CN107089828B - 一种宽温宽频低比磁导率温度系数的锰锌高磁导率材料及其制备方法 - Google Patents

一种宽温宽频低比磁导率温度系数的锰锌高磁导率材料及其制备方法 Download PDF

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CN107089828B
CN107089828B CN201710168607.4A CN201710168607A CN107089828B CN 107089828 B CN107089828 B CN 107089828B CN 201710168607 A CN201710168607 A CN 201710168607A CN 107089828 B CN107089828 B CN 107089828B
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吕飞雨
卢飞翔
严正信
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Hengdian Group DMEGC Magnetics Co Ltd
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Abstract

本发明涉及铁氧体技术领域，公开了一种宽温宽频低比磁导率温度系数的锰锌高磁导率材料及其制备方法。该材料包含主成分，所述主成分由以下物质组成：占53.0‑54.0mol%的Fe2O3，以MnO换算计占29.5‑30.5mol%的Mn3O4，占16.0‑17.0mol%的ZnO。本发明的宽温宽频低比磁导率温度系数的锰锌高磁导率材料可应用于电子电路宽带变压器、滤波电感等中，其能够在很大程度上解决现有软磁铁氧体材料在极端条件下的应用范围小的技术问题。

Description

一种宽温宽频低比磁导率温度系数的锰锌高磁导率材料及其 制备方法
技术领域
本发明涉及铁氧体技术领域，尤其涉及一种宽温宽频低比磁导率温度系数的锰锌高磁导率材料及其制备方法。
背景技术
近年来，随着铁氧体在通信、IT产业、汽车产业、航空航天领域、舰船及国防武器装备系统等各行业的广泛应用，现代通信设备的户外设施、卫星等设备，无论在炎热的热带还是寒冷的寒带地区，不仅要求耐高温，还要承受严寒。这就要求所使用的元器件具有宽温、高稳定、长寿命的优良特性。
但是，现有技术中的锰锌铁氧体材料存在在-55℃至125℃温度区间、频率在1KHZ和700KHZ电感变化大的问题，从而严重影响电感器在极端低温条件下输出稳定性。
发明内容
为了解决上述技术问题，本发明提供了一种宽温宽频低比磁导率温度系数的锰锌高磁导率材料及其制备方法。本发明的宽温宽频低比磁导率温度系数的锰锌高磁导率材料可应用于电子电路宽带变压器、滤波电感等中，其能够在很大程度上解决现有软磁铁氧体材料在极端条件下的应用范围小的技术问题。
本发明的具体技术方案为：一种宽温宽频低比磁导率温度系数的锰锌高磁导率材料，包含主成分，所述主成分由以下物质组成：占53.0-54.0mol％的Fe2O3，以MnO换算计占29.5-30.5mol％的Mn3O4，占16.0-17.0mol％的ZnO。
本发明的宽温宽频低比磁导率温度系数的锰锌高磁导率材料，为了得到较高的磁导率值，通过增加Fe2O3的含量，以及减少ZnO的含量来实现，由于需要保持在-55℃下的磁导率，Fe2O3和ZnO的含量需要搭配调整来实现。本发明人通过长期研究发现：当Fe2O3和ZnO的含量在上述特定范围内时，可以同时满足磁导率和宽温的要求，当Fe2O3含量低于上述特定范围时，在-55℃下的磁导率将低于3300。当Fe2O3的含量高于上述特定范围时，在125℃下的磁导率将高于5500。
作为优选，该宽温宽频低比磁导率温度系数的锰锌高磁导率材料还包括第一副成分Co2O3，以主成分为基础，Co2O3的含量为0.05-0.3wt％。
在本发明中，第一副成分Co2O3的主要作用是：通过添加Co2O3可以生成K1正值很大的CoFe2O4，由于Co2+的K1值很大，所以组成中CoFe2O4含量的多少在很大程度上决定了材料的II峰位置，从而可以兼顾在-55℃和125℃下的磁导率变化。由于Co2+不仅对K1有影响，而且会使K2增加，如果Fe2+或Co2+过量的话，会导致高温下K1值远大于零，而且随着温度的升高，K1值增大，对应的μi～T曲线在高温区明显下降，出现较大的负温度系数，综合利用Fe2+和Co2+对K1的补偿作用，若Fe2+和Co2+的比例适当，K1值可能有多个补偿点，对应的μi～T曲线在较宽的温度范围较平坦，由此可获得宽温低温度系数材料，另外磁滞系数与磁导率有一定的对应关系，磁导率高的材料磁滞系数亦小，相反磁导率低的材料磁滞系数大，而磁导率与K1的倒数呈正比，显然，磁滞系数与K1有着内在的联系，调节Fe2+与Co2+的含量，使K1值趋近于零，减小磁滞系数，提高磁导率。本发明人通常长期研究后发现：主成分及第一副成分控制在上述特定范围以内的软磁铁氧体材料，在-55℃下的磁导率μi为4400±25％(3300-5500)(测试条件f＝10kHz，u＝0.05v)，在125℃下的磁导率μi为4400±25％(3300-5500)(测试条件f＝10kHz，u＝0.05v)，比磁导率温度系数αμr(-55℃-125℃)(测试条件f＝10kHz，u＝0.05v)小于0.86×10-6/℃。
