CN111116190A - 一种高电磁性能的锰锌铁氧体及其制备方法 - Google Patents

一种高电磁性能的锰锌铁氧体及其制备方法 Download PDF

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CN111116190A
CN111116190A CN201911415911.XA CN201911415911A CN111116190A CN 111116190 A CN111116190 A CN 111116190A CN 201911415911 A CN201911415911 A CN 201911415911A CN 111116190 A CN111116190 A CN 111116190A
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temperature
manganese
heating
sintering
high electromagnetic
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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

本发明公开了一种高电磁性能的锰锌铁氧体及其制备方法，所述锰锌铁氧体的主成分为：Fe2O3 69‑72wt％，Mn3O4 18‑22wt％，其余为ZnO；在主成分基础上掺杂氧化物为：CaCO3 0.08‑0.12wt％，Nb2O5 0.01‑0.08wt％，Ta2O5 0.01‑0.08wt％，Co2O3 0.1‑0.3wt％，TiO2 0.02‑0.08wt％，ZrO2 0.008‑0.02wt％，V2O5 0.08‑0.12wt％中的至少一种。本发明通过主料和掺杂氧化物之间的相互配合，并优化制备工艺，从而提升了锰锌铁氧体的电磁性能。

Description

一种高电磁性能的锰锌铁氧体及其制备方法
技术领域
本发明涉及锰锌磁铁氧体技术领域，尤其涉及一种高电磁性能的锰锌铁氧体及其制备方法。
背景技术
铁氧体在应用上一般是作为磁性介质材料被加以利用的，是由铁以及其他一种或者多种相应的金属元素通过复合氧化的方法得到的，因此它在早期也被称为铁淦氧。日、德等国家自20世纪30年代以来就开始对铁氧体进行了非常系统的研究并加以生产，发展十分迅猛，现在在无线电、通讯、雷达导航、宇宙飞行、自动控制等诸多领域都实现了非常广泛的利用。
锰锌铁氧体具有高起始磁导率、高饱和磁通密度(Bs)、高电阻率、低损耗等优点，因此被广泛地应用于电子设备，如：宽带脉冲变压器、轭流线圈、噪音滤波器和记录磁头等。另外，由锰锌铁氧体制成的变压器磁芯，在计算机、彩电、录像机及其他电子设备的开关电源中也得到了广泛地应用。在航天、舰艇等国防武器装备系统和民用家电仪器仪表等关乎国计民生的众多部门，特别在是现代通信设备的户外设施，如中继器、增音机、微波接力站、海底光缆系统的水下设备等领域，软磁锰锌铁氧体材料也有着极为重要的应用。
随着锰锌铁氧体应用范围的日益增大以及电子信息产业的高速发展，对锰锌铁氧体的性能要求也越来越高。然而，功率铁氧体应用领域的日益拓展同样也预示着高电磁性能的锰锌铁氧体的开发之路仍很长。
发明内容
本发明提出了一种高电磁性能的锰锌铁氧体及其制备方法，通过主料和掺杂氧化物之间的相互配合，并优化制备工艺，从而提升了锰锌铁氧体的电磁性能。
本发明提出的一种高电磁性能的锰锌铁氧体，主成分为：Fe2O3 69-72wt％，Mn3O418-22wt％，其余为ZnO；在主成分基础上掺杂氧化物为：CaCO3 0.08-0.12wt％，Nb2O5 0.01-0.08wt％，Ta2O5 0.01-0.08wt％，Co2O3 0.1-0.3wt％，TiO2 0.02-0.08wt％，ZrO2 0.008-0.02wt％，V2O5 0.08-0.12wt％中的至少一种。
本发明还提出了一种高电磁性能的锰锌铁氧体的制备方法，包括如下步骤：
S1、按主成分：Fe2O3 69-72wt％，Mn3O4 18-22wt％，其余为ZnO进行配料，一次球磨混合后，预烧后，再加入掺杂氧化物：CaCO3 0.08-0.12wt％，Nb2O5 0.01-0.08wt％，Ta2O50.01-0.08wt％，Co2O3 0.1-0.3wt％，TiO2 0.02-0.08wt％，ZrO2 0.008-0.02wt％，V2O50.08-0.12wt％中的至少一种，二次球磨混合，造粒，成型，得到胚料；
