CN113788671A - 一种耐高温浸锡的高性能镍锌软磁铁氧体材料及制备方法 - Google Patents

一种耐高温浸锡的高性能镍锌软磁铁氧体材料及制备方法 Download PDF

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CN113788671A
CN113788671A CN202111162929.0A CN202111162929A CN113788671A CN 113788671 A CN113788671 A CN 113788671A CN 202111162929 A CN202111162929 A CN 202111162929A CN 113788671 A CN113788671 A CN 113788671A
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sintering
immersion
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CN113788671B (zh
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蒋玉梅
郑国友
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Hengdian Group DMEGC Magnetics Co Ltd
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Abstract

本发明属于软磁铁氧体技术领域，公开了一种耐高温浸锡的高性能镍锌软磁铁氧体材料及其制备方法。本发明耐高温浸锡的高性能镍锌软磁铁氧体材料由主成份和添加剂组成，其中，所述主成分由Fe2O3：47～52.5mol％，NiO：16.2～24.06mol％，ZnO：19.3～27.44mol％，以及CuO：4.05～8.12mol％组成；所述添加剂由Al2O3：0.01～0.5wt％，ZrO：0.01～0.5wt％，V2O5：0.05～0.8wt％，Bi2O3：0.05～0.6wt％，以及CaCO3：0.05～0.5wt％组成。该高性能镍锌软磁铁氧体材料主要针对现有技术NiZn软磁铁氧体材料在客户端使用存在严重的浸锡开裂不良、直流叠加不良、强度低等问题，通过改良主成分和添加剂及制作工艺，可批量生产获得高磁导率高Bs高强度且满足耐高温浸锡工艺的镍锌铁氧体材料。

