CN111138182A - 一种制备高磁导率锰锌铁氧体的方法 - Google Patents

一种制备高磁导率锰锌铁氧体的方法 Download PDF

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CN111138182A
CN111138182A CN201911415747.2A CN201911415747A CN111138182A CN 111138182 A CN111138182 A CN 111138182A CN 201911415747 A CN201911415747 A CN 201911415747A CN 111138182 A CN111138182 A CN 111138182A
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manganese
zinc ferrite
sintering
ferrite
high magnetic
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瞿德林
沈建元
王久如
王晓祥
李丛俊
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Zhongde Electronics Co ltd
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Abstract

本发明提出了一种制备高磁导率锰锌铁氧体的方法，包括如下步骤：称取氯化锰、硫酸锌、氯化钴、三氯化铁，加入去离子水中配制成混合溶液，向所述混合溶液中加入混合碱溶液，加热反应，过滤，洗涤，干燥，研磨，预烧，即得化学式为MnxZnyCo1‑x‑yFe2O4的钴掺杂锰锌铁氧体；将钴掺杂锰锌铁氧体与CaCO3、Nb2O5、TiO2、ZrO2、Bi2O3混合，球磨，造粒，成型，再进行烧结，将温度升至1250‑1350℃，保温烧结2‑4h，随炉冷却，得到所述磁导率锰锌铁氧体。本发明通过化学共沉淀法对锰锌铁氧体进行有效掺杂，从而大大增强了锰锌铁氧体的磁导性能。

