CN114560690A - 自偏置环行器用高矫顽力m型钡铁氧体致密化技术 - Google Patents

自偏置环行器用高矫顽力m型钡铁氧体致密化技术 Download PDF

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CN114560690A
CN114560690A CN202210310182.7A CN202210310182A CN114560690A CN 114560690 A CN114560690 A CN 114560690A CN 202210310182 A CN202210310182 A CN 202210310182A CN 114560690 A CN114560690 A CN 114560690A
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张涛
蒋晓娜
余忠
邬传健
孙科
兰中文
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University of Electronic Science and Technology of China
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Abstract

本发明提供了一种具有高矫顽力和高密度的六角铁氧体及制备方法。在保证材料矫顽力的同时，通过掺杂2.5％Bi2O3、2.0％CuO和0.1％～1.0％V2O5来提高M型钡铁氧体密度，结合湿法磁场成型工艺制备生坯，再结合优化的烧结工艺，最终制备的M型六角铁氧体材料。其特征在于，矫顽力大于2200Oe，密度达到5.14g/cm3。

Description

自偏置环行器用高矫顽力M型钡铁氧体致密化技术
技术领域
本技术属于铁氧体材料制备技术领域，特别涉及自偏置环行器用高剩磁比的M型六角铁氧体材料及制备技术。
背景技术
铁氧体环行器基板所使用材料分为尖晶石型、石榴石型及磁铅石型三种。而传统的微波铁氧体环行器由尖晶石或石榴石材料制成，而这类环行器通常需要外加永磁体来提供一个偏置磁场，所需永磁体体积随器件工作频率的增加而增大，这将极大地增加环行器的体积和质量，不利于小型化和集成化的发展。而磁铅石型的六角铁氧体具有较高的各向异性场，可为环行器的铁氧体基板提供一个自偏置场，因此可将环行器的磁钢减小，甚至完全去除，这对于实现环行器的小型化和片式化具有重要意义。采用具有高剩磁的六角铁氧体材料进行制备铁氧体基板，可减小外置磁钢尺寸，甚至完全去除磁钢。由于高矫顽力是保证高剩磁的前提，但为了保证高矫顽力通常使材料在较低温度下进行烧结，这导致材料的气孔率较高，难以致密化，这会降低铁氧体基板上图形化薄膜的附着力。
本发明提供了一种具有高矫顽力和高密度的六角铁氧体及制备方法。通过掺杂剂配方控制材料的成分，结合湿法磁场成型工艺制备生坯，再结合优化的烧结工艺，最终制备的M型六角铁氧体材料。其特征在于，矫顽力大于2300Oe，密度达到5.17g/cm3。
发明内容
本发明主要针对自偏置环行器用六角铁氧体材料高致密度和高矫顽力难以兼顾的问题，提供一种高矫顽力和高致密度的六角永磁铁氧体材料及其制备方法。
本发明的高矫顽力和高密度铁氧体材料制备方法包括以下步骤：
1、配方
原材料选取按质量百分比，以氧化物计算，称取15.27wt％BaCO3、3.12wt％La2O3、80.07wt％Fe2O3、其余为CuO原料；
2、一次球磨
将上述料粉在球磨机内混合均匀，球磨时间为10～12小时；
3、预烧
将步骤2所得球磨料烘干，在1100℃预烧2～4小时；
4、掺杂
将步骤3所得粉料按重量比加入以下掺杂剂：2.5％Bi2O3、2.0％CuO和0.10％～0.20％V2O5；
5、二次球磨
将步骤4中得到的料粉在球磨机中球磨18小时；
