CN115403366B - 一种掺杂锂的镍锌铁氧体材料及其制备方法 - Google Patents

一种掺杂锂的镍锌铁氧体材料及其制备方法 Download PDF

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CN115403366B
CN115403366B CN202211019137.2A CN202211019137A CN115403366B CN 115403366 B CN115403366 B CN 115403366B CN 202211019137 A CN202211019137 A CN 202211019137A CN 115403366 B CN115403366 B CN 115403366B
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zinc ferrite
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张洪良
李文婷
丁兴雨
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Xiamen University
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Abstract

本发明公开了一种掺杂锂的镍锌铁氧体材料及其制备方法，本发明掺杂锂的镍锌铁氧体材料其化学式为Ni0.3LixZn0.7‑xFe2O4，其中x＝0.025～0.5，本发明方法以Ni0.3Zn0.7Fe2O4铁氧体为基础，通过Li+取代部分Zn2+以改善材料的磁性能。其制备方法为：先采用溶胶凝胶自蔓延燃烧法制备前驱体，经过预烧、研磨、成型和特定的烧结程序最终形成。本工艺可精确控制化学成分，操作简单，无废料污染问题，所得材料可以同时获得高磁导率和高饱和磁化强度，为功率电感器件提供关键材料，对进一步促进器件的小型化、集成化发展具有重要意义。