Description

一种制备高磁导率锰锌铁氧体的方法
技术领域
本发明涉及铁氧体的技术领域，尤其涉及一种制备高磁导率锰锌铁氧体的方法。
背景技术
锰锌铁氧体是一种典型的软磁材料，广泛应用于多路通讯、开关电源、变压器磁芯、滤波器、录音和录像的各种记录磁头、信息存储***、医疗诊断、军工和民用的抗电磁干扰材料等。它的基本要求是高磁导率、高饱和磁感应强度、低损耗、低矫顽力和高稳定性等。
目前，我国的锰锌铁氧体工业与国外相比具有较大差距，改善其性能的研究显得既十分重要又非常迫切。
发明内容
基于背景技术存在的技术问题，本发明提出了一种制备高磁导率锰锌铁氧体的方法，通过化学共沉淀法对锰锌铁氧体进行有效掺杂，从而大大增强了锰锌铁氧体的磁导性能。
本发明是通过如下技术方案实现的：
一种制备高磁导率锰锌铁氧体的方法，包括如下步骤：
S1、根据MnxZnyCo1-x-yFe2O4的化学计量配比称取氯化锰、硫酸锌、氯化钴、三氯化铁，加入去离子水中配制成混合溶液，搅拌条件下向所述混合溶液中加入混合碱溶液，加热反应，过滤，洗涤，干燥，研磨，预烧，得到化学式为MnxZnyCo1-x-yFe2O4的钴掺杂锰锌铁氧体；
S2、将S1得到的钴掺杂锰锌铁氧体与CaCO3、Nb2O5、TiO2、ZrO2、Bi2O3混合，球磨，造粒，成型，再进行烧结，在600-800℃的条件下保温烧结1-2h，再升温至1000-1150℃保温烧结1-2h，最后将温度升至1250-1350℃，保温烧结2-4h，随炉冷却，得到所述高磁导率锰锌铁氧体。
优选地，S1中，0.4≤y＜x≤0.5。
优选地，S1中，所述混合碱溶液为体积比为3-5:1-2:2-3的氨水、1，3-丙二胺和三乙醇胺混合溶液，其中，氨水的浓度为25-30wt％。
优选地，S1中，向所述混合溶液中加入混合碱溶液，调节溶液至pH＝8-9。
优选地，S1中，加热反应的温度为40-50℃，时间为0.5-1h。
优选地，S1中，预烧的温度为850-950℃，预烧时间为1-2h。
优选地，S2中，以钴掺杂锰锌铁氧体的质量为基准，CaCO3的加入量为0.1-0.2wt％，Nb2O5的加入量为0.05-0.1wt％，TiO2的加入量为0.1-0.2wt％，ZrO2的加入量为0.01-0.08wt％，Bi2O3的加入量为0.01-0.1wt％。
优选地，S2中，球磨为湿法球磨，球磨时间为2-4h，球磨后的颗粒平均粒径为0.4-0.8μm。
优选地，S2中，造粒的方式为喷雾造粒，造粒所采用的试剂为浓度为8-10wt％的聚乙烯醇溶液。
优选地，S2中，烧结时，以2-3℃\min的升温速率升温到600-800℃。
本发明所述制备高磁导率锰锌铁氧体的方法中，湿法制备的锰锌铁氧体较干法来说不仅工艺简单，而且可以得到钴掺杂的微米级的锰锌铁氧体，初始磁导率较高，晶粒的尺寸较小，均匀性较好。进一步的，本发明中还对钴掺杂锰锌铁氧体进行了其他氧化物的复合掺杂，有利于对锰锌铁氧体的磁导率性能进行进一步改善。
具体实施方式
为便于理解本发明，本发明列举实施例如下。本领域技术人员应该明了，所述实施例仅仅是帮助理解本发明，不应视为对本发明的具体限制。
实施例1
一种制备高磁导率锰锌铁氧体的方法，包括如下步骤：
(1)根据Mn0.48Zn0.5Co0.02Fe2O4的化学计量配比称取氯化锰、硫酸锌、氯化钴、三氯化铁，加入去离子水中配制成混合溶液，搅拌条件下向所述混合溶液中加入混合碱溶液，所述混合碱溶液为体积比为4:1.5:2.5的氨水、1，3-丙二胺和三乙醇胺混合溶液，其中氨水的浓度为28wt％，调节溶液至pH＝9，45℃下加热反应0.8h，过滤，水洗，干燥，研磨，在900℃下预烧1.5h，得到化学式为Mn0.48Zn0.5Co0.02Fe2O4的钴掺杂锰锌铁氧体；
(2)将(1)得到的钴掺杂锰锌铁氧体与CaCO3、Nb2O5、TiO2、ZrO2、Bi2O3混合，以钴掺杂锰锌铁氧体的质量为基准，CaCO3的加入量为0.15wt％，Nb2O5的加入量为0.08wt％，TiO2的加入量为0.15wt％，ZrO2的加入量为0.05wt％，Bi2O3的加入量为0.05wt％，球磨6h，直至颗粒的平均粒径为0.9μm，烘干后加入浓度为9wt％的聚乙烯醇溶液进行喷雾造粒，聚乙烯醇溶液的加入量是烘干料重量的12％，压制成型，再进行烧结，以2.5℃\min的升温速率升温到700℃，在700℃的条件下保温烧结1.5h，再升温至1100℃保温烧结1.5h，最后将温度升至1300℃，保温烧结3h，随炉冷却，得到所述高磁导率锰锌铁氧体。
实施例2
一种制备高磁导率锰锌铁氧体的方法，包括如下步骤：
(1)根据Mn0.4Zn0.48Co0.02Fe2O4的化学计量配比称取氯化锰、硫酸锌、氯化钴、三氯化铁，加入去离子水中配制成混合溶液，搅拌条件下向所述混合溶液中加入混合碱溶液，所述混合碱溶液为体积比为3:2:2的氨水、1，3-丙二胺和三乙醇胺混合溶液，其中氨水的浓度为25wt％，调节溶液至pH＝9，40℃下加热反应1h，过滤，水洗，干燥，研磨，在850℃下预烧2h，得到化学式为Mn0.4Zn0.48Co0.02Fe2O4的钴掺杂锰锌铁氧体；