S2、将胚料升温至烧结温度，进行保温烧结，得到所述高电磁性能的锰锌铁氧体，其中烧结过程控制如下：从室温升温至800℃，升温速度为120-160℃/h，空气气氛；从800℃升温至1200℃，升温速度为200-300℃/h，氧分压为0.005-0.01％；从1200℃升温至1250℃，升温速度为30-80℃/h，氧分压为0.5-1％；从1250℃升温至1370℃的烧结温度，升温速度为100-150℃/h，氧分压为1-3％；烧结温度为1370℃，保温2-6h，氧分压为2-8％；保温结束后降温至1250℃，降温速度为100-200℃/h，氧分压为0.5-2％；从1250℃开始快速降温，降温速度为400-500℃/h，氧含量为0.01％以下。
优选地，S1中，所述一次球磨和二次球磨都为湿法球磨。
优选地，S1中，一次球磨时，球磨时间为2-4h；二次球磨时，球磨时间为4-8h，球磨后的颗粒平均粒径为0.8-1.0μm。
优选地，S1中，预烧温度为850-950℃，预烧时间为1-2h。
优选地，S1中，造粒的方式为喷雾造粒，造粒所采用的试剂为浓度为8-9wt％的聚乙烯醇溶液。
优选地，造粒后的颗粒分布为：60目以上≤30％200目以上≤3％。
优选地，S1中，成型后的胚料密度为3.00-3.15g/cm3。
本发明以Fe2O3、Mn3O4、ZnO作为主成分，控制三者合理配比，并加入CaCO3、Nb2O5等作为掺杂氧化物，促进铁氧体的传质和烧结，加速晶粒生长，进一步的，通过烧结阶段的温度控制，保证了铁氧体的内部晶粒在烧结过程中均匀细化，晶粒规则化，减少了晶界缺陷，大大提高了铁氧体材料的电磁性能。
具体实施方式
下面，通过具体实施例对本发明的技术方案进行详细说明。
实施例1
一种高电磁性能的锰锌铁氧体，主成分为：Fe2O3 70wt％，Mn3O4 20wt％，其余为ZnO；在主成分基础上掺杂氧化物为：CaCO3 0.1wt％，Nb2O5 0.05wt％，Ta2O5 0.04wt％，Co2O3 0.2wt％，TiO2 0.05wt％，ZrO2 0.014wt％，V2O5 0.1wt％；
由如下步骤制得：
(1)按主成分：Fe2O3 70wt％，Mn3O4 20wt％，其余为ZnO进行原材料配料，再将所称原材料混合放入球磨罐中，进行第一次湿法球磨，球磨时间为3h，使其充分混合均匀；将球磨好的混合料放入烘箱中烘干，再放入炉中预烧1.5h，预烧温度为900℃，得到预烧料；
(2)以预烧料总重为100wt％，在预烧料中加入掺杂氧化物：CaCO3 0.1wt％，Nb2O50.05wt％，Ta2O5 0.04wt％，Co2O3 0.2wt％，TiO2 0.05wt％，ZrO2 0.014wt％，V2O5 0.1wt％，进行第二次湿法球磨，球磨时间为6h，直至颗粒的平均粒径为0.9μm，放入烘箱中烘干；
(3)向烘干料中加入浓度为8wt％的聚乙烯醇溶液，聚乙烯醇溶液的加入量是烘干料重量的12％，喷雾造粒，制成颗粒后的颗粒分布为：60目以上≤30％200目以上≤3％，将该颗粒压制成型，得到为密度为3.12g/cm3的坯料；
(4)将胚料升温至烧结温度，进行保温烧结，得到所述高电磁性能的锰锌铁氧体，其中烧结过程控制如下：从室温升温至800℃，升温速度为140℃/h，空气气氛；从800℃升温至1200℃，升温速度为250℃/h，氧分压为0.008％；从1200℃升温至1250℃，升温速度为50℃/h，氧分压为0.7％；从1250℃升温至1370℃的烧结温度，升温速度为120℃/h，氧分压为2％；烧结温度为1370℃，保温4h，氧分压为5％；保温结束后降温至1250℃，降温速度为150℃/h，氧分压为1.2％；从1250℃开始快速降温，降温速度为450℃/h，氧含量为0.01％以下。
实施例2
一种高电磁性能的锰锌铁氧体，主成分为：Fe2O3 69wt％，Mn3O4 22wt％，其余为ZnO；在主成分基础上掺杂氧化物为：CaCO3 0.08wt％，Nb2O5 0.08wt％，Ta2O5 0.01wt％，Co2O3 0.3wt％，TiO2 0.02wt％，ZrO2 0.02wt％，V2O5 0.08wt％；
由如下步骤制得：
(1)按主成分：Fe2O3 69wt％，Mn3O4 22wt％，其余为ZnO进行原材料配料，再将所称原材料混合放入球磨罐中，进行第一次湿法球磨，球磨时间为2h，使其充分混合均匀；将球磨好的混合料放入烘箱中烘干，再放入炉中预烧2h，预烧温度为850℃，得到预烧料；
(2)以预烧料总重为100wt％，在预烧料中加入掺杂氧化物：CaCO3 0.08wt％，Nb2O50.08wt％，Ta2O5 0.01wt％，Co2O3 0.3wt％，TiO2 0.02wt％，ZrO2 0.02wt％，V2O5 0.08wt％，进行第二次湿法球磨，球磨时间8h，直至颗粒的平均粒径为0.8μm，放入烘箱中烘干；
(3)向烘干料中加入浓度为9wt％的聚乙烯醇溶液，聚乙烯醇溶液的加入量是烘干料重量的10％，喷雾造粒，制成颗粒后的颗粒分布为：60目以上≤30％200目以上≤3％，将该颗粒压制成型，得到为密度为3.15g/cm3的坯料；
