，粉碎，过200-400目筛；
（3）一次烧结
将步骤（2）制得的粉料在70%CO2+20%H2+10%CO气氛下升温至890-930℃，保温4-5h，再在75%N2+25%Ar气氛下降温至610-660℃，保温2-3h，再在60%H2+40%CO气氛下升温至900-950℃，保温5-6h，再在50%Ar+50%CO2气氛下降温至590-630℃，保温2-3h，得预烧料；
（4）二次配料
称取相当于预烧料2.7-4.1wt%的Mo2O3、1.8-3.4wt%的PbO、0.7-1.3wt%的Bi2O3、0.5-1.0wt%的V2O3、0.1-0.4wt%的LaFeO3、0.05-0.15wt%的SrCO3；
（5）二次球磨
将步骤（4）称取得到的原料与步骤（3）制得的预烧料混合均匀，然后加水搅拌制成质量浓度为50-55%的悬浮液，然后加入相当于悬浮液0.5-1wt%的十二烷基苯磺酸钠、0.4-0.8wt%的壬基酚聚氧乙烯醚磷酸酯、0.3-0.5wt%的鲸蜡硬脂基葡糖苷，5000-6000rpm高速球磨20-35min，然后喷雾干燥成颗粒状粉体；
（6）压制成型
将步骤（5）得到的粉料加入到成型模具中，加入相当于粉料7-11wt%的25%聚乙烯亚胺水溶液，搅拌均匀，在1.5-2.0GPa的压力成型；
（7）二次烧结
将成型的磁芯毛坯进行二次烧结处理：首先在85%N2+15%CO2气氛下升温至780-820℃，保温2-4h,再降温至430-470℃，保温1-2h；然后在80%Ar+10%H2+10%CO气氛下升温至710-750℃，保温2-3h，再升温至1180-1260℃,保温4-6h；再在70%N2+20%CO2+10%O2气氛下降温至860-920℃，保温3-4h，再升温至1220-1280℃，保温5-7h，最后在60%Ar+40%CO2气氛下降温至680-730℃，保温2-3h；之后快速冷却至常温即可。
本发明的有益效果：
本发明制得的高性能大功率软磁铁氧体磁芯材料综合性能优异，具有高磁导率、高饱和磁感应强度、高居里温度、高电阻率和低损耗因数等特点，完全满足软磁铁氧体磁芯材料在大功率应用状态下的性能要求。
具体实施方式
一种高性能大功率软磁铁氧体磁芯材料的制备方法，包括以下步骤：
（1）一次配料
以摩尔份计称取以下原料进行配料：52.8molFe2O3、19.3molNiO、28.6molZnO、3.3molCuO、1.2molCo2O3、15.3molMn3O4、0.45molGeO2、0.34molEu2O3、0.27molGaAs、0.11molCaB2O4；
（2）一次球磨
将步骤（1）称取得到的原料混合均匀，加入相当于混合粉末2wt%的十八胺聚氧乙烯醚、1wt%的十聚甘油单硬脂酸酯和0.6wt%的硫代硫酸钠，7500rpm高速球磨18min，烘干，粉碎，过300目筛；
（3）一次烧结
将步骤（2）制得的粉料在70%CO2+20%H2+10%CO气氛下升温至910℃，保温4h，再在75%N2+25%Ar气氛下降温至640℃，保温2.5h，再在60%H2+40%CO气氛下升温至930℃，保温6h，再在50%Ar+50%CO2气氛下降温至610℃，保温2.5h，得预烧料；
（4）二次配料
称取相当于预烧料3.4wt%的Mo2O3、2.7wt%的PbO、0.9wt%的Bi2O3、0.7wt%的V2O3、0.25wt%的LaFeO3、0.072wt%的SrCO3；
（5）二次球磨
将步骤（4）称取得到的原料与步骤（3）制得的预烧料混合均匀，然后加水搅拌制成质量浓度为52%的悬浮液，然后加入相当于悬浮液0.8wt%的十二烷基苯磺酸钠、0.6wt%的壬基酚聚氧乙烯醚磷酸酯、0.4wt%的鲸蜡硬脂基葡糖苷，5500rpm高速球磨25min，然后喷雾干燥成颗粒状粉体；
（6）压制成型
将步骤（5）得到的粉料加入到成型模具中，加入相当于粉料10wt%的25%聚乙烯亚胺水溶液，搅拌均匀，在1.7GPa的压力成型；
（7）二次烧结
将成型的磁芯毛坯进行二次烧结处理：首先在85%N2+15%CO2气氛下升温至805℃，保温3h,再降温至450℃，保温1.5h；然后在80%Ar+10%H2+10%CO气氛下升温至730℃，保温2.5h，再升温至1240℃,保温5h；再在70%N2+20%CO2+10%O2气氛下降温至890℃，保温3h，再升温至1260℃，保温6h，最后在60%Ar+40%CO2气氛下降温至710℃，保温2.5h；之后快速冷却至常温即可。
上述实施例制得的软磁铁氧体磁芯材料的性能检测结果如下表所示
检测项目 检测结果
1 起始磁导率μi 16000
2 最大磁导率μmax 25400
3 饱和磁通密度Bs（mT） 420
4 矫顽力Hc（A/m） 2.9
5 居里温度Tc（℃） 240
6 电阻率（Ω·m） 1.8×105
7 损耗因数tanδ/μi，100kHz 1.5×10－6

