CN106518039A - 一种高表面电阻率材料及其制备方法 - Google Patents

一种高表面电阻率材料及其制备方法 Download PDF

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CN106518039A
CN106518039A CN201610946584.0A CN201610946584A CN106518039A CN 106518039 A CN106518039 A CN 106518039A CN 201610946584 A CN201610946584 A CN 201610946584A CN 106518039 A CN106518039 A CN 106518039A
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main constituent
adding ingredient
weight
sand milling
surface resistivity
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赵新江
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Jingshi Magnetic Materials & Element Engineering Tech Research Co Ltd
Wuxi Spinel Magnetics Co Ltd
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Jingshi Magnetic Materials & Element Engineering Tech Research Co Ltd
Wuxi Spinel Magnetics Co Ltd
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Abstract

本发明公开了一种高表面电阻率材料，由主成分、添加成分1、添加成分2制成，所述主成分由以摩尔百分比计的以下原料组成：Fe2O3 52～54%、MnO 38～43%，余量为ZnO。本发明的材料表面电阻可达100KΩ以上，能够降低材料的涡流损耗，从而减少产品的发热，可解决传导干扰、辐射干扰等问题，还具有抗电磁干扰能力。该材料应用于国防、电子、医学、汽车、航天等各个领域，特别适用于对产品设计涡流损耗较小的场合。