作为优选，该宽温宽频低比磁导率温度系数的锰锌高磁导率材料还包括第二副成分，以主成分为基础，第二副成分的含量为：CaCO3占0.05-0.15wt％，Nb2O5占0.01-0.04wt％，TiO2占0.01-0.3wt％，ZrO2占0.01-0.04wt％。
作为优选，该宽温宽频低比磁导率温度系数的锰锌高磁导率材料在-55℃下的磁导率μi为3300～5500，测试条件f＝10kHz，f＝800kHz，u＝0.05v；在125℃下的磁导率μi为3300～5500，测试条件f＝10kHz，f＝800kHz，u＝0.05v；比磁导率温度系数αμr(-55℃-125℃，测试条件f＝10kHz，u＝0.05v)小于0.86×10-6/℃。
一种宽温宽频低比磁导率温度系数的锰锌高磁导率材料的制备方法，包括以下步骤：
(1)配料：称取主成分，主成分中由占53.0-54.0mol％的Fe2O3，以MnO换算计占29.5-30.5mol％的Mn3O4，占16.0-17.0mol％的ZnO组成；在砂磨机中加入去离子水进行混合和破碎35-45min，再循环混合8-12min后进行喷雾造粒，得到喷雾料。
(2)预烧：将喷雾料放入回转窑预烧炉中，在840-860℃下进行预烧，得到预烧料。
(3)二次砂磨：在预烧料中加入以下预烧料重量百分比的副成分：Co2O3 0.05-0.3wt％，CaCO3 0.05-0.15wt％，Nb2O5 0.01-0.04wt％，TiO2 0.01-0.3wt％，ZrO2 0.01-0.04wt％；然后将物料放入卧式通过式研磨机中，加入去离子水进行二次砂磨，得到粒度分布为X50＝1.0-1.3μm，X99＝2.0-4.0μm的二次砂磨料。
(4)喷雾造粒和成型：在二次砂磨料中加入其质量0.04-0.12wt％的PVA和0.001-0.05wt％的消泡剂，接着在喷雾塔中进行喷雾造粒成50-200μm的颗粒；然后将颗粒加工成型为密度为3.00-3.15g/cm3的毛坯。其中，PVA的作为其增强物料的可塑性和粘结性，使物料易于成型。
(5)烧结：在空气中按0.5-3℃\min的升温速率升温到890-910℃，然按2-5℃\min的升温速率升温到在1270-1290℃，此期间氧含量控制0-1％，到达目标温度后下烧结4-7小时，烧结时的氧含量为3-8％，然后在平衡氧分压气氛(氧含量0-3％)中冷却到室温，制得成品。
作为优选，步骤(2)中，预烧时的进料量为240-260kg/h。
作为优选，步骤(3)中，二次砂磨时，以干粉计，进料量为231-235kg/h。
作为优选，步骤(4)中，成型后的毛坯为尺寸为H25*15*8mm的标准样环毛坯。
与现有技术对比，本发明的有益效果是：本发明的宽温宽频低比磁导率温度系数的锰锌高磁导率材料可应用于电子电路宽带变压器、滤波电感等中，其能够在很大程度上解决现有软磁铁氧体材料在极端条件下的应用范围小的技术问题。
具体实施方式
下面结合实施例对本发明作进一步的描述。
一种宽温宽频低比磁导率温度系数的锰锌高磁导率材料，包括：
主成分，所述主成分由以下物质组成：占53.0-54.0mol％的Fe2O3，以MnO换算计占29.5-30.5mol％的Mn3O4，占16.0-17.0mol％的ZnO。
副成分，以主成分为基础，副成分包括：Co2O3占0.05-0.3wt％；CaCO3占0.05-0.15wt％，Nb2O5占0.01-0.04wt％，TiO2占0.01-0.3wt％，ZrO2占0.01-0.04wt％。
该材料的特性为：在-55℃下的磁导率μi为3300～5500，测试条件f＝10kHz，f＝800kHz，u＝0.05v；在125℃下的磁导率μi为3300～5500，测试条件f＝10kHz，f＝800kHz，u＝0.05v；比磁导率温度系数αμr(-55℃-125℃，测试条件f＝10kHz，u＝0.05v)小于0.86×10-6/℃。
实施例1-6以及对比例1-6中各原料含量为：
实施例7
实施例1的宽温宽频低比磁导率温度系数的锰锌高磁导率材料的制备方法，包括以下步骤：