(4)将胚料升温至烧结温度，进行保温烧结，得到所述高电磁性能的锰锌铁氧体，其中烧结过程控制如下：从室温升温至800℃，升温速度为120℃/h，空气气氛；从800℃升温至1200℃，升温速度为300℃/h，氧分压为0.005％；从1200℃升温至1250℃，升温速度为80℃/h，氧分压为0.5％；从1250℃升温至1370℃的烧结温度，升温速度为150℃/h，氧分压为1％；烧结温度为1370℃，保温6h，氧分压为2％；保温结束降温至1250℃，降温速度为200℃/h，氧分压为0.5％；从1250℃开始快速降温，降温速度为500℃/h，氧含量为0.01％以下。
实施例3
一种高电磁性能的锰锌铁氧体，主成分为：Fe2O3 72wt％，Mn3O4 18wt％，其余为ZnO；在主成分基础上掺杂氧化物为：CaCO3 0.12wt％，Nb2O5 0.01wt％，Ta2O5 0.08wt％，Co2O3 0.1wt％，TiO2 0.08wt％，ZrO2 0.008wt％，V2O5 0.12wt％；
由如下步骤制得：
(1)按主成分：Fe2O3 72wt％，Mn3O4 18wt％，其余为ZnO进行原材料配料，再将所称原材料混合放入球磨罐中，进行第一次湿法球磨，球磨时间4h，使其充分混合均匀；将球磨好的混合料放入烘箱中烘干，再放入炉中预烧1h，预烧温度为950℃，得到预烧料；
(2)以预烧料总重为100wt％，在预烧料中加入掺杂氧化物：CaCO3 0.12wt％，Nb2O50.01wt％，Ta2O5 0.08wt％，Co2O3 0.1wt％，TiO2 0.08wt％，ZrO2 0.008wt％，V2O50.12wt％，进行第二次湿法球磨，球磨时间4h，直至颗粒的平均粒径为1.0μm，放入烘箱中烘干；
(3)向烘干料中加入浓度为8wt％的聚乙烯醇溶液，聚乙烯醇溶液的加入量是烘干料重量的15％，喷雾造粒，制成颗粒后的颗粒分布为：60目以上≤30％200目以上≤3％，将该颗粒压制成型，得到为密度为3.00g/cm3的坯料；
(4)将胚料升温至烧结温度，进行保温烧结，得到所述高电磁性能的锰锌铁氧体，其中烧结过程控制如下：从室温升温至800℃，升温速度为160℃/h，空气气氛；从800℃升温至1200℃，升温速度为200℃/h，氧分压为0.01％；从1200℃升温至1250℃，升温速度为30℃/h，氧分压为1％；从1250℃升温至1370℃的烧结温度，升温速度为100℃/h，氧分压为3％；烧结温度为1370℃，保温2h，氧分压为8％；保温结束后降温至1250℃，降温速度为100℃/h，氧分压为2％；从1250℃开始快速降温，降温速度为400℃/h，氧含量为0.01％以下。
实施例4
一种高电磁性能的锰锌铁氧体，主成分为：Fe2O3 71wt％，Mn3O4 21wt％，其余为ZnO；在主成分基础上掺杂氧化物为：CaCO3 0.1wt％，Nb2O5 0.04wt％；
由如下步骤制得：
(1)按主成分：Fe2O3 71wt％，Mn3O4 21wt％，其余为ZnO进行原材料配料，再将所称原材料混合放入球磨罐中，进行第一次湿法球磨，球磨时间为3h，使其充分混合均匀；将球磨好的混合料放入烘箱中烘干，再放入炉中预烧1.5h，预烧温度为900℃，得到预烧料；
(2)以预烧料总重为100wt％，在预烧料中加入掺杂氧化物：CaCO3 0.1wt％，Nb2O50.04wt％，进行第二次湿法球磨，球磨时间为5h，直至颗粒的平均粒径为1.0μm，放入烘箱中烘干；
(3)向烘干料中加入浓度为9wt％的聚乙烯醇溶液，聚乙烯醇溶液的加入量是烘干料重量的13％，喷雾造粒，制成颗粒后的颗粒分布为：60目以上≤30％200目以上≤3％，将该颗粒压制成型，得到为密度为3.15g/cm3的坯料；
(4)将胚料升温至烧结温度，进行保温烧结，得到所述高电磁性能的锰锌铁氧体，其中烧结过程控制如下：从室温升温至800℃，升温速度为150℃/h，空气气氛；从800℃升温至1200℃，升温速度为280℃/h，氧分压为0.006％；从1200℃升温至1250℃，升温速度为60℃/h，氧分压为0.8％；从1250℃升温至1370℃的烧结温度，升温速度为130℃/h，氧分压为1.5％；烧结温度为1370℃，保温3h，氧分压为4％；保温结束后降温至1250℃，降温速度为160℃/h，氧分压为1.5％；从1250℃开始快速降温，降温速度为450℃/h，氧含量为0.01％以下。
性能测试：将上述实施例1-4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 BDA0002351177770000071
Figure BDA0002351177770000081
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揭露的技术范围内，根据本发明的技术方案及其发明构思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 (8)

