CN113087515A - 高饱和磁感应强度和宽温低磁芯损耗锰锌铁氧体及其制备方法和四氟铝酸钾的应用 - Google Patents

高饱和磁感应强度和宽温低磁芯损耗锰锌铁氧体及其制备方法和四氟铝酸钾的应用 Download PDF

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CN113087515A
CN113087515A CN202110336897.5A CN202110336897A CN113087515A CN 113087515 A CN113087515 A CN 113087515A CN 202110336897 A CN202110336897 A CN 202110336897A CN 113087515 A CN113087515 A CN 113087515A
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zinc ferrite
manganese
temperature
high saturation
core loss
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CN113087515B (zh
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符靓
黎树春
谢华林
廖新仁
马俊才
赵飞
张伟鹏
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Chongqing Shangjia Electronics Co ltd
Chongqing University
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Chongqing Shangjia Electronics Co ltd
Chongqing University
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Abstract

本发明公开了一种高饱和磁感应强度和宽温低磁芯损耗锰锌铁氧体及其制备方法和四氟铝酸钾的应用，由摩尔份数的以下主原材料制成，Fe2O3：60.5～70.5mol份；Mn3O4：15.5～22.5mol份；ZnO：10.5～20.5mol份，还包括掺杂成分，各掺杂成分以及它们的加入量占所有主原材料重量之和的百分比分别为：CaCO30.01～0.09wt％、TiO20.01～0.09％、NiO 0.01～0.09wt％、Nb2O50.03～0.10wt％、Li2CO30.01～0.08wt％、Bi2O30.01～0.06wt％、Co2O30.01～0.07wt％、KAlF41～5wt％。提高锰锌铁氧体烧结时的致密性，提高材料的Bs；通过掺杂改性提高锰锌铁氧体的居里温度，降低锰锌铁氧体的Pcv。

Description

高饱和磁感应强度和宽温低磁芯损耗锰锌铁氧体及其制备方 法和四氟铝酸钾的应用
技术领域
本发明涉及一种高饱和磁感应强度和宽温低磁芯损耗锰锌铁氧体及其制备方法和四氟铝酸钾的应用，属于软磁铁氧体材料领域。
背景技术
锰锌铁氧体作为在中低频段产量最大、应用最为广泛的软磁铁氧体材料，是由具有尖晶石结构的aMnFe2O4·bZnFe2O4立方晶系与少量的Fe3O4晶体混合组成的单相固溶体。锰锌铁氧体的晶体结构对称性非常高，具有矫顽力低、磁晶各向异性常数小、起始磁导率高、饱和磁感应强度高、截止频率高等诸多优异的磁性能和功率损耗低、温度稳定良好等特性，自研究开发以来，无论在计算机、通信技术、航空航天、电子电力技术、工业自动化技术、生物医用技术还是在日用生活产品等领域都成为非常重要的部分，在国民经济发展中占据极其重要的地位。