Description

一种高表面电阻率材料及其制备方法
技术领域
本发明涉及铁氧体磁性材料技术领域，尤其是一种高表面电阻率MnZn铁氧体磁性材料及其制备方法。
背景技术
MnZn铁氧体是现代电子工业及信息产业的基础材料。MnZn铁氧体按应用特征可以为为三大类型：功率MnZn铁氧体、高磁导率MnZn铁氧体和抗电磁干扰（EMI）MnZn铁氧体。近年来，随着通讯技术、计算机技术的飞速发展，促使电子产品向小型化、高频化、轻量化和高性能方向发展，MnZn铁氧体材料的发展由单一性能的纵深提高转向多项指标同时提高的横向拓展。
软磁铁氧体的损耗可以分为：涡流损耗、磁滞损耗和剩余损耗。对于变压器而言，其初级绕组通电后，线圈所产生的磁通在铁芯流动，因为铁芯本身也是导体，在垂直于磁力线的平面上就会产生感应电势，这个电势在铁芯的断面上形成闭合回路并产生电流，好像一个旋涡，所以称为“涡流”。这个“涡流”使变压器的损耗增加，并使变压器的铁芯发热变、温升增加，由“涡流”所产生的损耗称为“铁损”。另外要绕制变压器需要用大量的铜线，这些铜导线存在着电阻，电流流过时会消耗一定的功率，这部分损耗往往变成热量而消耗，称这种损耗为“铜损”。所以变压器的温升主要由铁损和铜损产生的。涡流损耗是指软磁材料在交流磁化时，由于电阻率很低而产生强大的涡电流，使产品发热，损失能耗。材料的涡流损耗与样品的厚度d2和频率f2成正比，即：Pe=π2f2Uod2/3ρ，由上式可知，增大材料的表面电阻ρ可以降低材料的涡流损耗。
发明内容
本发明的第一个目的是为了克服现有材料涡流损耗大的问题，提供了一种高表面电阻率的材料。
本发明的第二个目的是提供一种上述材料的制备方法。
本发明的目的通过以下技术方案来具体实现的：
一种高表面电阻率材料，由主成分、添加成分1、添加成分2制成，所述主成分由以摩尔百分比计的以下原料组成：Fe2O3 52～54%、MnO 38～43%，余量为ZnO；
以主成分的重量为基准，所述添加成分1为CaCO3 0.01～0.5％和/或 TiO2 0.05～0.5％；
以主成分的重量为基准，所述添加成分2包括Nb2O5 0.01～0.10％、Ta2O5 0.01～0.20％、NiO 0.05～0.35%、ZrO2 0.01～0.10％、V2O5 0.01～0.15％、SnO2 0.05～0.35%、SiO2 0.05～0.15%中的一种或其混合物，添加量不超过5000ppm。
上述高表面电阻率材料的制备方法，包括如下步骤：
（1）按主成分的摩尔百分比称取原料，混合得到主成分；
（2）按重量比称取添加成分1、添加成分2，将添加成分1、添加成分2分别与部分的步骤（1）得到的主成分混合进行预分散处理；
（3）一次砂磨，将步骤（1）剩余的主成分和步骤（2）预分散处理的添加成分1混合，加水进行砂磨；
（4）一次干燥，将粘合剂加入步骤（3）得到的混合物中搅拌，然后进行喷雾干燥；
（5）预烧，将步骤（4）得到的干燥物预烧，得到预烧料；
（6）二次砂磨，将步骤（2）预分散处理的添加成分2加入步骤（5）得到的预烧料中，加水进行砂磨；
（7）二次干燥，将粘合剂加入步骤（6）得到的混合物中搅拌，进行喷雾干燥，得到颗粒料。
进一步的，将步骤（7）得到的颗粒料压制成环形生坯，将环形生坯烧结，得到磁芯。
进一步的，步骤（2）的预分散处理方法为，分别将以重量比1:10计的添加成分1、添加成分2与主成分用球磨机混合2h以上。
进一步的，步骤（3）中水的加入量为步骤（1）主成分重量的50%，砂磨时间20～30min；
步骤（4）中的粘合剂为6～8wt%的聚乙烯醇PVA溶液，加入量为步骤（1）主成分重量的10%，搅拌时间2h；
步骤（5）中预烧温度为800～1000℃，预烧时间1～2h；
步骤（6）中水的加入量为步骤（1）主成分重量的50%，砂磨时间1.5～2.5h；
步骤（7）中粘合剂为8～9wt%的聚乙烯醇溶液，加入量为步骤（1）主成分重量的10%，搅拌时间2h。
进一步的，环形生坯在1180～1300℃、1.5～6%的氧分压下保温烧结3～5h。
本发明通过主成分、添加成分和烧结工艺的控制，得到一种高表面电阻率的MnZn铁氧体磁性材料，该材料应用于国防、电子、医学、汽车、航天等各个领域，特别适用于对产品设计涡流损耗较小的场合。
本发明的有益效果为：
1、提高MnZn铁氧体材料的表面电阻率，市售产品的表面电阻在20KΩ以下，本发明可以做到100KΩ以上；
2、降低材料的涡流损耗，从而减少产品的发热问题；
3、可解决传导干扰、辐射干扰等问题；
4、具有抗电磁干扰能力。
具体实施方式
以下对本发明的优选实施例进行说明，应当理解，此处所描述的优选实施例仅用于说明和解释本发明，并不用于限定本发明。
本发明所用的原料均为市场可得产品，PVA型号为：NJ-Ⅱ，厂家：中国石化集团四川维尼纶厂。
实施例1
称取Fe203 8464g（53mol）、MnO 2694g（38mol）、 ZnO 733g（9mol），混合得到主成分。称取CaCO3 30g、主成分300g，用球磨机混合3h；称取Nb2O5 10g、Ta2O5 20g、主成分300g，用球磨机混合3h。将剩余的11291g主成分和预分散处理后的CaCO3投入砂磨机中，加入 5946g去离子水，砂磨20min，抽至搅拌机中，加入1189g 6wt%的PVA 溶液，搅拌2h后，进行喷雾干燥。将干燥好的红色粉料在850℃的温度下预烧2 h，得到预烧料。将预烧料和预分散处理的Nb2O5、Ta2O5加入砂磨机中，加入5946g去离子水，砂磨2h，砂磨后抽至搅拌机，加入1189g 8wt%的PVA 溶液，搅拌2h，进行二次喷雾造粒，得到颗粒料。用压机将颗粒料压制成一定尺寸的环形生坯。将环形生坯置于1200°C、3%的氧分压下保温烧结4 h，得到所需磁芯。
本实施例1制备的磁芯，其表面电阻值为114.3KΩ。
实施例2
称取Fe203 8464g（53mol）、MnO 3049g（43mol）、 ZnO 326g（4mol），混合得到主成分。称取TiO2 40g、主成分400g，用球磨机混合3h；称取NiO20g、V2O5 15g、主成分350g，用球磨机混合3h。将剩余的11089g主成分和预分散处理后的TiO2投入砂磨机中，加入 5920g去离子水，砂磨30min，抽至搅拌机中，加入1184g 8wt%的PVA 溶液，搅拌2h后，进行喷雾干燥。将干燥好的红色粉料在1000℃的温度下预烧1.5 h，得到预烧料。将预烧料和预分散处理的NiO、V2O5加入砂磨机中，加入5920g去离子水，砂磨2.5h，砂磨后抽至搅拌机，加入1184g 9wt%的PVA 溶液，搅拌2h，进行二次喷雾造粒，得到颗粒料。用压机将颗粒料压制成一定尺寸的环形生坯。将环形生坯置于1280°C、6%的氧分压下保温烧结4.5 h，得到所需磁芯。
本实施例2制备的磁芯，其表面电阻值为124.1KΩ。
对比例
从市场上购买TDK公司生产的PQ2620型磁芯，随机抽取两个测其表面电阻，电阻值分别为6.5KΩ和13.3KΩ。
对比本发明实施例和对比例磁芯的表面电阻值，可见使用本发明的MnZn铁氧体材料制备的磁芯的表面电阻＞100KΩ，明显高于市面普通铁氧体磁芯的表面电阻。
以上所述仅为本发明的优选实施例而已，并不用于限制本发明，尽管参照前述实施例对本发明进行了详细的说明，对于本领域的技术人员来说，其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (6)