(2)将(1)得到的钴掺杂锰锌铁氧体与CaCO3、Nb2O5、TiO2、ZrO2、Bi2O3混合，以钴掺杂锰锌铁氧体的质量为基准，CaCO3的加入量为0.2wt％，Nb2O5的加入量为0.05wt％，TiO2的加入量为0.2wt％，ZrO2的加入量为0.01wt％，Bi2O3的加入量为0.1wt％，球磨4h，直至颗粒的平均粒径为1.0μm，烘干后加入浓度为8wt％的聚乙烯醇溶液进行喷雾造粒，聚乙烯醇溶液的加入量是烘干料重量的13％，压制成型，再进行烧结，以3℃\min的升温速率升温到600℃，在600℃的条件下保温烧结2h，再升温至1150℃保温烧结1h，最后将温度升至1350℃，保温烧结2h，随炉冷却，得到所述高磁导率锰锌铁氧体。
实施例3
一种制备高磁导率锰锌铁氧体的方法，包括如下步骤：
(1)根据Mn0.4Zn0.5Co0.01Fe2O4的化学计量配比称取氯化锰、硫酸锌、氯化钴、三氯化铁，加入去离子水中配制成混合溶液，搅拌条件下向所述混合溶液中加入混合碱溶液，所述混合碱溶液为体积比为5:1:3的氨水、1，3-丙二胺和三乙醇胺混合溶液，其中氨水的浓度为30wt％，调节溶液至pH＝8，50℃下加热反应0.5h，过滤，水洗，干燥，研磨，在950℃下预烧1h，得到化学式为Mn0.4Zn0.5Co0.01Fe2O4的钴掺杂锰锌铁氧体；
(2)将(1)得到的钴掺杂锰锌铁氧体与CaCO3、Nb2O5、TiO2、ZrO2、Bi2O3混合，以钴掺杂锰锌铁氧体的质量为基准，CaCO3的加入量为0.1wt％，Nb2O5的加入量为0.1wt％，TiO2的加入量为0.1wt％，ZrO2的加入量为0.08wt％，Bi2O3的加入量为0.01wt％，球磨8h，直至颗粒的平均粒径为0.8μm，烘干后加入浓度为10wt％的聚乙烯醇溶液进行喷雾造粒，聚乙烯醇溶液的加入量是烘干料重量的14％，压制成型，再进行烧结，以2℃\min的升温速率升温到800℃，在800℃的条件下保温烧结1h，再升温至1000℃保温烧结2h，最后将温度升至1250℃，保温烧结4h，随炉冷却，得到所述高磁导率锰锌铁氧体。
实施例4
一种制备高磁导率锰锌铁氧体的方法，包括如下步骤：
(1)根据Mn0.43Zn0.49Co0.08Fe2O4的化学计量配比称取氯化锰、硫酸锌、氯化钴、三氯化铁，加入去离子水中配制成混合溶液，搅拌条件下向所述混合溶液中加入混合碱溶液，所述混合碱溶液为体积比为4:1:3的氨水、1，3-丙二胺和三乙醇胺混合溶液，其中氨水的浓度为30wt％，调节溶液至pH＝8，50℃下加热反应0.5h，过滤，水洗，干燥，研磨，在900℃下预烧2h，得到化学式为Mn0.43Zn0.49Co0.08Fe2O4的钴掺杂锰锌铁氧体；
(2)将(1)得到的钴掺杂锰锌铁氧体与CaCO3、Nb2O5、TiO2、ZrO2、Bi2O3混合，以钴掺杂锰锌铁氧体的质量为基准，CaCO3的加入量为0.16wt％，Nb2O5的加入量为0.07wt％，TiO2的加入量为0.15wt％，ZrO2的加入量为0.05wt％，Bi2O3的加入量为0.06wt％，球磨5h，直至颗粒的平均粒径为1.0μm，烘干后加入浓度为9wt％的聚乙烯醇溶液进行喷雾造粒，聚乙烯醇溶液的加入量是烘干料重量的15％，压制成型，再进行烧结，以3℃\min的升温速率升温到700℃，在700℃的条件下保温烧结1.5h，再升温至1050℃保温烧结2h，最后将温度升至1300℃，保温烧结3h，随炉冷却，得到所述高磁导率锰锌铁氧体。
对比例1
一种制备锰锌铁氧体的方法，包括如下步骤：
(1)按照Fe2O3:ZnO:MnO摩尔比为50:25:24分别称取Fe2O3、ZnO、MnO，研磨，在900℃下预烧1.5h，得到预烧料；
(2)将(1)得到的预烧料与CoO、CaCO3、Nb2O5、TiO2、ZrO2、Bi2O3混合，以预烧料的质量为基准，CoO的加入量为0.64wt％，CaCO3的加入量为0.15wt％，Nb2O5的加入量为0.08wt％，TiO2的加入量为0.15wt％，ZrO2的加入量为0.05wt％，Bi2O3的加入量为0.05wt％，球磨6h，直至颗粒的平均粒径为0.9μm，烘干后加入浓度为9wt％的聚乙烯醇溶液进行喷雾造粒，聚乙烯醇溶液的加入量是烘干料重量的12％，压制成型，再进行烧结，以2.5℃\min的升温速率升温到700℃，在700℃的条件下保温烧结1.5h，再升温至1100℃保温烧结1.5h，最后将温度升至1300℃，保温烧结3h，随炉冷却，得到所述磁导率锰锌铁氧体。
性能测试：将上述实施例1-4和对比例1中得到的锰锌铁氧体材料成品进行电性能测试，结果如下表所示：
Figure BDA0002351149440000061
以上所述，仅为本发明较佳的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明的技术范围内，根据本发明的技术方案及其发明加以等同替换或改变，都应涵盖在本发明的保护范围之内。

