CN111138183B - 一种低损耗、高Bs的锰锌铁氧体材料及其制备方法 - Google Patents

一种低损耗、高Bs的锰锌铁氧体材料及其制备方法 Download PDF

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CN111138183B
CN111138183B CN201911415796.6A CN201911415796A CN111138183B CN 111138183 B CN111138183 B CN 111138183B CN 201911415796 A CN201911415796 A CN 201911415796A CN 111138183 B CN111138183 B CN 111138183B
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瞿德林
沈建元
王久如
王晓祥
李丛俊
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Zhongde Electronics Co ltd
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Abstract

本发明公开了一种低损耗、高Bs的锰锌铁氧体材料及其制备方法，所述锰锌铁氧体材料包括主成分Fe2O3、ZnO、Mn3O4和第一副成分Bi2O3，所述主成分中，Fe2O3含量为73.5‑74.1mol％、ZnO含量为12.2‑12.6mol％、Mn3O4含量为13.5‑13.9mol％；第一副成分Bi2O3以主成分为基础，其含量为0.4‑0.5wt％；所述Bi2O3为掺杂Mn2+的Bi2O3。本发明所述锰锌铁氧体材料的电性能可以达到低损耗、高Bs的要求，适合大批量的生产制作。

Description

一种低损耗、高Bs的锰锌铁氧体材料及其制备方法
技术领域
本发明涉及铁氧体材料技术领域，尤其涉及一种低损耗、高Bs的锰锌铁氧体材料。
背景技术
MnZn铁氧体磁芯运用越来越广泛，是各种通信设备、计算机、家用电器、汽车电子、电源装置、仪器仪表、航天工业等不可缺少的一种电子材料。
目前，业内通常采用提升锰锌铁氧体磁性材料中ZnO含量的方法，提升锰锌铁氧体磁性材料的磁导率。但是，在该锰锌铁氧体材料中，由于ZnO的含量较高，Fe2O3的含量相对较低，从而导致饱和磁通密度的降低；而且其功耗在25℃、80℃时也都在400kW/m3以上。
发明内容
本发明提出了一种低损耗、高Bs的锰锌铁氧体材料及其制备方法，所述锰锌铁氧体材料的电性能可以达到低损耗、高Bs的要求，适合大批量的生产制作。
本发明提出的一种低损耗、高Bs的锰锌铁氧体材料，包括主成分Fe2O3、ZnO、Mn3O4和第一副成分Bi2O3，所述主成分中，Fe2O3含量为73.5-74.1mol％、ZnO含量为12.2-12.6mol％、Mn3O4含量为13.5-13.9mol％；第一副成分Bi2O3以主成分为基础，其含量为0.4-0.5wt％；所述Bi2O3为掺杂Mn2+的Bi2O3。
优选地，还包括第二副成分CaCO3、Co2O3、TiO2、Nb2O5、ZrO2和/或V2O5，以主成分为基础，CaCO3含量为0.01-0.08wt％、Co2O3含量为0.1-0.2wt％、TiO2含量为0.05-0.08wt％、Nb2O5含量为0.02-0.05wt％、ZrO2含量为0.01-0.04wt％、V2O5含量为0.01-0.1wt％。