提高锰锌铁氧体的密度可提高材料的饱和磁感应强度(Bs)，在低温(700℃左右)烧结阶段，材料的致密性非常接近理论值，然而，随着烧结温度的提高，材料的密度略有下降。当烧结温度接近传统的烧结温度1300℃时，获得样品的密度却只有理论密度的90％。因此，必须提高锰锌铁氧体的致密性以确保材料的高Bs。
现有技术中的锰锌铁氧体其磁感应强度(Bs)也可以做到600mT左右(1000A/m，50Hz的条件下100℃)，但是存在功率损耗巨大(≥1200mW/cm3)的缺陷，从而使得这些锰锌铁氧体无法实现在工业上的应用。
发明内容
针对上述技术问题，本发明的第一目的在于提供一种氟铝酸钾在制备高饱和磁感应强度和宽温低磁芯损耗锰锌铁氧体中的应用，第二目的在于提供一种高饱和磁感应强度和宽温低磁芯损耗锰锌铁氧体，第三目的在于提供一种高饱和磁感应强度和宽温低磁芯损耗锰锌铁氧体的制备方法。提高锰锌铁氧体烧结时的致密性，提高材料的Bs；通过掺杂改性提高锰锌铁氧体的居里温度，降低锰锌铁氧体的Pcv。
为了实现上述第一目的，本发明的技术方案为：一种四氟铝酸钾在制备高饱和磁感应强度和宽温低磁芯损耗锰锌铁氧体中的应用。
本发明的第二目的是这样实现的：一种高饱和磁感应强度和宽温低磁芯损耗锰锌铁氧体，其特征在于：由摩尔份数的以下主原材料制成，Fe2O3：60.5～70.5mol份；Mn3O4：15.5～22.5mol份；ZnO：10.5～20.5mol份，
还包括掺杂成分，各掺杂成分以及它们的加入量占所有主原材料重量之和的百分比分别为：CaCO30.01～0.09wt％、TiO20.01～0.09％、NiO 0.01～0.09wt％、Nb2O50.03～0.10wt％、Li2CO30.01～0.08wt％、Bi2O30.01～0.06wt％、Co2O30.01～0.07wt％、KAlF41～5wt％。
上述方案中：还包括润滑剂和粘接剂。
上述方案中：所述润滑剂为硬脂酸锌，所述粘接剂为聚乙烯醇溶液，它们的加入量占所有主原材料重量之和的百分比分别为润滑剂0.1～0.5wt％，粘结剂8～12wt％。
本发明的第三目的是这样实现的：一种权利要求2-4任一项所述高饱和磁感应强度和宽温低磁芯损耗锰锌铁氧体的制备方法，其特征在于，按照如下方法制备：
(1)一次砂磨：称量所需的Fe2O3、Mn3O4、ZnO，装入砂磨机充分搅拌后加入蒸馏水，进行湿法砂磨后干燥；
(2)预烧：将一次砂磨后的粉料于750℃～950℃预烧1～6h后自然冷却至室温，得到预烧料；
(3)二次砂磨并掺杂：在上述预烧料中加入掺杂成分，装入砂磨机充分搅拌后加入蒸馏水，进行湿法二次砂磨后烘干；
(4)喷雾造粒和成型：将二次砂磨掺杂干燥后的粉料与润滑剂和粘结剂均匀搅拌混合后在喷雾塔中进行喷雾造粒，制成粒径为100～400μm的圆球形的颗粒料，烘去造粒料表面的水分，使颗粒料具有较好的流动性和分散性，压制成型；
(5)烧结：将压制成型的坯件在钟罩式气氛烧结炉中进行烧结，烧结温度控制在1300℃～1400℃，烧结保温时间4～6h，形成锰锌铁氧体。
本发明通过一次砂磨使原料混合均匀，以利于预烧时加大粉体的铁氧体化程度。通过预烧减少烧结时产品的收缩率，防止铁氧体产品因收缩过大而变形。
上述方案中：一次砂磨时间为50～120min，二次砂磨时间3-8h。
上述方案中：烧结过程是在气氛控制的环境下进行，其中平衡氧分压的范围为：0.5～8％。
