CN109626981A - 一种宽温宽频高磁导率锰锌铁氧体及其制备方法 - Google Patents

一种宽温宽频高磁导率锰锌铁氧体及其制备方法 Download PDF

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CN109626981A
CN109626981A CN201910059743.9A CN201910059743A CN109626981A CN 109626981 A CN109626981 A CN 109626981A CN 201910059743 A CN201910059743 A CN 201910059743A CN 109626981 A CN109626981 A CN 109626981A
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柯宇翔
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GUANDA MAGNETIC IND CO Ltd SUZHOU
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Abstract

本发明公开了一种宽温宽频高磁导率锰锌铁氧体及其制备方法，所述铁氧体包括：主成分和辅助成分，所述主成分包括的原料及其质量百分比为：三氧化二铁58%‑65％、氧化锰18%‑25％、氧化锌10%‑20％、氧化铜0.1%‑14％、氧化钴0.1%‑3％；所述辅助成分的组分及其含量为：CaO 250‑500ppm、Bi2O3500‑8000ppm、MoO3400‑800ppm、TiO2250‑700ppm；其制备方法包括：配料、振磨、造球、预烧、黑振、砂磨、加杂、喷雾造粒、混料、成型、烧结。通过上述方式，本发明材料工作温度范围宽、工作频率特性高、磁导率高，能够满足高性能变压器磁芯使用要求。