(1)配料：称取主成分；在砂磨机中加入去离子水进行混合和破碎40min，再循环混合10min后进行喷雾造粒，得到喷雾料。
(2)预烧：将喷雾料放入回转窑预烧炉中，在850℃下进行预烧，得到预烧料。其中预烧时的进料量为250kg/h。
(3)二次砂磨：在预烧料中加入副成分；然后将物料放入卧式通过式研磨机中，加入去离子水进行二次砂磨，得到粒度分布为X50＝1.0-1.3μm，X99＝2.0-4.0μm的二次砂磨料；其中二次砂磨时，以干粉计，进料量为233kg/h。
(4)喷雾造粒和成型：在二次砂磨料中加入其质量0.08wt％的PVA和0.002wt％的消泡剂，接着在喷雾塔中进行喷雾造粒成50-200μm的颗粒；然后将颗粒加工成型为密度为3.10g/cm3的毛坯；该毛坯为尺寸为H25*15*8mm的标准样环毛坯。
(5)烧结：在空气中按1.5℃\min的升温速率升温到900℃，然按3.5℃\min的升温速率升温到在1280℃，此期间氧含量控制0.5％，到达目标温度后下烧结5.5小时，烧结时的氧含量为6％，然后在平衡氧分压气氛(氧含量1.5％)中冷却到室温，制得成品。
实施例8
实施例2的宽温宽频低比磁导率温度系数的锰锌高磁导率材料的制备方法，包括以下步骤：
(1)配料：称取主成分；在砂磨机中加入去离子水进行混合和破碎35min，再循环混合8min后进行喷雾造粒，得到喷雾料。
(2)预烧：将喷雾料放入回转窑预烧炉中，在840℃下进行预烧，得到预烧料。其中预烧时的进料量为240kg/h。
(3)二次砂磨：在预烧料中加入副成分；然后将物料放入卧式通过式研磨机中，加入去离子水进行二次砂磨，得到粒度分布为X50＝1.0-1.3μm，X99＝2.0-4.0μm的二次砂磨料；其中二次砂磨时，以干粉计，进料量为231kg/h。
(4)喷雾造粒和成型：在二次砂磨料中加入其质量0.04wt％的PVA和0.001wt％的消泡剂，接着在喷雾塔中进行喷雾造粒成50-200μm的颗粒；然后将颗粒加工成型为密度为3.00g/cm3的毛坯；该毛坯为尺寸为H25*15*8mm的标准样环毛坯。
(5)烧结：在空气中按0.5℃\min的升温速率升温到890℃，然按2℃\min的升温速率升温到在1270℃，此期间氧含量控制0.1％，到达目标温度后下烧结7小时，烧结时的氧含量为3％，然后在平衡氧分压气氛(氧含量0.1％)中冷却到室温，制得成品。
实施例9
实施例3的宽温宽频低比磁导率温度系数的锰锌高磁导率材料的制备方法，包括以下步骤：
(1)配料：称取主成分；在砂磨机中加入去离子水进行混合和破碎45min，再循环混合12min后进行喷雾造粒，得到喷雾料。
(2)预烧：将喷雾料放入回转窑预烧炉中，在860℃下进行预烧，得到预烧料。其中预烧时的进料量为260kg/h。
(3)二次砂磨：在预烧料中加入副成分；然后将物料放入卧式通过式研磨机中，加入去离子水进行二次砂磨，得到粒度分布为X50＝1.0-1.3μm，X99＝2.0-4.0μm的二次砂磨料；其中二次砂磨时，以干粉计，进料量为235kg/h。
(4)喷雾造粒和成型：在二次砂磨料中加入其质量0.12wt％的PVA和0.05wt％的消泡剂，接着在喷雾塔中进行喷雾造粒成50-200μm的颗粒；然后将颗粒加工成型为密度为3.15g/cm3的毛坯；该毛坯为尺寸为H25*15*8mm的标准样环毛坯。
(5)烧结：在空气中按3℃\min的升温速率升温到910℃，然按5℃\min的升温速率升温到在1290℃，此期间氧含量控制1％，到达目标温度后下烧结4小时，烧结时的氧含量为8％，然后在平衡氧分压气氛(氧含量3％)中冷却到室温，制得成品。
性能测试
将烧结好的样环用惠普的HP4284A LCR测试仪进行电感测试。测试条件分别为：-55℃，25℃，125℃；f＝10kHz，f＝800kHz；u＝0.05v，将电感换算成磁导率，各实施例与对比例的材料的性能如下表所示：
由上表中数据对比可见：在测试条件(f＝10kHz，f＝800kHz，u＝0.05v)下，本发明软磁材料在-55℃下的磁导率μi为4400±25％(3300～5500)，在125℃下的磁导率μi为4400±25％(3300～5500)，在测试条件(f＝10kHz，u＝0.05v)下材料比磁导率温度系数αμr(-55℃～125℃)(小于0.86×10-6/℃。由此可见，本发明软磁铁氧体材料同时具备了宽温宽频低比磁导率温度系数，具有非常好的市场前景。
本发明中所用原料、设备，若无特别说明，均为本领域的常用原料、设备；本发明中所用方法，若无特别说明，均为本领域的常规方法。
以上所述，仅是本发明的较佳实施例，并非对本发明作任何限制，凡是根据本发明技术实质对以上实施例所作的任何简单修改、变更以及等效变换，均仍属于本发明技术方案的保护范围。

