CN111848147B - 一种NiCuZn铁氧体组合物及其制备方法和应用 - Google Patents

一种NiCuZn铁氧体组合物及其制备方法和应用 Download PDF

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CN111848147B
CN111848147B CN202010693428.4A CN202010693428A CN111848147B CN 111848147 B CN111848147 B CN 111848147B CN 202010693428 A CN202010693428 A CN 202010693428A CN 111848147 B CN111848147 B CN 111848147B
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颜冲
张建明
张维
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Suzhou Tianyuan Magnetic Materials Co ltd
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Abstract

本发明提供了一种NiCuZn铁氧体组合物及其制备方法和应用。该NiCuZn铁氧体组合物的原料组成中含有主成分和副成分；其中，以主成分的总摩尔百分比为100%计，以氧化物主成分的原料组成为：12.0 mol%‑21.0mol%的NiO、28.0mol%‑36.0mol%的ZnO、2.0mol%‑7.0mol%CuO和余量的Fe2O3；以主成分总重量计的副成分的原料组成为：50ppm‑300ppm的SiO2、100ppm‑500ppm的CaCO3、100ppm‑1500ppm的Sb2O3、500ppm‑4000ppm的MgO、500ppm‑5000ppm的MnO。本发明还提供了上述铁氧体的制备方法和应用，本发明的NiCuZn铁氧体同时具有较高的磁导率和抗弯强度。

Description

一种NiCuZn铁氧体组合物及其制备方法和应用
技术领域
本发明涉及一种铁氧体，尤其涉及一种NiCuZn铁氧体组合物及其制备方法，属于软磁铁氧体组合物技术领域。
背景技术
NiCuZn铁氧体广泛用于高频变压器和电感器，对其性能有多方面的要求，主要包括在高频(1MHz及以上)下具有较高的初始磁导率、损耗小、较高的断裂韧性、高的抗弯强度等。
此外，为了减少漏磁，提高变压器的能量转化效率，生产过程中需要进行高精度的研磨、切削加工，以提高磁心的有效磁导率。但是为了避免研磨、切削产生破损，提高加工精度，必须降低研磨、切削速度，导致生产效率降低，成本升高。要避免在较高研磨、切削速度下产生掉块或裂纹，需要提高磁心材料的韧性和抗弯强度。此外为提高变压器的能量转化效率，还需要保持材料具有较高的初始磁导率。
现有的材料技术为了提高磁心的韧性和抗弯强度，都以牺牲材料的初始磁导率为代价，而初始磁导率的提高，也会导致材料韧性的劣化。
发明内容
为了解决现有的上述技术问题，本发明的目的在于提供一种同时具有较高的磁导率和抗弯强度的铁氧体。
本发明的另一目的是提供上述铁氧体的制备方法。
为了解决上述任一技术问题，本发明首先提供了一种NiCuZn铁氧体组合物，该NiCuZn铁氧体组合物的原料组成中含有主成分和副成分；其中，以主成分的总摩尔百分比为100％计，以氧化物主成分的原料组成为：12.0mol％-21.0mol％的NiO、28.0mol％-36.0mol％的ZnO、2.0mol％-7.0mol％的CuO和余量的Fe2O3；
以主成分总重量计的副成分的原料组成为：50ppm-300ppm的SiO2、100ppm-500ppm的CaCO3、100ppm-1500ppm的Sb2O3、500ppm-4000ppm的MgO、500ppm-5000ppm的MnO。
在本发明的一具体实施方式中，主成分的氧化物原料组成为：14.0mol％-18.0mol％的NiO、30.0mol％-34.0mol％的ZnO、4mol％-5.0mol％CuO和余量的Fe2O3。
在本发明的一具体实施方式中，以主成分总重量计的副成分的原料组成为：80ppm-260ppm的SiO2、150ppm-400ppm的CaCO3、150ppm-1000ppm的Sb2O3、700ppm-2000ppm的MgO、700ppm-3000ppm的MnO。
在本发明的一具体实施方式中，以主成分的总摩尔百分比为100％计，主成分的氧化物原料组成为：15.0mol％的NiO、32.0mol％的ZnO、5.0mol％的CuO和余量的Fe2O3；以主成分总重量计的副成分的原料组成为：100ppm的SiO2、500ppm的CaCO3、1000ppm的Sb2O3、1000ppm的MgO、2000ppm的MnO。
本发明的NiCuZn铁氧体组合物通过特定的主成分和副成分协同作用，使该铁氧体同时具有较高的磁导率和抗弯强度，在1MHz下的初始磁导率至少为800，同时抗弯强度至少1200kg/cm2。
本发明还提供了一种器件，该器件含有由本发明的NiCuZn铁氧体组合物制备而成的部件。这里需要说明的是，器件包括但不限于高频变压器和电感器等。
本发明还提供了上述NiCuZn铁氧体的制备方法，该制备方法包括：
将主成分的原料进行湿式混合，得到混合均匀的粉料；
对粉料进行预烧；预烧温度为750-950℃，保温时间为0.5-5小时；
向预烧料中加入副成分的原料组成进行湿式砂磨处理，得到料浆；
向料浆中加入PVA粘结剂，进行喷雾造粒并成型；
成型体在空气中于保温温度下烧结，冷却至室温，得到铁氧体组合物。
优化地，保温温度为970-1070℃；烧结时间为0.5-6小时；降温段从700℃至室温的降温速率为3.0℃/分钟以下。
本发明通过特定主成分及副成分组成特别是副成分SiO2、CaCO3、Sb2O3含量以及MgO和MnO添加物形成复合铁氧体，配合适当的烧结工艺，使本发明的NiCuZn铁氧体组合物，在1MHz下的初始磁导率在800以上，同时抗弯强度在1200kg/cm2以上。
本发明的铁氧体在不改变传统生产工艺，通过限制材料主成分及副成分组成，在保持材料较高初始磁导率的同时，提高了材料的抗弯强度，改善了材料脆性不足，同时，原材料易得。
具体实施方式
实施例1
本实施例提供了一种NiCuZn铁氧体，其包括：
将主组成为表1的原材料在砂磨机中混合1小时，然后在850℃下预烧2小时。以预烧后的粉料质量为基准，在上述预烧料中加入辅助成分，添加的辅助成分是：100ppm的SiO2，500ppm的CaCO3，1000ppm的Sb2O3，1000ppm的MgO和2000ppm的MnO。然后进行二次砂磨2小时，加入PVA后进行喷雾造粒，成型后在1050℃的温度下空气中保温烧结3小时，然后冷却至室温。其中冷却段700℃以下的降温速率为2.0℃/分钟。
烧结样品在1MHz下的初始磁导率和抗弯强度数据示于表1中。
表1
Figure GDA0002642292700000031
实施例2
本实施例提供了一种NiCuZn铁氧体，其包括：
以实施例101配方作为主成分，添加的副成分如表2所示，其它与实施例1相同。
烧结样品在1MHz下的初始磁导率和抗弯强度数据示于表2中。
表2
Figure GDA0002642292700000032
实施例3
本实施例提供了一种NiCuZn铁氧体，其包括：
改变实施例101、实施例102比较例101、比较例102、比较例103的保温温度和冷却段700℃后的降温速率如表3。
烧结样品在1MHz下的初始磁导率和抗弯强度数据示于表3中。
表3
Figure GDA0002642292700000041
以上实施例说明，本发明的铁氧体通过特定主成分及副成分的原料组成，配合适当的烧结工艺，使本发明的NiCuZn铁氧体组合物，在1MHz下的初始磁导率在800以上，同时抗弯强度在1200kg/cm2以上。
上述实施例只为说明本发明的技术构思及特点，其目的在于让熟悉此项技术的人士能够了解本发明的内容并据以实施，并不能以此限制本发明的保护范围。凡根据本发明精神实质所作的等效变化或修饰，都应涵盖在本发明的保护范围之内。