1.一种高电磁性能的锰锌铁氧体，其特征在于，主成分为：Fe2O3 69-72wt％，Mn3O4 18-22wt％，其余为ZnO；在主成分基础上掺杂氧化物为：CaCO30.08-0.12wt％，Nb2O5 0.01-0.08wt％，Ta2O5 0.01-0.08wt％，Co2O3 0.1-0.3wt％，TiO20.02-0.08wt％，ZrO2 0.008-0.02wt％，V2O5 0.08-0.12wt％中的至少一种。
2.一种高电磁性能的锰锌铁氧体的制备方法，其特征在于，包括如下步骤：
S1、按主成分：Fe2O3 69-72wt％，Mn3O4 18-22wt％，其余为ZnO进行配料，一次球磨混合后，预烧，再加入掺杂氧化物：CaCO3 0.08-0.12wt％，Nb2O50.01-0.08wt％，Ta2O5 0.01-0.08wt％，Co2O3 0.1-0.3wt％，TiO2 0.02-0.08wt％，ZrO20.008-0.02wt％，V2O5 0.08-0.12wt％中的至少一种，二次球磨混合，造粒，成型，得到胚料；
S2、将胚料升温至烧结温度进行保温烧结，得到所述高电磁性能的锰锌铁氧体，其中烧结过程控制如下：从室温升温至800℃，升温速度为120-160℃/h，空气气氛；从800℃升温至1200℃，升温速度为200-300℃/h，氧分压为0.005-0.01％；从1200℃升温至1250℃，升温速度为30-80℃/h，氧分压为0.5-1％；从1250℃升温至1370℃的烧结温度，升温速度为100-150℃/h，氧分压为1-3％；烧结温度为1370℃，保温2-6h，氧分压为2-8％；保温结束后降温至1250℃，降温速度为100-200℃/h，氧分压为0.5-2％；从1250℃开始快速降温，降温速度为400-500℃/h，氧含量为0.01％以下。
3.根据权利要求2所述高电磁性能的锰锌铁氧体的制备方法，其特征在于，S1中，所述一次球磨和二次球磨都为湿法球磨。
4.根据权利要求3所述高电磁性能的锰锌铁氧体的制备方法，其特征在于，S1中，一次球磨时，球磨时间为2-4h；二次球磨时，球磨时间为4-8h，球磨后的颗粒平均粒径为0.8-1.0μm。
5.根据权利要求2-4任一项所述高电磁性能的锰锌铁氧体的制备方法，其特征在于，S1中，预烧温度为850-950℃，预烧时间为1-2h。
6.根据权利要求2-5任一项所述高电磁性能的锰锌铁氧体的制备方法，其特征在于，S1中，造粒的方式为喷雾造粒，造粒所采用的试剂为浓度为8-9wt％的聚乙烯醇溶液。
7.根据权利要求6所述高电磁性能的锰锌铁氧体的制备方法，其特征在于，S 1中，造粒后的颗粒分布为：60目以上≤30％200目以上≤3％。
8.根据权利要求2-7任一项所述高电磁性能的锰锌铁氧体的制备方法，其特征在于，S1中，成型后的胚料密度为3.00-3.15g/cm3。
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112851328A (zh) * 2021-03-30 2021-05-28 横店集团东磁股份有限公司 一种锰锌铁氧体、其制备方法及用途