Description

一种掺杂锂的镍锌铁氧体材料及其制备方法
技术领域
本发明属于软磁铁氧体材料技术领域，具体涉及一种掺杂锂的镍锌铁氧体材料的制备方法。
背景技术
随着5G时代的到来，工业4.0和汽车电动化的继续推进，新一代宽禁带半导体在电子电力器件的应用将越来越广泛，涵盖智能家居、智能手机、可穿戴设备和新能源汽车等生活的方方面面。与此同时，这也对与其协同工作的电感器件提出了更高的要求，即小型化、高频化和高功率。
电感器件的核心是软磁材料。在目前的软磁材料中，镍锌铁氧体由于使用频率较高、损耗低以及制备简单等优点，被广泛应用于功率电感器件中。但镍锌铁氧体也存在磁导率低、饱和磁化强度低的缺点。材料的高磁导率对减小器件尺寸意义深远，而饱和磁通密度决定了功率转换器件传输的功率上限。因此，亟需对镍锌铁氧体进行改性研究，以满足电子通讯、5G应用的小型化、高功率、高效率的持续需求。此外，材料性能也会受到制备方法、工艺条件等因素的影响。
发明内容
本发明的目的在于提供一种掺杂锂的镍锌铁氧体材料及其制备方法，
本发明掺杂锂的镍锌铁氧体材料，其化学式为Ni0.3LixZn0.7-xFe2O4，其中x＝0.025～0.5。
优选的，本发明掺杂锂的镍锌铁氧体材料，其化学式为Ni0.3LixZn0.7-xFe2O4，其中x＝0.025～0.3。
进一步地，本发明掺杂锂的镍锌铁氧体材料，其化学式为Ni0.3LixZn0.7-xFe2O4，其中x＝0.05～0.1。
本发明掺杂锂的镍锌铁氧体材料的制备方法，包括如下步骤：
(1)称取硝酸铁、硝酸镍、硝酸锌、硝酸锂溶于去离子水，充分搅拌后加入柠檬酸，控制柠檬酸与溶液中金属离子的摩尔比为1-2:1-2，继续搅拌0.5～1h；
(2)量取氨水，逐滴加入，搅拌0.5～1h，氨水与柠檬酸的摩尔比为2.5-3.5:0.5-1.5；在90～100℃的油浴中加热至自蔓延燃烧，生成蓬松的棕褐色粉体；
(3)将上述棕褐色粉体置于马弗炉中预烧；预烧升温速率为8～10℃/min，预烧温度为200～400℃，预烧时间为6～12h；
(4)研磨，造粒，压制成型；
(5)将压制好的材料置于马弗炉中烧结，烧结升温速率为5～10℃/min，烧结温度为1000～1300℃，烧结时间为6～8h，即得掺杂锂的镍锌铁氧体材料。
作为优选方案，步骤(1)中，柠檬酸与溶液中金属离子的摩尔比为1:1。
作为优选方案，步骤(2)当中，氨水与柠檬酸的摩尔比为3:1。
优选的，步骤(3)当中，预烧升温速率为8～10℃/min，预烧温度为200～400℃，预烧时间为6～12h。
优选的，步骤(4)中，研磨后的粉体加入含有酚醛环氧树脂的胶水造粒。
优选的，步骤(4)当中，含有酚醛环氧树脂的胶水为15ml酚醛环氧树脂F51、10ml固化剂和25ml乙醇的混合溶液。
优选的，胶水与粉体的比例为5～10％，压制的压力为2～4MPa。
本发明原理为：因镍锌铁氧体中存在易变价的Ni和Fe离子，若采用低价离子(一价离子)掺杂可引入空穴，促使八面体位点的Fe2+转变为磁矩更大的Fe3+，增强了四面体、八面体位点的交换作用，有利于饱和磁化强度的增大。而且，部分空穴与晶体中的磁性离子也存在超交换作用。因此，本发明提出在不改变原有磁性离子的情况下，以同样非磁性的Li+代替部分Zn2+，可能会提高材料的饱和磁化强度。同时，采用溶胶凝胶自蔓延燃烧法，实现原子级混合，可精确控制化学计量比，合成过程无废料无污染，且工艺过程简单。
与现有技术相比，本发明具有的有益效果是：磁导率在烧结温度为1200℃、Li掺杂量为0.05时达到1793.0，此时饱和磁化强度为57.8emu/g，成功制备了一种具有高磁导率、高饱和磁化强度的镍锌铁氧体材料，与国内外代表性企业的镍锌铁氧体产品相比富有竞争力。且制备工艺简单环保，可用于制备功率电感器件，有望实现器件的小型化和高功率的应用。
附图说明
图1为本发明实施例与对比例的XRD谱图；
图2为本发明实施例1制备的掺锂镍锌铁氧体标准环的SEM形貌图；
图3为本发明实施例2制备的掺锂镍锌铁氧体标准环的SEM形貌图；
图4为本发明对比例1制备的纯镍锌铁氧体标准环的SEM形貌图；
图5为本发明实施例与对比例的磁频谱图；
图6为本发明实施例与对比例的磁滞回线。
具体实施方式
下面根据具体的实施例详细的描述本发明。
实施例1
(1)按掺锂镍锌铁氧体Ni0.3Li0.05Zn0.65Fe2O4的化学计量摩尔比称取Ni(NO3)2·6H2O、Zn(NO3)2·6H2O、Fe(NO3)3·9H2O、LiNO3溶于去离子水中，搅拌0.5h后加入柠檬酸，控制柠檬酸与溶液中金属离子的摩尔比为1:1，继续搅拌1h；
(2)量取一定量的氨水，控制氨水与柠檬酸的摩尔比为3:1，逐滴加入，搅拌1h，在90～100℃的油浴中加热至自蔓延燃烧，生成蓬松的棕褐色粉体；
(3)将上述棕褐色粉体置于马弗炉中预烧，以10℃/min的速度升温到200℃保温12h，得到锂掺杂镍锌铁氧体的预烧粉料；
(4)将此预烧粉料进行研磨，加入5％的酚醛环氧树脂胶水(含有酚醛环氧树脂的胶水为15ml酚醛环氧树脂F51、10ml固化剂(环氧树脂固化剂594)和25ml乙醇的混合溶液)混合均匀，在2.5MPa的压力下压制成型；
(5)将压制好的环形磁芯置于马弗炉中烧结，以10℃/min的速度升温到1200℃保温7h，即得掺杂锂的镍锌铁氧体材料。所制备材料的表征及性能如图1、图2、图5和图6所示。可见100kHz下，锂掺杂量x＝0.05的镍锌铁氧体磁导率为1793.0，与在相同条件下制备的纯Ni0.3Zn0.7Fe2O4相比提高了约32％，饱和磁化强度也有提升。
实施例2
(1)按掺锂镍锌铁氧体Ni0.3Li0.1Zn0.6Fe2O4的化学计量摩尔比称取Ni(NO3)2·6H2O、Zn(NO3)2·6H2O、Fe(NO3)3·9H2O、LiNO3溶于去离子水中，搅拌0.5h后加入柠檬酸，控制柠檬酸与溶液中金属离子的摩尔比为1:1，继续搅拌1h；
(2)量取一定量的氨水，控制氨水与柠檬酸的摩尔比为3:1，逐滴加入，搅拌1h，在90～100℃的油浴中加热至自蔓延燃烧，生成蓬松的棕褐色粉体；
(3)将上述棕褐色粉体置于马弗炉中预烧，以10℃/min的速度升温到200℃保温12h，得到锂掺杂镍锌铁氧体的预烧粉料；
(4)将此预烧粉料进行研磨，加入5％的酚醛环氧树脂胶水(同实施例1)混合均匀，在2.5MPa的压力下压制成型；
(5)将压制好的环形磁芯置于马弗炉中烧结，以10℃/min的速度升温到1200℃保温7h，即得掺杂锂的镍锌铁氧体材料。所制备材料的表征及性能如图1、图3、图5和图6所示。可见100kHz下，锂掺杂量x＝0.1的镍锌铁氧体磁导率为1396.9，与纯Ni0.3Zn0.7Fe2O4相比有提升，而饱和磁化强度提高了约39％。
对比例1
(1)按镍锌铁氧体Ni0.3Zn0.7Fe2O4的化学计量摩尔比称取Ni(NO3)2·6H2O、Zn(NO3)2·6H2O、Fe(NO3)3·9H2O溶于去离子水中，搅拌0.5h后加入柠檬酸，控制柠檬酸与溶液中金属离子的摩尔比为1:1，继续搅拌1h；
(2)量取一定量的氨水，控制氨水与柠檬酸的摩尔比为3:1，逐滴加入，搅拌1h，在90～100℃的油浴中加热至自蔓延燃烧，生成蓬松的棕褐色粉体；
(3)将上述棕褐色粉体置于马弗炉中预烧，以10℃/min的速度升温到200℃保温12h，得到纯镍锌铁氧体的预烧粉料；
(4)将此预烧粉料进行研磨，加入5％的酚醛环氧树脂胶水(同实施例1)混合均匀，在2.5MPa的压力下压制成型；
(5)将压制好的环形磁芯置于马弗炉中烧结，以10℃/min的速度升温到1200℃保温7h，即得纯镍锌铁氧体材料。所制备材料的表征及性能如图1、图4、图5和图6所示。

