CN113603473A - 一种具有高磁导率的Mn-Zn铁氧体滤波材料 - Google Patents

一种具有高磁导率的Mn-Zn铁氧体滤波材料 Download PDF

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CN113603473A
CN113603473A CN202110963501.XA CN202110963501A CN113603473A CN 113603473 A CN113603473 A CN 113603473A CN 202110963501 A CN202110963501 A CN 202110963501A CN 113603473 A CN113603473 A CN 113603473A
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silicon nitride
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CN113603473B (zh
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沈大伟
沈宏江
张学舟
牟大兵
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ANHUI HUALIN MAGNETIC TECHNOLOGY
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Abstract

本发明涉及涉及一种具有高磁导率的Mn‑Zn铁氧体滤波材料，所述滤波材料主成分和辅助成分组成，所述主成分由氧化铁、氧化锌、四氧化三铁组成，所述辅助成分由氧化钼、氧化铌、氧化铌、碳酸钙、氮化硅、钛酸钾组成。本发明通过添加氮化硅以及钛酸钾，不仅能在低频环境下增加滤波材料的磁导率，同时也能增强滤波材料在高频环境下的磁导率，从而实现了铁氧体滤波材料综合性能的提升。

Description

一种具有高磁导率的Mn-Zn铁氧体滤波材料
技术领域
本发明涉及滤波材料技术领域，尤其涉及一种具有高磁导率的Mn-Zn铁氧体滤波材料及其制备方法。
背景技术
锰锌铁氧体作为软磁材料的一种，广泛应用于电力工业设备、家电仪器及信息化技术领域等，是目前产量最大、用量也最大的一种软磁材料，在兆赫兹级别的电子元器件中有着不可替代的作用。随着通信技术和电子产品数字化的发展，对软磁铁氧体和元件提出了新的要求，高性能高磁导率磁芯广泛应用于各类电信及信息用基本材料，如共模滤波器、饱和电感、电流互感器、漏电保护器、绝缘变压器、信号及脉冲变压器等领域得到了广泛应用。现在电子通讯行业需要铁氧体磁芯具有低磁芯损耗和高磁导率，以满足现在电器设备的微型化和高效率的要求，现有的磁芯材料难以满足上述要求。
基于上述情况，本发明提出了一种高强度环氧树脂组合物及其制备方法，可有效解决以上问题。
发明内容
本发明的目的在于提供一种具有高磁导率的Mn-Zn铁氧体滤波材料及其制备方法。
为实现上述目的，本发明提供了一种具有高磁导率的Mn-Zn铁氧体滤波材料，所述滤波材料主成分和辅助成分组成，所述主成分包括52～54mol％氧化铁、20～22mol％氧化锌、24～28mol％四氧化三锰，按主成分总重量计，所述辅助成分包括：400～600ppm氧化钼、100～300ppm氧化铌、300～500ppm氧化铋、200～300ppm碳酸钙。
优选地，所述辅助成分还包括钛酸钾、氮化硅。
优选地，所述辅助成分还包括100～300ppm钛酸钾、200～400ppm氮化硅。
本发明还提供一种具有高磁导率的Mn-Zn铁氧体滤波材料，所述滤波材料主成分和辅助成分组成，所述主成分包括52mol％氧化铁、20mol％氧化锌、28mol％四氧化三锰；按主成分总重量计，所述辅助成分包括100ppm钛酸钾、200ppm氮化硅、400ppm氧化钼、100ppm氧化铌、300ppm氧化铋、200ppm碳酸钙。