优选地，所述Bi2O3中Mn2+的掺杂量为0.1-2.8wt％。
优选地，所述Bi2O3采用如下方法制备得到：将硝酸铋溶于乙二醇中，加入锰盐混匀，再送入微波反应器中进行微波加热处理，冷却，过滤，洗涤，干燥，在580-630℃下焙烧1-2h，得到掺杂Mn2+的Bi2O3。
本发明还提出一种低损耗、高Bs的锰锌铁氧体材料的制备方法，包括如下步骤：
(1)按照配方比例，分别称取主料Fe2O3、ZnO和Mn3O4进行第一次湿法砂磨30min以上，喷雾干燥制成颗粒，进行预烧，预烧温度为850-880℃，得到预烧料；
(2)在预烧料中按照配方比例加入第一副成分Bi2O3和第二副成分，进行第二次湿法砂磨，直至颗粒的平均粒径为0.8-1.0μm，再加入10-15wt％总配料重量的聚乙烯醇溶液，喷雾干燥，制成粒径为50-200μm的颗粒；
(3)将上述颗粒加工成型后进行烧结，在1320-1380℃下烧结4-6h，烧结时控制氧含量为3-8％，得到成品，即为所述低损耗、高Bs的锰锌铁氧体材料。
优选地，所述聚乙烯醇溶液为浓度8-9wt％的聚乙烯醇溶液。
优选地，喷雾干燥时，喷雾塔进口温度320-360℃，出口温度90-110℃。
优选地，烧结时，以2-5℃\min的升温速率升温到1320-1380℃。
本发明所述的锰锌铁氧体磁性材料，通过提升原材料中Fe2O3的含量，降低原材料中ZnO的含量，合理设置Fe2O3、ZnO、Mn3O4的比例，提高饱和磁通密度；并且通过在原材料中加入掺杂Mn2+的Bi2O3，增加了磁芯的密度，降低了其功率损耗。
具体实施方式
实施例1
一种低损耗、高Bs的锰锌铁氧体材料，包括主成分Fe2O3、ZnO、Mn3O4和副成分Bi2O3、CaCO3、Co2O3、TiO2、Nb2O5、ZrO2和V2O5；
主成分：Fe2O3含量为73.8mol％、ZnO含量为12.4mol％、Mn3O4含量为13.8mol％；
副成分：Bi2O3含量为0.45wt％，CaCO3含量为0.04wt％、Co2O3含量为0.15wt％、TiO2含量为0.06wt％、Nb2O5含量为0.04wt％、ZrO2含量为0.03wt％、V2O5含量为0.05wt％；
所述Bi2O3为掺杂Mn2+的Bi2O3，其Mn2+的掺杂量为1.5wt％，采用如下方法制备得到：将硝酸铋溶于乙二醇中，加入氯化锰混匀，再送入微波反应器中进行微波加热处理，微波功率为600W，时间为15min，冷却，过滤，洗涤，干燥，在600℃下焙烧1.5h，得到掺杂Mn2+的Bi2O3；
上述低损耗、高Bs的锰锌铁氧体材料的制备方法包括：
(1)按照配方比例，分别称取主料Fe2O3、ZnO和Mn3O4进行第一次湿法砂磨50min，喷雾干燥制成颗粒，进行预烧，预烧温度为870℃，得到预烧料；
(2)在预烧料中按照配方比例加入第一副成分Bi2O3和第二副成分CaCO3、Co2O3、TiO2、Nb2O5、ZrO2、V2O5，进行第二次湿法砂磨，直至颗粒的平均粒径为0.9μm，再加入12wt％总配料重量浓度8wt％的聚乙烯醇溶液，喷雾干燥，制成粒径为100μm的颗粒；
(3)将上述颗粒加工成型后进行烧结，以3℃\min的升温速率升温到1350℃，在1350℃下烧结5h，烧结时控制氧含量为5％(体积分数)，得到成品，即为所述低损耗、高Bs的锰锌铁氧体材料。
实施例2
一种低损耗、高Bs的锰锌铁氧体材料，包括主成分Fe2O3、ZnO、Mn3O4和副成分Bi2O3、CaCO3、Co2O3、TiO2、Nb2O5、ZrO2和V2O5；