Description

一种耐高温浸锡的高性能镍锌软磁铁氧体材料及制备方法
技术领域
本发明涉及软磁铁氧体技术领域，具体是涉及一种耐高温浸锡的高性能镍锌软磁铁氧体材料及其制备方法。
背景技术
由于镍锌铁氧体具有高导磁率、高电阻率、高使用频率的特点，适用于各类表面贴装元件，被广泛用于各类智能穿戴、5G通信、电动汽车以及消费电子等。随着自动化程度越来越高，电感器件厂商自动化工艺对铁氧体的物理性能要求也越来越高，要求在保持原有电气性能的前提下，提高物理性能；特别是类似于DR+RI配套的磁芯，或者直接磁芯表面电镀的扁平型DR CORE。当前国内NiZn系铁氧体材料存在的主要问题是电感达到了要求，直流叠加达不到；就算电感和直流叠加都满足了要求，强度又达不到要求；最主要的是无法满足高温浸锡要求。国内现有NiZn系材料只能满足一般工艺的浸锡要求，即380℃左右的浸锡温度，无法满足430℃高温的浸锡工艺要求。像美国Coilcraft、日本村田、日本太阳诱电等公司都有对于机械强度、耐高温浸锡条件的硬性要求。现今，电子产品向平板、薄型、表面贴装方向发展，软磁元件尺寸越来越小，因此要求电感器件材料具有较高的饱和磁感应强度Bs、更高的机械强度，且能满足耐高温浸锡工艺要求。
发明内容
本发明的目的是为了克服上述背景技术的不足，提供一种耐高温浸锡的高性能镍锌软磁铁氧体材料。本发明的高性能镍锌软磁铁氧体材料主要针对现有技术NiZn软磁铁氧体材料在客户端使用存在严重的浸锡开裂不良、直流叠加不良、强度低等问题，通过改良主成分和添加剂及制作工艺，可批量生产获得高磁导率高Bs高强度且满足耐高温浸锡工艺的镍锌铁氧体材料。
为达到本发明的目的，本发明耐高温浸锡的高性能镍锌软磁铁氧体材料由主成份和添加剂组成，其中，所述主成分由Fe2O3：47～52.5mol％，NiO：16.2～24.06mol％，ZnO：19.3～27.44mol％，以及CuO：4.05～8.12mol％组成；所述添加剂由Al2O3：0.01～0.5wt％，ZrO：0.01～0.5wt％，V2O5：0.05～0.8wt％，Bi2O3：0.05～0.6wt％，以及CaCO3：0.05～0.5wt％(wt％为添加剂占总投料量的重量百分比)组成。
优选地，在本发明的一些实施例中，所述主成分由Fe2O3：48～51.5mol％，NiO：17.25～21.02mol％，ZnO：19.3～26.64mol％，以及CuO：5.05～8.02mol％组成。
优选地，在本发明的一些实施例中，所述添加剂由Al2O3：0.05～0.3wt％，ZrO：0.01～0.2wt％，V2O5：0.1～0.5wt％，Bi2O3 0.05～0.3wt％，以及CaCO3 0.1～0.3wt％组成。
另一方面，本发明还提供了一种前述耐高温浸锡的高性能镍锌软磁铁氧体材料的制备方法，所述方法包括如下步骤：
(1)配料球磨：按所需主成分的配比，称取Fe2O3、NiO、ZnO、CuO四种原料，然后在砂磨机中加入去离子水进行混合和破碎，球磨0.5～2h得一次球磨粉料；
(2)预烧：将一次球磨粉料通风烘干后放在箱式预烧炉进行预烧，预烧温度控制在930±10℃，烧结1～3h，冷却后得一次预烧料；
(3)二次砂磨：在预烧料中按所需添加剂的量加入Al2O3、ZrO、V2O5、Bi2O3、CaCO3，然后将粉料放入砂磨机中加入去离子水进行二次砂磨，砂磨时间1～3h，粒径控制在0.6～1.3μm之间，成正态分布，烘干、研磨分散得二次砂磨粉料；
(4)喷雾造粒：在二次砂磨料中加入质量浓度为8～12％的PVA，以及干粉重量0.01％～0.1wt％的消泡剂，然后进行离心喷雾造粒得50～250μm的颗粒；
(5)成型：在颗粒料中添加质量浓度为2～8％的PVA，搅拌均匀，采用粉末成型机压制成密度为3.05～3.25g/cm3毛坯。
(6)烧结：将毛坯放在辊道窑中空气气氛烧结，烧结温度控制在1050～1200℃之间，以2～3℃/min升温，升到高温区保温3～5h，以3～5℃/min降温，冷却后得NiZn铁氧体磁芯。
进一步地，在本发明的一些实施例中，所述消泡剂为正辛醇。
与现有技术相比，本发明的优点如下：
(1)本发明通过配方研制和微量元素改性，克服了低磁导率、低Bs、低强度及耐热性差等问题，开发出具有高磁导率、高Bs、高强度且可以满足耐高温浸锡工艺的高性能NiZn软磁铁氧体材料。
(2)本发明中制得的NiZn铁氧体材料具有高磁导率高Bs高强度及耐高温浸锡等特性，其中：
初始磁导率μi[25℃]＝450±25％(@1KHz,0.25V)；
饱和磁感应强度Bs[25℃]≥440mT(@50Hz,4000A/m)；
居里温度Tc[℃]≥230；
电阻率ρ(Ω·m)≥106；
烧结密度d(g/cm3)：5.1。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合实施例，对本发明进行进一步详细说明。本发明的附加方面和优点将在下面的描述中部分给出，部分将从下面的描述中变得明显，或通过本发明的实践了解到。应当理解，以下描述仅仅用以解释本发明，并不用于限定本发明。
本文中所用的术语“包含”、“包括”、“具有”、“含有”或其任何其它变形，意在覆盖非排它性的包括。例如，包含所列要素的组合物、步骤、方法、制品或装置不必仅限于那些要素，而是可以包括未明确列出的其它要素或此种组合物、步骤、方法、制品或装置所固有的要素。