优选地，所述滤波材料主成分和辅助成分组成，所述主成分包括53mol％氧化铁、21mol％氧化锌、26mol％四氧化三锰；按主成分总重量计，所述辅助成分包括200ppm钛酸钾、300ppm氮化硅、500ppm氧化钼、200ppm氧化铌、400ppm氧化铋、250ppm碳酸钙。
优选地，所述滤波材料主成分和辅助成分组成，所述主成分包括54mol％氧化铁、22mol％氧化锌、24mol％四氧化三锰；按主成分总重量计，所述辅助成分包括300ppm钛酸钾、400ppm氮化硅、600ppm氧化钼、300ppm氧化铌、500ppm氧化铋、300ppm碳酸钙。
本发明还提供一种上述具有高磁导率的Mn-Zn铁氧体滤波材料的制备方法，所述方法包括以下步骤：
S1：将氧化铁、四氧化三锰和氧化锌加入球磨机进行球磨，球磨机的转速为200～250r/min，球磨时间为2～2.5h，得到混合料A；
S2：将混合料A在860～950℃和空气气氛下进行预烧55～60min，然后冷却至室温得到预烧料B；
S3：将预烧料B、钛酸钾、氮化硅、氧化钼、氧化铌、氧化铋、碳酸钙加入球磨机进行二次球磨，球磨机的转速为200～250r/min，球磨时间为8～8.5h，在80～90℃下烘干22～24h，得到混合料C；
S4：向混合料C中加入聚乙烯醇溶液混合进行喷雾造粒，然后过100～200目筛，得到粉末颗粒；
S5：将粉末颗粒放入环形模具，利用恒载荷压力机进行压制成型，恒载荷压力机施加的载荷为450～500MPa，保压360～400s，得到坯件；
S6：将S5中得到的坯件放入烧结炉，烧结气氛为氧气，在1000℃，压力1.0～1.2MPa条件下保温8.5～9.0h后随炉冷却即得。
优选地，所述S3中，在80～90℃下烘干22～24h。
优选地，所述S6中，从室温以2.5℃/min速率升温至550℃，以1.5℃/min速率升温至700℃，以4℃/min速率升温至最高烧结温度1000℃。
与现有技术相比，本发明具有如下有益效果：
1.本发明通过添加氮化硅以及钛酸钾，不仅能在低频环境下增加滤波材料的磁导率，同时也能增强滤波材料在高频环境下的磁导率，从而实现了铁氧体滤波材料综合性能的提升。
2.本发明原材料在国内充足，价格适宜，使其规模化生产没有太高的成本限制；同时，制备方法简单，总体生产成本不高，有利于工业的大规模生产。
具体实施方式
实施例1
按表1称量具体原料，步骤制备步骤如下：
S1：将氧化铁、四氧化三锰和氧化锌加入球磨机进行球磨，球磨机的转速为200r/min，球磨时间为2.5h，得到混合料A；
S2：将混合料A在860℃和空气气氛下进行预烧55min，然后冷却至室温得到预烧料B；
S3：将预烧料B、钛酸钾、氮化硅、氧化钼、氧化铌、氧化铋、碳酸钙加入球磨机进行二次球磨，球磨机的转速为200r/min，球磨时间为8.5h，在80℃下烘干24h，得到混合料C；
S4：向混合料C中加入适量聚乙烯醇溶液混合进行喷雾造粒，然后过100目筛，得到粉末颗粒；
S5：将粉末颗粒放入环形模具，利用恒载荷压力机进行压制成型，恒载荷压力机施加的载荷为450MPa，保压400s，得到坯件；
S6：将S5中得到的坯件放入烧结炉，烧结气氛为氧气，从室温以2.5℃/min速率升温至450℃，以1.5℃/min速率升温至850℃，以4℃/min速率升温至最高烧结温度1000℃，在压力1.0MPa条件下保温9h后随炉冷却即得。
实施例2
按表1称量具体原料，步骤制备步骤如下：
S1：将氧化铁、四氧化三锰和氧化锌加入球磨机进行球磨，球磨机的转速为250r/min，球磨时间为2h，得到混合料A；
S2：将混合料A在950℃和空气气氛下进行预烧55min，然后冷却至室温得到预烧料B；
S3：将预烧料B、钛酸钾、氮化硅、氧化钼、氧化铌、氧化铋、碳酸钙加入球磨机进行二次球磨，球磨机的转速为250r/min，球磨时间为8～8.5h，在80～90℃下烘干22h，得到混合料C；
S4：向混合料C中加入聚乙烯醇溶液混合进行喷雾造粒，然后过200目筛，得到粉末颗粒；