主成分：Fe2O3含量为73.9mol％、ZnO含量为12.6mol％、Mn3O4含量为13.5mol％；
副成分：Bi2O3含量为0.5wt％，CaCO3含量为0.01wt％、Co2O3含量为0.2wt％、TiO2含量为0.05wt％、Nb2O5含量为0.05wt％、ZrO2含量为0.01wt％、V2O5含量为0.1wt％；
所述Bi2O3为掺杂Mn2+的Bi2O3，其Mn2+的掺杂量为0.1wt％，采用如下方法制备得到：将硝酸铋溶于乙二醇中，加入氯化锰混匀，再送入微波反应器中进行微波加热处理，微波功率为650W，时间为10min，冷却，过滤，洗涤，干燥，在630℃下焙烧1h，得到掺杂Mn2+的Bi2O3；
上述低损耗、高Bs的锰锌铁氧体材料的制备方法包括：
(1)按照配方比例，分别称取主料Fe2O3、ZnO和Mn3O4进行第一次湿法砂磨30min，喷雾干燥制成颗粒，进行预烧，预烧温度为880℃，得到预烧料；
(2)在预烧料中按照配方比例加入第一副成分Bi2O3和第二副成分CaCO3、Co2O3、TiO2、Nb2O5、ZrO2、V2O5，进行第二次湿法砂磨，直至颗粒的平均粒径为0.8μm，再加入15wt％总配料重量浓度8wt％的聚乙烯醇溶液，喷雾干燥，制成粒径为200μm的颗粒；
(3)将上述颗粒加工成型后进行烧结，以2℃\min的升温速率升温到1380℃，在1380℃下烧结6h，烧结时控制氧含量为3％，得到成品，即为所述低损耗、高Bs的锰锌铁氧体材料。
实施例3
一种低损耗、高Bs的锰锌铁氧体材料，包括主成分Fe2O3、ZnO、Mn3O4和副成分Bi2O3、CaCO3、Co2O3、TiO2、Nb2O5、ZrO2和V2O5；
主成分：Fe2O3含量为74.1mol％、ZnO含量为12.2mol％、Mn3O4含量为13.7mol％；
副成分：Bi2O3含量为0.4wt％，CaCO3含量为0.08wt％、Co2O3含量为0.1wt％、TiO2含量为0.08wt％、Nb2O5含量为0.02wt％、ZrO2含量为0.04wt％、V2O5含量为0.01wt％；
所述Bi2O3为掺杂Mn2+的Bi2O3，其Mn2+的掺杂量为2.8wt％，采用如下方法制备得到：将硝酸铋溶于乙二醇中，加入氯化锰混匀，再送入微波反应器中进行微波加热处理，微波功率为550W，时间为20min，冷却，过滤，洗涤，干燥，在580℃下焙烧2h，得到掺杂Mn2+的Bi2O3；
上述低损耗、高Bs的锰锌铁氧体材料的制备方法包括：
(1)按照配方比例，分别称取主料Fe2O3、ZnO和Mn3O4进行第一次湿法砂磨40min，喷雾干燥制成颗粒，进行预烧，预烧温度为850℃，得到预烧料；
(2)在预烧料中按照配方比例加入第一副成分Bi2O3和第二副成分CaCO3、Co2O3、TiO2、Nb2O5、ZrO2、V2O5，进行第二次湿法砂磨，直至颗粒的平均粒径为1.0μm，再加入10wt％总配料重量浓度9wt％的聚乙烯醇溶液，喷雾干燥，制成粒径为50μm的颗粒；
(3)将上述颗粒加工成型后进行烧结，以5℃\min的升温速率升温到1320℃，在1320℃下烧结4h，烧结时控制氧含量为8％，得到成品，即为所述低损耗、高Bs的锰锌铁氧体材料。
实施例4
一种低损耗、高Bs的锰锌铁氧体材料，包括主成分Fe2O3、ZnO、Mn3O4和副成分Bi2O3、CaCO3、Co2O3、TiO2、Nb2O5、ZrO2和V2O5；
主成分：Fe2O3含量为73.5mol％、ZnO含量为12.6mol％、Mn3O4含量为13.9mol％；