Claims (6)

1.一种NiCuZn铁氧体组合物，该NiCuZn铁氧体组合物的原料组成中含有主成分和副成分；其特征在于：以主成分的总摩尔百分比为100%计，主成分的氧化物原料组成为：12.0mol%-21.0mol%的NiO、28.0mol%-36.0mol%的ZnO、2.0mol%-7.0mol%的CuO和余量的Fe2O3；
以主成分总重量计的副成分的原料组成为：50ppm-300ppm的SiO2、100ppm-500ppm的CaCO3、100ppm-1500ppm的Sb2O3、500ppm-4000ppm的MgO、500ppm-5000ppm的MnO；
所述NiCuZn铁氧体组合物的制备方法，包括：
将主成分的原料进行湿式混合，得到混合均匀的粉料；
对粉料进行预烧；预烧温度为750-950℃，保温时间为0.5-5小时；
向预烧料中加入副成分的原料组成进行湿式砂磨处理，得到料浆；
向料浆中加入PVA粘结剂，进行喷雾造粒并成型；
成型体在空气中于970-1070℃保温温度下烧结0.5-6小时，冷却至室温，降温从700℃至室温的降温速率为3.0℃/分钟以下，得到NiCuZn铁氧体组合物。
2.根据权利要求1所述的NiCuZn铁氧体组合物，其特征在于：主成分的氧化物原料组成为：14.0mol%-18.0mol%的NiO、30.0mol%-34.0mol%的ZnO、4mol%-5.0mol%的CuO和余量的Fe2O3。
3.根据权利要求1所述的NiCuZn铁氧体组合物，其特征在于：以主成分总重量计的副成分的原料组成为：80ppm-260ppm的SiO2、150ppm-500ppm的CaCO3、150ppm-1000ppm的Sb2O3、700ppm-2000ppm的MgO、700ppm-3000ppm的MnO。
4.根据权利要求1所述的NiCuZn铁氧体组合物，其特征在于：以主成分的总摩尔百分比为100%计，主成分的氧化物原料组成为：15.0mol%的NiO、32.0mol%的ZnO、5.0mol%的CuO和余量的Fe2O3；
以主成分总重量计的副成分的原料组成为：100ppm的SiO2、500ppm的CaCO3、1000ppm的Sb2O3、1000ppm的MgO、2000ppm的MnO。
5.根据权利要求1所述的NiCuZn铁氧体组合物，其特征在于：该铁氧体在1MHz下的初始磁导率至少为800，同时抗弯强度至少1200kg/cm2。
6.一种器件，该器件含有由权利要求1-5任一项所述的NiCuZn铁氧体组合物制备而成的部件。
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