S5：将粉末颗粒放入环形模具，利用恒载荷压力机进行压制成型，恒载荷压力机施加的载荷为500MPa，保压360s，得到坯件；
S6：将S5中得到的坯件放入烧结炉，烧结气氛为氧气，从室温以2.5℃/min速率升温至550℃，以1.5℃/min速率升温至700℃，以4℃/min速率升温至最高烧结温度1000℃，在压力1.2MPa条件下保温8.5h后随炉冷却即得。
实施例3
按表1称量具体原料，步骤制备步骤如下：
S1：将氧化铁、四氧化三锰和氧化锌加入球磨机进行球磨，球磨机的转速为200r/min，球磨时间为2.5h，得到混合料A；
S2：将混合料A在860℃和空气气氛下进行预烧55min，然后冷却至室温得到预烧料B；
S3：将预烧料B、钛酸钾、氮化硅、氧化钼、氧化铌、氧化铋、碳酸钙加入球磨机进行二次球磨，球磨机的转速为200r/min，球磨时间为8.5h，在80℃下烘干24h，得到混合料C；
S4：向混合料C中加入聚乙烯醇溶液混合进行喷雾造粒，然后过200目筛，得到粉末颗粒；
S5：将粉末颗粒放入环形模具，利用恒载荷压力机进行压制成型，恒载荷压力机施加的载荷为500MPa，保压360s，得到坯件；
S6：将S5中得到的坯件放入烧结炉，烧结气氛为氧气，从室温以2.5℃/min速率升温至550℃，以1.5℃/min速率升温至700℃，以4℃/min速率升温至最高烧结温度1000℃，在压力1.2MPa条件下保温8.5h后随炉冷却即得。
对比例1
按表1称量具体原料，步骤制备步骤如下：
S1：将氧化铁、四氧化三锰和氧化锌加入球磨机进行球磨，球磨机的转速为200r/min，球磨时间为2.5h，得到混合料A；
S2：将混合料A在860℃和空气气氛下进行预烧55min，然后冷却至室温得到预烧料B；
S3：将预烧料B、氧化钼、氧化铌、氧化铋、碳酸钙加入球磨机进行二次球磨，球磨机的转速为200r/min，球磨时间为8.5h，在80℃下烘干24h，得到混合料C；
S4：向混合料C中加入聚乙烯醇溶液混合进行喷雾造粒，然后过200目筛，得到粉末颗粒；
S5：将粉末颗粒放入环形模具，利用恒载荷压力机进行压制成型，恒载荷压力机施加的载荷为500MPa，保压360s，得到坯件；
S6：将S5中得到的坯件放入烧结炉，烧结气氛为氧气，从室温以2.5℃/min速率升温至550℃，以1.5℃/min速率升温至700℃，以4℃/min速率升温至最高烧结温度1000℃，在压力1.2MPa条件下保温8.5h后随炉冷却即得。
表1
物料种类 实施例1 实施例2 实施例3 对比例1 对比例2
氧化铁(mol％) 52 53 54 54 54
氧化锌(mol％) 20 21 22 22 22
四氧化三锰(mol％) 28 26 24 24 24
钛酸钾(ppm) 100 200 300 / 300
氮化硅(ppm) 200 300 400 400 /
氧化钼(ppm) 400 500 600 600 600
氧化铌(ppm) 100 200 300 300 300
氧化铋(ppm) 300 400 500 500 500
碳酸钙(ppm) 200 250 300 300 300
实施例4磁导率测试
使用E4991A型LCR测试仪测试实施例1～3、对比例1、2的磁导率μ，测试结果见表2。
表2磁导率测试结果
频率f 10kHz 100kHz 200kHz 500kHz
实施例1 15641 15550 14285 13632
实施例2 14829 14625 12862 11380
实施例3 14548 13584 12062 11126
对比例1 11362 9328 7483 5972
对比例2 10953 8718 6184 4670
前述对本发明的具体示例性实施方案的描述是为了说明和例证的目的。这些描述并非想将本发明限定为所公开的精确形式，并且很显然，根据上述教导，可以进行很多改变和变化。对示例性实施例进行选择和描述的目的在于解释本发明的特定原理及其实际应用，从而使得本领域的技术人员能够实现并利用本发明的各种不同的示例性实施方案以及各种不同的选择和改变。本发明的范围意在由权利要求书及其等同形式所限定。