副成分：Bi2O3含量为0.4wt％，CaCO3含量为0.05wt％、Co2O3含量为0.16wt％、TiO2含量为0.07wt％、Nb2O5含量为0.03wt％、ZrO2含量为0.02wt％、V2O5含量为0.06wt％；
所述Bi2O3为掺杂Mn2+的Bi2O3，其Mn2+的掺杂量为2wt％，采用如下方法制备得到：将硝酸铋溶于乙二醇中，加入锰盐混匀，再送入微波反应器中进行微波加热处理，微波功率为580W，时间为16min，冷却，过滤，洗涤，干燥，在600℃下焙烧1h，得到掺杂Mn2+的Bi2O3；
上述低损耗、高Bs的锰锌铁氧体材料的制备方法包括：
(1)按照配方比例，分别称取主料Fe2O3、ZnO和Mn3O4进行第一次湿法砂磨30min以上，喷雾干燥制成颗粒，进行预烧，预烧温度为880℃，得到预烧料；
(2)在预烧料中按照配方比例加入第一副成分Bi2O3和第二副成分CaCO3、Co2O3、TiO2、Nb2O5、ZrO2、V2O5，进行第二次湿法砂磨，直至颗粒的平均粒径为0.8μm，再加入13wt％总配料重量浓度9wt％的聚乙烯醇溶液，喷雾干燥，制成粒径为100μm的颗粒；
(3)将上述颗粒加工成型后进行烧结，以4℃\min的升温速率升温到1360℃，在1360℃下烧结5h，烧结时控制氧含量为6％，得到成品，即为所述低损耗、高Bs的锰锌铁氧体材料。
对比例1
一种锰锌铁氧体材料，包括主成分Fe2O3、ZnO、Mn3O4和副成分Bi2O3、CaCO3、Co2O3、TiO2、Nb2O5、ZrO2和V2O5；
主成分：Fe2O3含量为73.8mol％、ZnO含量为12.4mol％、Mn3O4含量为13.8mol％；
副成分：Bi2O3含量为0.45wt％，CaCO3含量为0.04wt％、Co2O3含量为0.15wt％、TiO2含量为0.06wt％、Nb2O5含量为0.04wt％、ZrO2含量为0.03wt％、V2O5含量为0.05wt％；
上述锰锌铁氧体材料的制备方法包括：
(1)按照配方比例，分别称取主料Fe2O3、ZnO和Mn3O4进行第一次湿法砂磨50min，喷雾干燥制成颗粒，进行预烧，预烧温度为870℃，得到预烧料；
(2)在预烧料中按照配方比例加入第一副成分Bi2O3和第二副成分CaCO3、Co2O3、TiO2、Nb2O5、ZrO2、V2O5，进行第二次湿法砂磨，直至颗粒的平均粒径为0.9μm，再加入12wt％总配料重量浓度8wt％的聚乙烯醇溶液，喷雾干燥，制成粒径为100μm的颗粒；
(3)将上述颗粒加工成型后进行烧结，以3℃\min的升温速率升温到1350℃，在1350℃下烧结5h，烧结时控制氧含量为5％(体积分数)，得到成品。
对比例2
一种锰锌铁氧体材料，包括主成分Fe2O3、ZnO、Mn3O4和副成分Bi2O3、CaCO3、Co2O3、TiO2、Nb2O5、ZrO2和V2O5；
主成分：Fe2O3含量为71.7mol％、ZnO含量为14.5mol％、Mn3O4含量为13.8mol％；
副成分：Bi2O3含量为0.45wt％，CaCO3含量为0.04wt％、Co2O3含量为0.15wt％、TiO2含量为0.06wt％、Nb2O5含量为0.04wt％、ZrO2含量为0.03wt％、V2O5含量为0.05wt％；
上述锰锌铁氧体材料的制备方法包括：
(1)按照配方比例，分别称取主料Fe2O3、ZnO和Mn3O4进行第一次湿法砂磨50min，喷雾干燥制成颗粒，进行预烧，预烧温度为870℃，得到预烧料；