1.一种高表面电阻率材料，其特征在于，该材料由主成分、添加成分1、添加成分2制成，所述主成分由以摩尔百分比计的以下原料组成：Fe2O3 52～54%、MnO 38～43%，余量为ZnO；
以主成分的重量为基准，所述添加成分1为CaCO3 0.01～0.5％和/或 TiO2 0.05～0.5％；
以主成分的重量为基准，所述添加成分2包括Nb2O5 0.01～0.10％、Ta2O5 0.01～0.20％、NiO 0.05～0.35%、ZrO2 0.01～0.10％、V2O5 0.01～0.15％、SnO2 0.05～0.35%、SiO2 0.05～0.15%中的一种或其混合物，添加量不超过5000ppm。
2.权利要求1所述的高表面电阻率材料的制备方法，其特征在于，包括如下步骤：
（1）按权利要求1的摩尔百分比称取主成分原料，混合得到主成分；
（2）按权利要求1的重量比称取添加成分1、添加成分2，将添加成分1、添加成分2分别与部分的步骤（1）得到的主成分混合进行预分散处理；
（3）一次砂磨，将步骤（1）剩余的主成分和步骤（2）预分散处理的添加成分1混合，加水进行砂磨；
（4）一次干燥，将粘合剂加入步骤（3）得到的混合物中搅拌，然后进行喷雾干燥；
（5）预烧，将步骤（4）得到的干燥物预烧，得到预烧料；
（6）二次砂磨，将步骤（2）预分散处理的添加成分2加入步骤（5）得到的预烧料中，加水进行砂磨；
（7）二次干燥，将粘合剂加入步骤（6）得到的混合物中搅拌，进行喷雾干燥，得到颗粒料。
3.根据权利要求2所述的高表面电阻率材料的制备方法，其特征在于，将步骤（7）得到的颗粒料压制成环形生坯，将环形生坯烧结，得到磁芯。
4.根据权利要求2所述的高表面电阻率材料的制备方法，其特征在于，步骤（2）的预分散处理方法为，分别将以重量比1:10计的添加成分1、添加成分2与主成分用球磨机混合2h以上。
5.根据权利要求2所述的高表面电阻率材料的制备方法，其特征在于，步骤（3）中水的加入量为步骤（1）主成分重量的50%，砂磨时间20～30min；
步骤（4）中的粘合剂为6～8wt%的聚乙烯醇溶液，加入量为步骤（1）主成分重量的10%，搅拌时间2h；
步骤（5）中预烧温度为800～1000℃，预烧时间1～2h；
步骤（6）中水的加入量为步骤（1）主成分重量的50%，砂磨时间1.5～2.5h；
步骤（7）中粘合剂为8～9wt%的聚乙烯醇溶液，加入量为步骤（1）主成分重量的10%，搅拌时间2h。
6.根据权利要求3所述的高表面电阻率材料的制备方法，其特征在于，环形生坯在1180～1300℃、1.5～6%的氧分压下保温烧结3～5h。
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