上述方案中：Fe2O3、Mn3O4、ZnO粉体的粒度为0.84～1.36μm。
本发明的CaCO3作为第二相沉积在锰锌铁氧体晶界中。TiO2、NiO、Nb2O5、Li2CO3进入锰锌铁氧体尖晶石结构内取代金属离子位置。Bi2O3、Co2O3为在锰锌铁氧体烧结过程中形成液相促进烧结的低溶点氧化物。
众所周知，制备工艺对Bs的影响主要体现在对密度的影响上，当密度增高时，Bs也会随之增高。现有制备工艺基本都是从改善烧成制度着手，如提高成型密度、提高烧结温度、改善氧分压等等。本发明人通过长期对烧结过程的研究发现：在二次砂磨中添加KAlF4能显著提高后期烧结材料的致密性，KAlF4主要应用于钎焊，具有良好的流动性。二次砂磨粉料中，KAlF4以固体的形式均匀分布，在烧结过程中，由于KAlF4的熔点远低于烧结温度，高温使KAlF4熔融以液体的形式流动于烧结体中，由于KAlF4缺乏黏性，不会停留于晶粒之间的间隙里，在不停流动过程一方面带走残留气体，另一方面使晶粒的晶界之间阻力变小，提高了材料的致密性。并且KAlF4的特殊结构不会在熔融过程中电离，形成气态时仍然以KAlF4蒸气存在，因此，在烧结过程中，随着KAlF4的流动逐渐气化，以气体的形式从材料的表面逸出而没有残留，有提高材料致密性的同时不会影响材料的其他磁学性能，通过对比发现，添加KAlF4进行烧结后锰锌铁氧体的密度非常接近理论值。基于NiFe2O4和Li0.5Fe2.5O4的居里温度比FeFe2O4的高，通过加入NiO和Li2CO3改善材料的宽温特性，同时进行材料的配方优化和掺杂改性降低了功率损耗，最终制备了高Bs和宽温低Pcv的锰锌铁氧体。该高Bs和宽温低Pcv的锰锌铁氧体功耗谷点在90℃，在100kHz，200mT时的功率损耗≤250mW/cm3，在1000A/m，50Hz的条件下25℃时Bs≥560mT，在1000A/m，50Hz的条件下100℃时Bs≥460mT。获得了兼具高Bs和宽温低Pcv的高叠加材料。
具体实施方式
下面通过实施例，对本发明作进一步说明：
实施例1
一种高饱和磁感应强度和宽温低磁芯损耗锰锌铁氧体，由Fe2O3：60.5mol；Mn3O4：22.5mol；ZnO：20.5mol和掺杂成分制成。
各掺杂成分以及它们的加入量占所有主原材料重量之和的百分比分别为：CaCO30.01wt％、TiO20.01％、NiO 0.01wt％、Nb2O50.10wt％、Li2CO30.08wt％、Bi2O30.01wt％、Co2O30.01wt％、KAlF41wt％。
润滑剂硬脂酸锌0.5wt％和粘接剂聚乙烯醇溶液8wt％。
按照如下方法制备：
(1)一次砂磨：称量所需的Fe2O3、Mn3O4、ZnO，Fe2O3、Mn3O4、ZnO粉体的粒度为0.84～1.36μm，装入砂磨机充分搅拌后加入蒸馏水，进行湿法砂磨后干燥，一次砂磨时间为120min。
(2)预烧：将一次砂磨后的粉料于750℃～950℃预烧1h后自然冷却至室温，得到预烧料。
(3)二次砂磨并掺杂：在上述预烧料中加入掺杂成分，装入砂磨机充分搅拌后加入蒸馏水，进行湿法二次砂磨后于110℃烘干，二次砂磨时间3h。
(4)喷雾造粒和成型：将二次砂磨掺杂干燥后的粉料与润滑剂和粘结剂均匀搅拌混合后在喷雾塔中进行喷雾造粒，制成粒径为100～400μm的圆球形的颗粒料，烘去造粒料表面的水分，使颗粒料具有较好的流动性和分散性，压制成型。