Claims (1)

1.一种高性能大功率软磁铁氧体磁芯材料的制备方法，其特征在于包括以下步骤：
（1）一次配料
以摩尔份计称取以下原料进行配料：50.2-54.6molFe2O3、17.3-20.7molNiO、28.4-31.2molZnO、1.6-3.8molCuO、0.8-1.6molCo2O3、12.5-16.1molMn3O4、0.3-0.8molGeO2、0.2-0.4molEu2O3、0.16-0.33molGaAs、0.08-0.19molCaB2O4；
（2）一次球磨
将步骤（1）称取得到的原料混合均匀，加入相当于混合粉末1-3wt%的十八胺聚氧乙烯醚、0.5-1.5wt%的十聚甘油单硬脂酸酯和0.4-0.8wt%的硫代硫酸钠，7000-8000rpm高速球磨15-20min，烘干，粉碎，过200-400目筛；
一次烧结
将步骤（2）制得的粉料在70%CO2+20%H2+10%CO气氛下升温至890-930℃，保温4-5h，再在75%N2+25%Ar气氛下降温至610-660℃，保温2-3h，再在60%H2+40%CO气氛下升温至900-950℃，保温5-6h，再在50%Ar+50%CO2气氛下降温至590-630℃，保温2-3h，得预烧料；
二次配料
称取相当于预烧料2.7-4.1wt%的Mo2O3、1.8-3.4wt%的PbO、0.7-1.3wt%的Bi2O3、0.5-1.0wt%的V2O3、0.1-0.4wt%的LaFeO3、0.05-0.15wt%的SrCO3；
二次球磨
将步骤（4）称取得到的原料与步骤（3）制得的预烧料混合均匀，然后加水搅拌制成质量浓度为50-55%的悬浮液，然后加入相当于悬浮液0.5-1wt%的十二烷基苯磺酸钠、0.4-0.8wt%的壬基酚聚氧乙烯醚磷酸酯、0.3-0.5wt%的鲸蜡硬脂基葡糖苷，5000-6000rpm高速球磨20-35min，然后喷雾干燥成颗粒状粉体；
压制成型
将步骤（5）得到的粉料加入到成型模具中，加入相当于粉料7-11wt%的25%聚乙烯亚胺水溶液，搅拌均匀，在1.5-2.0GPa的压力成型；
（7）二次烧结
将成型的磁芯毛坯进行二次烧结处理：首先在85%N2+15%CO2气氛下升温至780-820℃，保温2-4h,再降温至430-470℃，保温1-2h；然后在80%Ar+10%H2+10%CO气氛下升温至710-750℃，保温2-3h，再升温至1180-1260℃,保温4-6h；再在70%N2+20%CO2+10%O2气氛下降温至860-920℃，保温3-4h，再升温至1220-1280℃，保温5-7h，最后在60%Ar+40%CO2气氛下降温至680-730℃，保温2-3h；之后快速冷却至常温即可。
CN201510839838.4A 2015-11-27 2015-11-27 一种高性能大功率软磁铁氧体磁芯材料的制备方法 Pending CN105481359A (zh)

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