Description

一种宽温宽频高磁导率锰锌铁氧体及其制备方法
技术领域
本发明涉及锰锌铁氧体领域，特别是涉及一种宽温宽频高磁导率锰锌铁氧体及其制备方法。
背景技术
随着电气产品性能要求的不断提高，要求其变压器在不同宽度环境及不同工作频率下要保持性能稳定，而现有的变压器磁芯使用的软磁铁氧体材料适用的工作温度范围较窄，且工作频率特性低、磁导率低，在使用中不能满足高性能变压器使用要求。
发明内容
本发明主要解决的技术问题是提供一种宽温宽频高磁导率锰锌铁氧体及其制备方法，能够解决现有软磁铁氧体材料因工作温度范围窄、工作频率特性低、磁导率低而不能满足高性能变压器使用要求的问题。
为解决上述技术问题，本发明采用的一个技术方案是：提供一种宽温宽频高磁导率锰锌铁氧体，包括：主成分和辅助成分，所述主成分包括的原料及其质量百分比为：三氧化二铁 58%-65％、氧化锰 18%-25％、氧化锌 10%-20％、氧化铜 0.1%-14％、氧化钴 0.1%-3％；所述辅助成分的组分及其含量为：CaO 250-500ppm、Bi2O3 500-8000ppm、MoO3 400-800ppm、TiO2 250-700ppm。
在本发明一个较佳实施例中，所述主成分包括的原料及其质量百分比为：三氧化二铁 60%-65％、氧化锰 18%-22％、氧化锌 12%-16％、氧化铜 5.5%-10％、氧化钴 0.5%-1.5％。
为解决上述技术问题，本发明采用的另一个技术方案是：提供一种宽温宽频高磁导率锰锌铁氧体的制备方法，包括如下步骤：
（1）配料：称取配方量的三氧化二铁、氧化锰、氧化锌和氧化铜，加入搅拌机中混合20-40分钟，使各原料充分混合至颜色一致；
（2）振磨：将搅拌混合均匀后的原料加入振动研磨机中，振后粒度控制在0.8μm 以下；
（3）造球：将振磨后的原料加入转盘中，同时加入总质量为7-13％的水，混合后制成球料；
（4）预烧：将步骤（3）制得的球料放入天然气回转窑中预烧，预烧完成后磁化度为5％ -8％；
（5）黑振：在密闭无光条件下将步骤（4）预烧后的球料进行振实，黑振后球料粒度控制在1.2μm 以下；
（6）砂磨：将黑振完成后的球料进行砂磨处理，并加入配方量的氧化钴、以及占球料总质量1/2 的水，混合后进行砂磨；其中砂磨时间1-2h，粒度控制在1.0μm 以下；
（7）加杂：向砂磨后的球料加入配方量的辅助成分；
（8）喷雾造粒：对步骤（7）加杂后的球料加入压力式喷雾造粒干燥机内，经过喷雾干燥后得到粉体；
（9）混料：将粉体与润滑剂搅拌混合5-20min 至均匀得到颗粒料；
（10）成型：将颗粒料进行压制成型得到磁芯坯体
（11）烧结：将磁芯坯体转移至烧结设备进行烧结处理，制得所述宽温宽频高磁导率锰锌铁氧体。
在本发明一个较佳实施例中，步骤（2）中所述的研磨机的振动频率设置为30-50Hz。
在本发明一个较佳实施例中，步骤（3）中所述的转盘，设置其转速为30-50rpm，设置其倾角30-35°，待球料的球径成长至3-8mm 时停止转盘运转。
在本发明一个较佳实施例中，步骤（4）中所述的预烧的工艺条件为：在0.5-2h 内从25℃升温至550℃，再在1-2h内从550℃二次升温至950℃，然后在950℃下预烧1-1.5h，最后在1-1.5h内将回转窑温度从950℃降至25℃，其中回转窑的转速控制在3-5rpm，回转窑倾角为2.1°。
在本发明一个较佳实施例中，步骤（8）中所述的压力式喷雾造粒干燥机，设置其进口温度为380℃，出口温度为150℃，泵压为1.8-2.5Kpa。
在本发明一个较佳实施例中，步骤（11）所述的烧结的工艺条件为：采用平衡氧气气氛进行烧结，在700℃-1200℃升温段，控制氧含量＜1.0Vol%，在1200℃开始致密化烧结，最高烧结温度控制在1330℃至1370℃。
本发明的有益效果是：本发明通过优化材料配方，结合特殊的掺杂工艺及烧结工艺曲线，使其材料的磁导率μi常温达12000，频率特性 L(100KHz)/L(1KHz) ≥95%、L(500KHz)/L(1KHz) ≥70%，居里温度Tc达到120以上，同时适合工作温度范围为0±2℃—110±2℃，使该材料能够满足高性能变压器磁芯使用要求。
具体实施方式
下面对本发明的较佳实施例进行详细阐述，以使本发明的优点和特征能更易于被本领域技术人员理解，从而对本发明的保护范围做出更为清楚明确的界定。
本发明实施例包括：
实施例1：
一种宽温宽频高磁导率锰锌铁氧体，包括：主成分和辅助成分，所述主成分包括的原料及其质量百分比为：三氧化二铁 60％、氧化锰 20％、氧化锌 13.5％、氧化铜 5.5％、氧化钴 1％；所述辅助成分的组分及其含量为：CaO 300 ppm、Bi2O3 2000ppm、MoO3 500ppm、TiO2500ppm。
上述宽温宽频高磁导率锰锌铁氧体的制备方法，包括如下步骤：
（1）配料：称取上述配方量的三氧化二铁、氧化锰、氧化锌和氧化铜，加入搅拌机中混合20-40分钟，使各原料充分混合至颜色一致；