Claims (6)

1.一种宽温宽频低比磁导率温度系数的锰锌高磁导率材料，其特征在于包含主成分和第一副成分Co2O3，所述主成分由以下物质组成：占53.2-53.8mol％的Fe2O3，以MnO换算计占30.0-30.3mol％的Mn3O4，占16.2-16.5mol％的ZnO；Co2O3以主成分为基础，Co2O3的含量为0.15-0.25wt％：
所述锰锌高磁导率材料在-55℃下的磁导率μi为3300～5500，测试条件f＝10kHz，f＝800kHz，u＝0.05v；在125℃下的磁导率μi为3300～5500，测试条件f＝10kHz，f＝800kHz，u＝0.05v；在-55℃-125℃下的比磁导率温度系数αμr小于0.86×10-6/℃，测试条件f＝10kHz，u＝0.05v。
2.如权利要求1所述的一种宽温宽频低比磁导率温度系数的锰锌高磁导率材料，其特征在于还包括第二副成分，以主成分为基础，第二副成分的含量为：CaCO3占0.05-0.15wt％，Nb2O5占0.01-0.04wt％，TiO2占0.01-0.3wt％，ZrO2占0.01-0.04wt％。
3.一种宽温宽频低比磁导率温度系数的锰锌高磁导率材料的制备方法，其特征在于包括以下步骤：
(1)配料：称取主成分，主成分中由占53.2-53.8mol％的Fe2O3，以MnO换算计占30.0-30.3mol％的Mn3o4，占16.2-16.5mol％的ZnO组成；在砂磨机中加入去离子水进行混合和破碎35-45min，再循环混合8-12min后进行喷雾造粒，得到喷雾料；
(2)预烧：将喷雾料放入回转窑预烧炉中，在840-860℃下进行预烧，得到预烧料；
(3)二次砂磨：在预烧料中加入以下预烧料重量百分比的副成分：Co2O3 0.05-0.3wt％，CaCO30.05-0.15wt％，Nb2O5 0.01-0.04wt％，TiO2 0.01-0.3wt％，ZrO2 0.01-0.04wt％；然后将物料放入卧式通过式研磨机中，加入去离子水进行二次砂磨，得到粒度分布为X50＝1.0-1.3μm，X99＝2.0-4.0μm的二次砂磨料；
(4)喷雾造粒和成型：在二次砂磨料中加入其质量0.04-0.12wt％的PVA和0.001-0.05wt％的消泡剂，接着在喷雾塔中进行喷雾造粒成50-200μm的颗粒；然后将颗粒加工成型为密度为3.00-3.15g/cm3的毛坯；
(5)烧结：在空气中按0.5-3℃\min的升温速率升温到890-910℃，然后按2-5℃\min的升温速率升温到在1270-1290℃，此期间氧含量控制0-1％，到达目标温度后下烧结4-7小时，烧结时的氧含量为3-8％，然后在氧含量为0-3％的平衡氧分压气氛中冷却到室温，制得成品。
4.如权利要求3所述的一种宽温宽频低比磁导率温度系数的锰锌高磁导率材料的制备方法，其特征在于，步骤(2)中，预烧时的进料量为240-260kg/h。
5.如权利要求3所述的一种宽温宽频低比磁导率温度系数的锰锌高磁导率材料的制备方法，其特征在于，步骤(3)中，二次砂磨时，以干粉计，进料量为231-235kg/h。
6.如权利要求3所述的一种宽温宽频低比磁导率温度系数的锰锌高磁导率材料及制备方法，其特征在于，步骤(4)中，成型后的毛坯为尺寸为H25*15*8mm的标准样环毛坯。
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