(5)烧结：将压制成型的坯件在钟罩式气氛烧结炉中进行烧结，烧结温度控制在1300℃～1400℃，烧结保温时间6h，形成锰锌铁氧体。烧结过程是在气氛控制的环境下进行，其中平衡氧分压的范围为：0.5～8％，烧结完后冷却时可用保护气氮气、二氧化碳或循环利用的二氧化碳废气保护。锰锌铁氧体功耗谷点在90℃，在100kHz，200mT时的功率损耗≤250mW/cm3，在1000A/m，50Hz的条件下25℃时Bs 560mT，在1000A/m，50Hz的条件下100℃时Bs 460mT。获得了兼具高Bs和宽温低Pcv的高叠加材料。
实施例2
一种高饱和磁感应强度和宽温低磁芯损耗锰锌铁氧体，由Fe2O3：70.5mol；Mn3O4：15.5mol；ZnO：10.5mol和掺杂成分制成。
各掺杂成分以及它们的加入量占所有主原材料重量之和的百分比分别为：CaCO30.09wt％、TiO20.09％、NiO 0.09wt％、Nb2O50.03wt％、Li2CO30.01wt％、Bi2O30.06wt％、Co2O30.07wt％、KAlF45wt％。
润滑剂硬脂酸锌0.1wt％和粘接剂聚乙烯醇溶液12wt％。
按照如下方法制备：
(1)一次砂磨：称量所需的Fe2O3、Mn3O4、ZnO，Fe2O3、Mn3O4、ZnO粉体的粒度为0.84～1.36μm，装入砂磨机充分搅拌后加入蒸馏水，进行湿法砂磨后干燥，一次砂磨时间为50min。
(2)预烧：将一次砂磨后的粉料于750℃～950℃预烧6h后自然冷却至室温，得到预烧料。
(3)二次砂磨并掺杂：在上述预烧料中加入掺杂成分，装入砂磨机充分搅拌后加入蒸馏水，进行湿法二次砂磨后于110℃烘干，二次砂磨时间8h。
(4)喷雾造粒和成型：将二次砂磨掺杂干燥后的粉料与润滑剂和粘结剂均匀搅拌混合后在喷雾塔中进行喷雾造粒，制成粒径为100～400μm的圆球形的颗粒料，烘去造粒料表面的水分，使颗粒料具有较好的流动性和分散性，压制成型。
(5)烧结：将压制成型的坯件在钟罩式气氛烧结炉中进行烧结，烧结温度控制在1300℃～1400℃，烧结保温时间4h，形成锰锌铁氧体。烧结过程是在气氛控制的环境下进行，其中平衡氧分压的范围为：0.5～8％，烧结完后冷却时可用保护气氮气、二氧化碳或循环利用的二氧化碳废气保护。锰锌铁氧体功耗谷点在90℃，在100kHz，200mT时的功率损耗≤250mW/cm3，在1000A/m，50Hz的条件下25℃时Bs 562mT，在1000A/m，50Hz的条件下100℃时Bs463mT。获得了兼具高Bs和宽温低Pcv的高叠加材料。
实施例3
一种高饱和磁感应强度和宽温低磁芯损耗锰锌铁氧体，由Fe2O3：65.5mol；Mn3O4：15mol；ZnO：15mol和掺杂成分制成。
各掺杂成分以及它们的加入量占所有主原材料重量之和的百分比分别为：CaCO30.05wt％、TiO20.04％、NiO 0.04wt％、Nb2O50.06wt％、Li2CO30.05wt％、Bi2O30.02wt％、Co2O30.03wt％、KAlF43wt％。
润滑剂硬脂酸锌0.2wt％和粘接剂聚乙烯醇溶液10wt％。
按照如下方法制备：
(1)一次砂磨：称量所需的Fe2O3、Mn3O4、ZnO，Fe2O3、Mn3O4、ZnO粉体的粒度为0.84～1.36μm，装入砂磨机充分搅拌后加入蒸馏水，进行湿法砂磨后干燥，一次砂磨时间为80min。
(2)预烧：将一次砂磨后的粉料于750℃～950℃预烧4h后自然冷却至室温，得到预烧料。
(3)二次砂磨并掺杂：在上述预烧料中加入掺杂成分，装入砂磨机充分搅拌后加入蒸馏水，进行湿法二次砂磨后于110℃烘干，二次砂磨时间5h。
(4)喷雾造粒和成型：将二次砂磨掺杂干燥后的粉料与润滑剂和粘结剂均匀搅拌混合后在喷雾塔中进行喷雾造粒，制成粒径为100～400μm的圆球形的颗粒料，烘去造粒料表面的水分，使颗粒料具有较好的流动性和分散性，压制成型。