（2）振磨：将搅拌混合均匀后的原料加入振动研磨机中，以30Hz 的频率振动研磨，振后粒度控制在0.8μm 以下；
（3）造球：将振磨后的原料加入转盘中，同时加入总质量为10％的水，混合后制成球料；
（4）预烧：将步骤（3）制得的球料放入天然气回转窑中预烧，预烧完成后磁化度为6％；其中所述预烧的工艺条件为：在1h内从25℃升温至550℃，再在1.5h内从550℃二次升温至950℃，然后在950℃下预烧1h，最后在1h内将回转窑温度从950℃降至25℃，并且回转窑的转速控制在3.5rpm，回转窑倾角设置为2.1°；
（5）黑振：在密闭无光条件下将步骤（4）预烧后的球料进行振实，黑振后球料粒度控制在1.2μm 以下；
（6）砂磨：将黑振完成后的球料进行砂磨处理，并加入配方量的氧化钴、以及占球料总质量1/2 的水，混合后进行砂磨；其中砂磨时间1-2h，粒度控制在1.0μm 以下；
（7）加杂：向砂磨后的球料加入配方量的辅助成分；
（8）喷雾造粒：对步骤（7）加杂后的球料加入压力式喷雾造粒干燥机内，设置所述压力式喷雾造粒干燥机进口温度为380℃，出口温度为150℃，泵压为2Kpa，经过喷雾干燥后得到粉体；
（9）混料：将粉体与润滑剂搅拌混合5-20min 至均匀得到颗粒料；
（10）成型：将颗粒料进行压制成型得到磁芯坯体
（11）烧结：将磁芯坯体转移至烧结设备进行烧结处理，制得所述宽温宽频高磁导率锰锌铁氧体，其中所述烧结的工艺条件为：采用平衡氧气气氛进行烧结，在700℃-1200℃升温段，控制氧含量＜1.0Vol%，在1200℃开始致密化烧结，最高烧结温度控制在1350℃。
实施例2：
一种宽温宽频高磁导率锰锌铁氧体，包括：主成分和辅助成分，所述主成分包括的原料及其质量百分比为：三氧化二铁63％、氧化锰18％、氧化锌 12％、氧化铜 6.5％、氧化钴0.5％；所述辅助成分的组分及其含量为：CaO 450 ppm、Bi2O3 6000ppm、MoO3 650ppm、TiO2400ppm。
上述宽温宽频高磁导率锰锌铁氧体的制备方法，包括如下步骤：
（1）配料：称取上述配方量的三氧化二铁、氧化锰、氧化锌和氧化铜，加入搅拌机中混合20-40分钟，使各原料充分混合至颜色一致；
（2）振磨：将搅拌混合均匀后的原料加入振动研磨机中，以40Hz 的频率振动研磨，振后粒度控制在0.8μm 以下；
（3）造球：将振磨后的原料加入转盘中，同时加入总质量为12％的水，混合后制成球料；
（4）预烧：将步骤（3）制得的球料放入天然气回转窑中预烧，预烧完成后磁化度为6％；其中所述预烧的工艺条件为：在1.5h内从25℃升温至550℃，再在2h内从550℃二次升温至950℃，然后在950℃下预烧1h，最后在1.5h内将回转窑温度从950℃降至25℃，并且回转窑的转速控制在4rpm，回转窑倾角设置为2.1°；
（5）黑振：在密闭无光条件下将步骤（4）预烧后的球料进行振实，黑振后球料粒度控制在1.2μm 以下；
（6）砂磨：将黑振完成后的球料进行砂磨处理，并加入配方量的氧化钴、以及占球料总质量1/2 的水，混合后进行砂磨；其中砂磨时间1-2h，粒度控制在1.0μm 以下；
（7）加杂：向砂磨后的球料加入配方量的辅助成分；
（8）喷雾造粒：对步骤（7）加杂后的球料加入压力式喷雾造粒干燥机内，设置所述压力式喷雾造粒干燥机进口温度为380℃，出口温度为150℃，泵压为2.5Kpa，经过喷雾干燥后得到粉体；
（9）混料：将粉体与润滑剂搅拌混合5-20min 至均匀得到颗粒料；
（10）成型：将颗粒料进行压制成型得到磁芯坯体
（11）烧结：将磁芯坯体转移至烧结设备进行烧结处理，制得所述宽温宽频高磁导率锰锌铁氧体，其中所述烧结的工艺条件为：采用平衡氧气气氛进行烧结，在700℃-1200℃升温段，控制氧含量＜1.0Vol%，在1200℃开始致密化烧结，最高烧结温度控制在1370℃。
上述方法得到的宽温宽频高磁导率锰锌铁氧体，工作温度范围宽、工作频率特性高、磁导率高，能够满足高性能变压器磁芯使用要求。其具体性能指标如下：
初始磁导率μi＝12000±30％(1.0KHz，0.3V， 23±3℃)；
适合工作温度 (0±2℃---110±2℃)；
频率特性 L(100KHz)/L(1KHz) ≥95%，L(500KHz)/L(1KHz) ≥70% ；
饱和磁通密度Bs≥380mT(H=1194A/m，25℃)；
居里温度Tc≥120℃。
以上所述仅为本发明的优选实施例而已，并不用于限制本发明，对于本领域的技术人员来说，本发明可以有各种更改和变化。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
以上所述仅为本发明的实施例，并非因此限制本发明的专利范围，凡是利用本发明说明书内容所作的等效结构或等效流程变换，或直接或间接运用在其他相关的技术领域，均同理包括在本发明的专利保护范围内。