当量、浓度、或者其它值或参数以范围、优选范围、或一系列上限优选值和下限优选值限定的范围表示时，这应当被理解为具体公开了由任何范围上限或优选值与任何范围下限或优选值的任一配对所形成的所有范围，而不论该范围是否单独公开了。例如，当公开了范围“1至5”时，所描述的范围应被解释为包括范围“1至4”、“1至3”、“1至2”、“1至2和4至5”、“1至3和5”等。当数值范围在本文中被描述时，除非另外说明，否则该范围意图包括其端值和在该范围内的所有整数和分数。
此外，下面所描述的术语“一个实施例”、“一些实施例”、“示例”、“具体示例”、或“一些示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中，对上述术语的示意性表述不是必须针对相同的实施例或示例。而且，本发明各个实施方式中所涉及到的技术特征只要彼此之间未构成冲突就可以相互组合。
实施例1
一种耐高温浸锡的高性能镍锌软磁铁氧体材料，所述材料中各主成分和添加剂的配比如表1所示，其制备方法包括如下步骤：
1.配料球磨
按照表1中各主成分的配比，分别以Fe2O3、ZnO、NiO和CuO形式计算比例，称取Fe2O3、NiO、ZnO、CuO四种原料，然后在砂磨机中加入去离子水进行混合和破碎，球磨1.5h得一次球磨粉料。
2.预烧
将一次球磨粉料通风烘干后放在箱式预烧炉进行预烧，预烧温度控制在930±10℃，烧结2h，冷却后得一次预烧料。
3.二次砂磨
在预烧料中按照表1中成分配比加入添加剂：Al2O3、ZrO、V2O5、Bi2O3、CaCO3，然后将粉料放入砂磨机中加入去离子水进行二次砂磨，砂磨时间2h，粒径控制在0.6～1.3μm之间(粉体颗粒的粒径成正态分布)，烘干、研磨分散得二次砂磨粉料。
4.喷雾造粒
在二次砂磨料中加入质量浓度为10％的PVA，以及干粉重量的0.05wt％的消泡剂正辛醇，然后在喷雾塔中进行离心喷雾造粒成50～250μm的颗粒。
5.成型
在颗粒料中添加质量浓度为5％的PVA，搅拌均匀，采用粉末成型机压制成密度为3.15g/cm3毛坯。
6.烧结
将毛坯放在辊道窑中空气气氛烧结，烧结温度控制在1050～1200℃之间，以2.5℃/min升温，升到高温区保温4h，以4℃/min降温，冷却后得NiZn铁氧体磁芯。
实施例2-4和对比例1-4
除材料中各主成分和添加剂的配比如表1所示外，其制备方法基本与实施例1一致。
表1实施例1-4和对比例1-4主成分配方及添加剂比例
Figure BDA0003290458730000051
Figure BDA0003290458730000061
对各实施例和对比例烧结后的磁芯进行测试和评价：用标环在匝数N＝20Ts条件下，用E4980A型LCR测试仪测试磁环样品的起始磁导率μi；用SY-8258型B-H分析仪测试样品的饱和磁感应强度Bs(50Hz/4000A/m)，用LCR-4225型电感分析仪和专用烘箱测试样品的居里温度Tc；采用Agilent4339B高阻计测试Ф10*2mm两端的绝缘电阻值R，计算电阻率ρ；用DPX-20TR 强度测试仪测试机械强度，用T＝(435±10)℃的锡炉，时间3秒,浸2次，20倍放大镜下看磁芯是否开裂。
具体的性能测试结果如表2所示。
表2实施例1-4和对比例1-4的性能测试表
Figure BDA0003290458730000062
本发明提供的NiCuZn铁氧体材料，为了实现低温烧结及获得优良的电磁性能，本发明在主成分的基础上，添加不同添加剂比例对耐高温浸锡和机械强度的影响有关键的改善作用；添加Bi2O3以促进材料的低温烧结；添加V2O5、ZrO和AL2O3改善材料的强度特性和耐高温浸锡特性，同时对抑制Fe2+也起到一定作用，而加入CaCO3和AL2O3有利于增大晶界厚度，抑制晶粒生长，提高材料的Q值；通过对辅助成分的多组实验，对比例1当AL2O3、V2O5、ZrO都不添加时，耐高温浸锡不能达到430℃高温的浸锡工艺要求，机械强度也比实施例要差，达不到效果；对比例2当AL2O3、ZrO都不添加时，但是添加V2O5时，机械强度有提高，也比实施例要差，耐高温浸锡还是不能达到430℃高温的浸锡工艺要求；机械强度也比实施例要差；对比例3当V2O5不添加并且ZrO添加比例在极下限时，耐高温浸锡不能达到430℃高温的浸锡工艺要求，机械强度也比实施例要差，达不到效果；对比例4当V2O5不添加并且Al2O3和ZrO添加比例在极下限时，耐高温浸锡不能达到430℃高温的浸锡工艺要求，机械强度也比对比例3要差，达不到效果；在综合添加量为Al2O3 0.05～0.3wt％，ZrO 0.01～0.2wt％，V2O5 0.1～0.5wt％，Bi2O3 0.05～0.3wt％，CaCO3 0.1～0.3wt％时，材料可获得较高的磁导率、高Bs、高强度及耐高温浸锡特性。通过以上各个成分的共同协同，本发明提供的NiCuZn铁氧体材料可在1140℃以下烧结，获得的材料电阻率在109Ω·cm以上，可起绝缘作用；获得的材料的起始磁导率有450，Bs大于440mT，局里温度大于240℃，且具有良好的机械强度和430℃浸锡不开裂的特性，尤其适用于小型化表面贴装电感器件的产品。
本领域的技术人员容易理解，以上所述仅为本发明的实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。