(5)烧结：将压制成型的坯件在钟罩式气氛烧结炉中进行烧结，烧结温度控制在1300℃～1400℃，烧结保温时间4～6h，形成锰锌铁氧体。烧结过程是在气氛控制的环境下进行，其中平衡氧分压的范围为：0.5～8％，烧结完后冷却时可用保护气氮气、二氧化碳或循环利用的二氧化碳废气保护。锰锌铁氧体功耗谷点在90℃，在100kHz，200mT时的功率损耗≤250mW/cm3，在1000A/m，50Hz的条件下25℃时Bs 566mT，在1000A/m，50Hz的条件下100℃时Bs 465mT。获得了兼具高Bs和宽温低Pcv的高叠加材料。
本发明不局限于上述实施例，本领域的普通技术人员可以理解：在不脱离本发明的原理和宗旨的情况下可以对这些实施例进行多种变化，修改，替换和变型，本发明的范围由权利要求及其等同物限定。

Claims (8)

1.一种四氟铝酸钾在制备高饱和磁感应强度和宽温低磁芯损耗锰锌铁氧体中的应用。
2.一种高饱和磁感应强度和宽温低磁芯损耗锰锌铁氧体，其特征在于，由摩尔份数的以下主原材料制成：Fe2O3：60.5～70.5mol份；Mn3O4：15.5～22.5mol份；ZnO：10.5～20.5mol份；
还包括掺杂成分，各掺杂成分以及它们的加入量占所有主原材料重量之和的百分比分别为：CaCO30.01～0.09wt％、TiO20.01～0.09wt％、NiO 0.01～0.09wt％、Nb2O50.03～0.10wt％、Li2CO30.01～0.08wt％、Bi2O30.01～0.06wt％、Co2O30.01～0.07wt％、KAlF41～5wt％。
3.根据权利要求2所述高饱和磁感应强度和宽温低磁芯损耗锰锌铁氧体，其特征在于：还包括润滑剂和粘接剂。
4.根据权利要求3所述高饱和磁感应强度和宽温低磁芯损耗锰锌铁氧体，其特征在于：所述润滑剂为硬脂酸锌，所述粘接剂为聚乙烯醇溶液，它们的加入量占所有主原材料重量之和的百分比分别为润滑剂0.1～0.5wt％，粘结剂8～12wt％。
5.一种权利要求2-4任一项所述高饱和磁感应强度和宽温低磁芯损耗锰锌铁氧体的制备方法，其特征在于，按照如下方法制备：
(1)一次砂磨：称量所需的Fe2O3、Mn3O4、ZnO，装入砂磨机充分搅拌后加入蒸馏水，进行湿法砂磨后干燥；
(2)预烧：将一次砂磨后的粉料于750℃～950℃预烧1～6h后自然冷却至室温，得到预烧料；
(3)二次砂磨并掺杂：在上述预烧料中加入掺杂成分，装入砂磨机充分搅拌后加入蒸馏水，进行湿法二次砂磨后烘干；
(4)喷雾造粒和成型：将二次砂磨掺杂干燥后的粉料与润滑剂和粘结剂均匀搅拌混合后在喷雾塔中进行喷雾造粒，制成粒径为100～400μm的圆球形颗粒料，烘去造粒料表面的水分，使颗粒料具有较好的流动性和分散性，压制成型；
(5)烧结：将压制成型的坯件在钟罩式气氛烧结炉中进行烧结，烧结温度控制在1300℃～1400℃，烧结保温时间4～6h，形成锰锌铁氧体。
6.根据权利要求5所述高饱和磁感应强度和宽温低磁芯损耗锰锌铁氧体的制备方法，其特征在于：一次砂磨时间为50～120min，二次砂磨时间3-8h。
7.根据权利要求6所述高饱和磁感应强度和宽温低磁芯损耗锰锌铁氧体的制备方法，其特征在于：烧结过程是在气氛控制的环境下进行，其中平衡氧分压的范围为：0.5～8％。
8.根据权利要求5所述高饱和磁感应强度和宽温低磁芯损耗锰锌铁氧体的制备方法，其特征在于：Fe2O3、Mn3O4、ZnO粉体的粒度为0.84～1.36μm。
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