Claims (10)

1.一种制备高磁导率锰锌铁氧体的方法，其特征在于，包括如下步骤：
S1、根据MnxZnyCo1-x-yFe2O4的化学计量配比称取氯化锰、硫酸锌、氯化钴、三氯化铁，加入去离子水中配制成混合溶液，搅拌条件下向所述混合溶液中加入混合碱溶液，加热反应，过滤，洗涤，干燥，研磨，预烧，得到化学式为MnxZnyCo1-x-yFe2O4的钴掺杂锰锌铁氧体；
S2、将S1得到的钴掺杂锰锌铁氧体与CaCO3、Nb2O5、TiO2、ZrO2、Bi2O3混合，球磨，造粒，成型，再进行烧结，在600-800℃的条件下保温烧结1-2h，再升温至1000-1150℃保温烧结1-2h，最后将温度升至1250-1350℃，保温烧结2-4h，随炉冷却，得到所述高磁导率锰锌铁氧体。
2.根据权利要求1所述制备高磁导率锰锌铁氧体的方法，其特征在于，S1中，0.4≤y＜x≤0.5。
3.根据权利要求1或2所述制备高磁导率锰锌铁氧体的方法，其特征在于，S1中，所述混合碱溶液为体积比为3-5:1-2:2-3的氨水、1，3-丙二胺和三乙醇胺混合溶液，其中，氨水的浓度为25-30wt％。
4.根据权利要求1-3任一项所述制备高磁导率锰锌铁氧体的方法，其特征在于，S1中，向所述混合溶液中加入混合碱溶液，调节溶液至pH＝8-9。
5.根据权利要求1-4任一项所述制备高磁导率锰锌铁氧体的方法，其特征在于，S1中，加热反应的温度为40-50℃，时间为0.5-1h。
6.根据权利要求1-5任一项所述制备高磁导率锰锌铁氧体的方法，其特征在于，S1中，预烧的温度为850-950℃，预烧时间为1-2h。
7.根据权利要求1-6任一项所述制备高磁导率锰锌铁氧体的方法，其特征在于，S2中，以钴掺杂锰锌铁氧体的质量为基准，CaCO3的加入量为0.1-0.2wt％，Nb2O5的加入量为0.05-0.1wt％，TiO2的加入量为0.1-0.2wt％，ZrO2的加入量为0.01-0.08wt％，Bi2O3的加入量为0.01-0.1wt％。
8.根据权利要求1-7任一项所述制备高磁导率锰锌铁氧体的方法，其特征在于，S2中，球磨为湿法球磨，球磨时间为2-4h，球磨后的颗粒平均粒径为0.4-0.8μm。
9.根据权利要求1-8任一项所述制备高磁导率锰锌铁氧体的方法，其特征在于，S2中，造粒的方式为喷雾造粒，造粒所采用的试剂为浓度为8-10wt％的聚乙烯醇溶液。
10.根据权利要求1-9任一项所述制备高磁导率锰锌铁氧体的方法，其特征在于，S2中，烧结时，以2-3℃\min的升温速率升温到600-800℃。
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