Claims (8)

1.一种宽温宽频高磁导率锰锌铁氧体，其特征在于，包括：主成分和辅助成分，所述主成分包括的原料及其质量百分比为：三氧化二铁 58%-65％、氧化锰 18%-25％、氧化锌10%-20％、氧化铜 0.1%-14％、氧化钴 0.1%-3％；所述辅助成分的组分及其含量为：CaO250-500ppm、Bi2O3 500-8000ppm、MoO3 400-800ppm、TiO2 250-700ppm。
2.根据权利要求1所述的宽温宽频高磁导率锰锌铁氧体，其特征在于，所述主成分包括的原料及其质量百分比为：三氧化二铁 60%-65％、氧化锰 18%-22％、氧化锌 12%-16％、氧化铜 5.5%-10％、氧化钴 0.5%-1.5％。
3.一种如权利要求1或2所述的宽温宽频高磁导率锰锌铁氧体的制备方法，其特征在于，包括如下步骤：
（1）配料：称取配方量的三氧化二铁、氧化锰、氧化锌和氧化铜，加入搅拌机中混合20-40分钟，使各原料充分混合至颜色一致；
（2）振磨：将搅拌混合均匀后的原料加入振动研磨机中，振后粒度控制在0.8μm 以下；
（3）造球：将振磨后的原料加入转盘中，同时加入总质量为7-13％的水，混合后制成球料；
（4）预烧：将步骤（3）制得的球料放入天然气回转窑中预烧，预烧完成后磁化度为5％ -8％；
（5）黑振：在密闭无光条件下将步骤（4）预烧后的球料进行振实，黑振后球料粒度控制在1.2μm 以下；
（6）砂磨：将黑振完成后的球料进行砂磨处理，并加入配方量的氧化钴、以及占球料总质量1/2 的水，混合后进行砂磨；其中砂磨时间1-2h，粒度控制在1.0μm 以下；
（7）加杂：向砂磨后的球料加入配方量的辅助成分；
（8）喷雾造粒：对步骤（7）加杂后的球料加入压力式喷雾造粒干燥机内，经过喷雾干燥后得到粉体；
（9）混料：将粉体与润滑剂搅拌混合5-20min 至均匀得到颗粒料；
（10）成型：将颗粒料进行压制成型得到磁芯坯体
（11）烧结：将磁芯坯体转移至烧结设备进行烧结处理，制得所述宽温宽频高磁导率锰锌铁氧体。
4.根据权利要求3所述的宽温宽频高磁导率锰锌铁氧体的制备方法，其特征在于，步骤（2）中所述的研磨机的振动频率设置为30-50Hz。
5.根据权利要求3所述的宽温宽频高磁导率锰锌铁氧体的制备方法，其特征在于，步骤（3）中所述的转盘，设置其转速为30-50rpm，设置其倾角30-35°，待球料的球径成长至3-8mm时停止转盘运转。
6.根据权利要求3所述的宽温宽频高磁导率锰锌铁氧体的制备方法，其特征在于，步骤（4）中所述的预烧的工艺条件为：在0.5-2h 内从25℃升温至550℃，再在1-2h内从550℃二次升温至950℃，然后在950℃下预烧1-1.5h，最后在1-1.5h内将回转窑温度从950℃降至25℃，其中回转窑的转速控制在3-5rpm，回转窑倾角为2.1°。
7.根据权利要求3所述的宽温宽频高磁导率锰锌铁氧体的制备方法，其特征在于，步骤（8）中所述的压力式喷雾造粒干燥机，设置其进口温度为380℃，出口温度为150℃，泵压为1.8-2.5Kpa。
8.根据权利要求3所述的宽温宽频高磁导率锰锌铁氧体的制备方法，其特征在于，步骤（11）所述的烧结的工艺条件为：采用平衡氧气气氛进行烧结，在700℃-1200℃升温段，控制氧含量＜1.0Vol%，在1200℃开始致密化烧结，最高烧结温度控制在1330℃至1370℃。
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