Claims (10)

1.一种掺杂锂的镍锌铁氧体材料，其化学式为Ni0.3LixZn0.7-xFe2O4，其中x=0.025~0.5；所述掺杂锂的镍锌铁氧体材料的制备方法，包括如下步骤：
（1）称取硝酸铁、硝酸镍、硝酸锌、硝酸锂溶于去离子水，充分搅拌后加入柠檬酸，控制柠檬酸与溶液中金属离子的摩尔比为1-2:1-2，继续搅拌0.5~1h；
（2）量取氨水，逐滴加入，搅拌0.5~1h，氨水与柠檬酸的摩尔比为2.5-3.5:0.5-1.5；在90~100℃的油浴中加热至自蔓延燃烧，生成蓬松的棕褐色粉体；
（3）将上述棕褐色粉体置于马弗炉中预烧；预烧升温速率为8~10℃/min，预烧温度为200~400℃，预烧时间为6~12h；
（4）研磨，造粒，压制成型；
（5）将压制好的材料置于马弗炉中烧结，烧结升温速率为5~10℃/min，烧结温度为1000~1300℃，烧结时间为6~8h，得掺杂锂的镍锌铁氧体材料。
2.如权利要求1所述的一种掺杂锂的镍锌铁氧体材料，其化学式为Ni0.3LixZn0.7-xFe2O4，其中x=0.025~0.3。
3.如权利要求1所述的一种掺杂锂的镍锌铁氧体材料，其化学式为Ni0.3LixZn0.7-xFe2O4，其中x=0.05~0.1。
4.如权利要求1或2或3所述的一种掺杂锂的镍锌铁氧体材料在制备功率转换器件中的应用。
5.如权利要求1或2或3所述的掺杂锂的镍锌铁氧体材料的制备方法，包括如下步骤：
（1）称取硝酸铁、硝酸镍、硝酸锌、硝酸锂溶于去离子水，充分搅拌后加入柠檬酸，控制柠檬酸与溶液中金属离子的摩尔比为1-2:1-2，继续搅拌0.5~1h；
（2）量取氨水，逐滴加入，搅拌0.5~1h，氨水与柠檬酸的摩尔比为2.5-3.5:0.5-1.5；在90~100℃的油浴中加热至自蔓延燃烧，生成蓬松的棕褐色粉体；
（3）将上述棕褐色粉体置于马弗炉中预烧；预烧升温速率为8~10℃/min，预烧温度为200~400℃，预烧时间为6~12h；
（4）研磨，造粒，压制成型；
（5）将压制好的材料置于马弗炉中烧结，烧结升温速率为5~10℃/min，烧结温度为1000~1300℃，烧结时间为6~8h，得掺杂锂的镍锌铁氧体材料。
6.根据权利要求5所述的掺杂锂的镍锌铁氧体材料的制备方法，其特征在于：步骤（1）中，柠檬酸与溶液中金属离子的摩尔比为1:1。
7.根据权利要求5所述的掺杂锂的镍锌铁氧体材料的制备方法，其特征在于：步骤（2）当中，氨水与柠檬酸的摩尔比为3:1。
8.根据权利要求5所述的掺杂锂的镍锌铁氧体材料的制备方法，其特征在于：步骤（4）中，研磨后的粉体加入含有酚醛环氧树脂的胶水造粒。
9.根据权利要求8所述的掺杂锂的镍锌铁氧体材料的制备方法，其特征在于：步骤（4）中，含有酚醛环氧树脂的胶水为15mL酚醛环氧树脂 F51、10mL固化剂和25mL乙醇的混合溶液。
10.根据权利要求9所述的掺杂锂的镍锌铁氧体材料的制备方法，其特征在于：混合溶液与粉体的比例为5~10%，压制的压力为2~4MPa。
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