Claims (5)

1.一种耐高温浸锡的高性能镍锌软磁铁氧体材料，其特征在于，所述耐高温浸锡的高性能镍锌软磁铁氧体材料由主成份和添加剂组成，其中，所述主成分由Fe2O3：47～52.5mol％，NiO：16.2～24.06mol％，ZnO：19.3～27.44mol％，以及CuO：4.05～8.12mol％组成；所述添加剂由Al2O3：0.01～0.5wt％，ZrO：0.01～0.5wt％，V2O5：0.05～0.8wt％，Bi2O3：0.05～0.6wt％，以及CaCO3：0.05～0.5wt％组成。
2.根据权利要求1所述的耐高温浸锡的高性能镍锌软磁铁氧体材料，其特征在于，所述主成分由Fe2O3：48～51.5mol％，NiO：17.25～21.02mol％，ZnO：19.3～26.64mol％，以及CuO：5.05～8.02mol％组成。
3.根据权利要求1所述的耐高温浸锡的高性能镍锌软磁铁氧体材料，其特征在于，所述添加剂由Al2O3：0.05～0.3wt％，ZrO：0.01～0.2wt％，V2O5：0.1～0.5wt％，Bi2O3 0.05～0.3wt％，以及CaCO3 0.1～0.3wt％组成。
4.权利要求1-3任一项所述耐高温浸锡的高性能镍锌软磁铁氧体材料的制备方法，其特征在于，所述方法包括如下步骤：
(1)配料球磨：按所需主成分的配比，称取Fe2O3、NiO、ZnO、CuO四种原料，然后在砂磨机中加入去离子水进行混合和破碎，球磨0.5～2h得一次球磨粉料；
(2)预烧：将一次球磨粉料通风烘干后放在箱式预烧炉进行预烧，预烧温度控制在930±10℃，烧结1～3h，冷却后得一次预烧料；
(3)二次砂磨：在预烧料中按所需添加剂的量加入Al2O3、ZrO、V2O5、Bi2O3、CaCO3，然后将粉料放入砂磨机中加入去离子水进行二次砂磨，砂磨时间1～3h，粒径控制在0.6～1.3μm之间，成正态分布，烘干、研磨分散得二次砂磨粉料；
(4)喷雾造粒：在二次砂磨料中加入质量浓度为8～12％的PVA，以及干粉重量0.01％～0.1wt％的消泡剂，然后进行离心喷雾造粒得50～250μm的颗粒；
(5)成型：在颗粒料中添加质量浓度为2～8％的PVA，搅拌均匀，采用粉末成型机压制成密度为3.05～3.25g/cm3毛坯。
(6)烧结：将毛坯放在辊道窑中空气气氛烧结，烧结温度控制在1050～1200℃之间，以2～3℃/min升温，升到高温区保温3～5h，以3～5℃/min降温，冷却后得NiZn铁氧体磁芯。
5.根据权利要求4所述耐高温浸锡的高性能镍锌软磁铁氧体材料的制备方法，其特征在于，所述消泡剂为正辛醇。
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CN106495677A (zh) * 2016-10-10 2017-03-15 电子科技大学 一种高强度耐热冲击功率镍锌铁氧体及其制备方法
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CN107098690A (zh) * 2017-05-12 2017-08-29 天长市中德电子有限公司 一种高饱和磁通密度低损耗铁氧体
CN111205075A (zh) * 2019-10-23 2020-05-29 横店集团东磁股份有限公司 一种镍锌铁氧体材料及其制备方法
CN111517775A (zh) * 2020-04-01 2020-08-11 深圳顺络电子股份有限公司 一种耐热冲击NiZn铁氧体材料及其制备方法

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