(2)在预烧料中按照配方比例加入第一副成分Bi2O3和第二副成分CaCO3、Co2O3、TiO2、Nb2O5、ZrO2、V2O5，进行第二次湿法砂磨，直至颗粒的平均粒径为0.9μm，再加入12wt％总配料重量浓度8wt％的聚乙烯醇溶液，喷雾干燥，制成粒径为100μm的颗粒；
(3)将上述颗粒加工成型后进行烧结，以3℃\min的升温速率升温到1350℃，在1350℃下烧结5h，烧结时控制氧含量为5％(体积分数)，得到成品。
性能测试：将上述实施例和对比例中得到的锰锌铁氧体材料成品进行电性能测试，结果如下表所示：
Figure BDA0002351154960000081
Figure BDA0002351154960000091
由上表可知，本发明所提出的锰锌铁氧体材料的饱和磁通密度Bs维持在较高水平的前提下，功耗损耗却得到了较大降低。
以上所述，仅为本发明较佳的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，根据本发明的技术方案及其发明构思加以等同替换或改变，都应涵盖在本发明的保护范围之内。

Claims (5)

1.一种低损耗、高Bs的锰锌铁氧体材料，其特征在于，由主成分Fe2O3、ZnO、Mn3O4和第一副成分Bi2O3以及第二副成分CaCO3、Co2O3、TiO2、Nb2O5、ZrO2和/或V2O5组成，所述主成分中，Fe2O3含量为73.5-74.1mol%、ZnO含量为12.2-12.6mol%、Mn3O4含量为13.5-13.9mol%；第一副成分Bi2O3以主成分为基础，其含量为0.4-0.5wt%；所述Bi2O3为掺杂Mn2+的Bi2O3；所述Bi2O3中Mn2+的掺杂量为0.1-2.8wt%；第二副成分以主成分为基础，CaCO3含量为0.01-0.08wt%、Co2O3含量为0.1-0.2wt%、TiO2含量为0.05-0.08wt%、Nb2O5含量为0.02-0.05wt%、ZrO2含量为0.01-0.04wt%、V2O5含量为0.01-0.1wt%；
其中，所述Bi2O3采用如下方法制备得到：将硝酸铋溶于乙二醇中，加入锰盐混匀，再送入微波反应器中进行微波加热处理，冷却，过滤，洗涤，干燥，在580-630℃下焙烧1-2h，得到掺杂Mn2+的Bi2O3。
2.一种根据权利要求1所述低损耗、高Bs的锰锌铁氧体材料的制备方法，其特征在于，包括如下步骤：
（1）按照配方比例，分别称取主料Fe2O3、ZnO和Mn3O4进行第一次湿法砂磨30min以上，喷雾干燥制成颗粒，进行预烧，预烧温度为850-880℃，得到预烧料；
（2）在预烧料中按照配方比例加入第一副成分Bi2O3和第二副成分，进行第二次湿法砂磨，直至颗粒的平均粒径为0.8-1.0μm，再加入10-15wt%总配料重量的聚乙烯醇溶液，喷雾干燥，制成粒径为50-200μm的颗粒；
（3）将上述颗粒加工成型后进行烧结，在1320-1380℃下烧结4-6h，烧结时控制氧含量为3-8%，得到成品，即为所述低损耗、高Bs的锰锌铁氧体材料。
3.根据权利要求2所述低损耗、高Bs的锰锌铁氧体材料的制备方法，其特征在于，所述聚乙烯醇溶液为浓度8-9wt%的聚乙烯醇溶液。
4.根据权利要求2所述低损耗、高Bs的锰锌铁氧体材料的制备方法，喷雾干燥时，喷雾塔进口温度320-360℃，出口温度90-110℃。
5.根据权利要求2所述低损耗、高Bs的锰锌铁氧体材料的制备方法，其特征在于，烧结时，以2-5℃/min的升温速率升温到1320-1380℃。
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