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1793020A (zh) * 2005-11-17 2006-06-28 上海交通大学 高性能低功耗锰锌铁氧体材料及其制备方法
CN108275992A (zh) * 2018-01-18 2018-07-13 常熟市三佳磁业有限公司 宽温低功耗高磁导率锰锌铁氧体材料及其制备方法
CN109851347A (zh) * 2018-12-31 2019-06-07 天长市中德电子有限公司 一种锰锌铁氧体及其制备方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1793020A (zh) * 2005-11-17 2006-06-28 上海交通大学 高性能低功耗锰锌铁氧体材料及其制备方法
CN108275992A (zh) * 2018-01-18 2018-07-13 常熟市三佳磁业有限公司 宽温低功耗高磁导率锰锌铁氧体材料及其制备方法
CN109851347A (zh) * 2018-12-31 2019-06-07 天长市中德电子有限公司 一种锰锌铁氧体及其制备方法

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
夏德贵: "《软磁铁氧体制造原理与技术》", 31 December 2010, 陕西科学技术出版社 *
杨潇斐: "ZrO2添加对MnZn 铁氧体磁性能温度特性的影响", 《磁性材料及器件》 *
田民波: "《磁性材料》", 30 April 2001, 清华大学出版社 *
邹姝颖: "V2O5掺杂改善锰锌铁氧体组织及性能的研究", 《电子元件与材料》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112851328A (zh) * 2021-03-30 2021-05-28 横店集团东磁股份有限公司 一种锰锌铁氧体、其制备方法及用途

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