Claims (9)

1.一种具有高磁导率的Mn-Zn铁氧体滤波材料，其特征在于，所所述滤波材料主成分和辅助成分组成，所述主成分包括52～54mol％氧化铁、20～22mol％氧化锌、24～28mol％四氧化三锰，按主成分总重量计，所述辅助成分包括：400～600ppm氧化钼、100～300ppm氧化铌、300～500ppm氧化铋、200～300ppm碳酸钙。
2.根据权利要求1所述的铁氧体滤波材料，其特征在于，所述辅助成分还包括钛酸钾、氮化硅。
3.根据权利要求1所述的铁氧体滤波材料，其特征在于，所述辅助成分还包括100～300ppm钛酸钾、200～400ppm氮化硅。
4.根据权利要求3所述的铁氧体滤波材料，其特征在于，所述滤波材料主成分和辅助成分组成，所述主成分包括52mol％氧化铁、20mol％氧化锌、28mol％四氧化三锰；按主成分总重量计，所述辅助成分包括100ppm钛酸钾、200ppm氮化硅、400ppm氧化钼、100ppm氧化铌、300ppm氧化铋、200ppm碳酸钙。
5.根据权利要求3所述的铁氧体滤波材料，其特征在于，所述滤波材料主成分和辅助成分组成，所述主成分包括53mol％氧化铁、21mol％氧化锌、26mol％四氧化三锰；按主成分总重量计，所述辅助成分包括200ppm钛酸钾、300ppm氮化硅、500ppm氧化钼、200ppm氧化铌、400ppm氧化铋、250ppm碳酸钙。
6.根据权利要求3所述的铁氧体滤波材料，其特征在于，所述滤波材料主成分和辅助成分组成，所述主成分包括54mol％氧化铁、22mol％氧化锌、24mol％四氧化三锰；按主成分总重量计，所述辅助成分包括300ppm钛酸钾、400ppm氮化硅、600ppm氧化钼、300ppm氧化铌、500ppm氧化铋、300ppm碳酸钙。
7.一种制备具有高磁导率的Mn-Zn铁氧体滤波材料的方法，其特征在于，所述方法包括以下步骤：
S1：将氧化铁、四氧化三锰和氧化锌加入球磨机进行球磨，球磨机的转速为200～250r/min，球磨时间为2～2.5h，得到混合料A；
S2：将混合料A在860～950℃和空气气氛下进行预烧55～60min，然后冷却至室温得到预烧料B；
S3：将预烧料B、钛酸钾、氮化硅、氧化钼、氧化铌、氧化铋、碳酸钙加入球磨机进行二次球磨，球磨机的转速为200～250r/min，球磨时间为8～8.5h，烘干，得到混合料C；
S4：向混合料C中加入聚乙烯醇溶液混合进行喷雾造粒，然后过100～200目筛，得到粉末颗粒；
S5：将粉末颗粒放入环形模具，利用恒载荷压力机进行压制成型，恒载荷压力机施加的载荷为450～500MPa，保压360～400s，得到坯件；
S6：将S5中得到的坯件放入烧结炉，烧结气氛为氧气，在1000℃，压力1.0～1.2MPa条件下保温8.5～9.0h后随炉冷却即得。
8.根据权利要求7所述的制备方法，其特征在于，所述S3中，在80～90℃下烘干22～24h。
9.根据权利要求7所述的制备方法，其特征在于，所述S6中，从室温以2.5℃/min速率升温至550℃，以1.5℃/min速率升温至700℃，以4℃/min速率升温至最高烧结温度1000℃。
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JPH1187126A (ja) * 1997-07-16 1999-03-30 Tdk Corp フェライトおよびインダクタ
CN101354941A (zh) * 2008-05-16 2009-01-28 广东风华高新科技股份有限公司 一种含镁、镍、锌元素的软磁铁氧体材料及其制造方法
CN101684044A (zh) * 2008-09-25 2010-03-31 Tdk株式会社 MnZnLi系铁氧体
CN103102148A (zh) * 2013-02-19 2013-05-15 常熟市信立磁业有限公司 宽频高磁导率锰-锌铁氧体材料的制备方法

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* Cited by examiner, † Cited by third party
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JPH1187126A (ja) * 1997-07-16 1999-03-30 Tdk Corp フェライトおよびインダクタ
CN101354941A (zh) * 2008-05-16 2009-01-28 广东风华高新科技股份有限公司 一种含镁、镍、锌元素的软磁铁氧体材料及其制造方法
CN101684044A (zh) * 2008-09-25 2010-03-31 Tdk株式会社 MnZnLi系铁氧体
CN103102148A (zh) * 2013-02-19 2013-05-15 常熟市信立磁业有限公司 宽频高磁导率锰-锌铁氧体材料的制备方法

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