6、脱水
将步骤5中所得的球磨浆料经纱布脱水，料浆含水量控制在15～30％之间；
7、成型
将步骤6所得脱水浆料在磁场成型机下压制成型，成型磁场强度为1.2～1.8T,成型压力为80～120MPa；
8、烧结
将步骤7所得坯件置于烧结炉内烧结，在1160℃保温1～1.5小时；
9、测试
将步骤8所得样品进行磁性能测试。
采用美国LakeShore 8604型振动样品磁强计测试样品的矫顽力Hc、饱和磁化强度4πMs、剩余磁化强度4πMr以及剩磁比Mr/Ms等静磁性能。
本发明自偏置环行器铁氧体基板材料的技术指标如下：
饱和磁化强度4πMs：>4.3kGs；
剩余磁化强度4πMr：>3.4kGs；
剩磁比Mr/Ms：>0.79
内禀矫顽力Hcj：>2.2kOe；
本发明采用氧化物陶瓷工艺制备高矫顽力及高密度的M型六角铁氧体。本实验流程操作简单，成本低，周期短，适用于大型工业生产。主要采用离子取代、湿法磁场成型、二次添加剂等获得高矫顽力及高密度。
以下根据具体实施方式对本发明作进一步的说明。
具体实施方式
针对目前M型铁氧体块材高矫顽力和高密度不能同时兼容的问题，本发明提供一种高矫顽力和高密度的M型六角铁氧体材料及其制备方法。
包括以下步骤：本发明的高矫顽力和高密度六角永磁铁氧体材料主成分按摩尔百分比，以氧化物计算，掺杂剂成分按重量百分比，以氧化物计算。本发明的高矫顽力和高密度铁氧体材料及其制备方法，包括以下步骤：
实施例1：
1、配方
原材料选取按质量百分比，以氧化物计算，称取15.27wt％BaCO3、3.12wt％La2O3、80.07wt％Fe2O3、其余为CuO原料；
2、一次球磨
将上述料粉在球磨机内混合均匀，时间12小时；
3、预烧
将步骤2所得球磨料烘干，在1100℃预烧2小时；
4、掺杂
将步骤3所得粉料按重量比加入以下掺杂剂2.5％Bi2O3、2.0％CuO和0.1％V2O5：
5、二次球磨
将步骤4中得到的料粉在球磨机中球磨18小时；
6、脱水
将步骤5中所得的球磨浆料经纱布脱水，料浆含水量控制在15～30％之间；
7、成型
将步骤6所得脱水浆料在磁场成型机下压制成型，成型磁场强度为1.8T,成型压力为80MPa；
8、烧结
将步骤7所得坯件置于烧结炉内烧结，在1160℃保温1.5小时；
实施例2：
1、配方
原材料选取按质量百分比，以氧化物计算，称取15.27wt％BaCO3、3.12wt％La2O3、80.07wt％Fe2O3、其余为CuO原料；
2、一次球磨
将上述料粉在球磨机内混合均匀，时间12小时；
3、预烧
将步骤2所得球磨料烘干，在1100℃预烧2小时；
4、掺杂
将步骤3所得粉料按重量比加入一下掺杂剂：2.5％Bi2O3、2.0％CuO和0.15％V2O5；
5、二次球磨
将步骤4中得到的料粉在球磨机中球磨18小时；
6、脱水
将步骤5中所得的球磨浆料经纱布脱水，料浆含水量控制在15～30％之间；
7、成型
将步骤6所得脱水浆料在磁场成型机下压制成型，成型磁场强度为1.8T,成型压力为120MPa；
8、烧结
将步骤7所得坯件置于烧结炉内烧结，在1160℃保温1.5小时；
实施例3：
1、配方
原材料选取按质量百分比，以氧化物计算，称取15.27wt％BaCO3、3.12wt％La2O3、80.07wt％Fe2O3、其余为CuO原料；
2、一次球磨
将上述料粉在球磨机内混合均匀，时间12小时；
3、预烧
将步骤2所得球磨料烘干，在1100℃预烧2小时；
4、掺杂
将步骤3所得粉料按重量比加入一下掺杂剂：2.5％Bi2O3、2.0％CuO和0.20％V2O5；
5、二次球磨
将步骤4中得到的料粉在球磨机中球磨18小时；
6、脱水
将步骤5中所得的球磨浆料经纱布脱水，料浆含水量控制在15～30％之间；
7、成型
将步骤6所得脱水浆料在磁场成型机下压制成型，成型磁场强度为1.8T,成型压力为120MPa；
8、烧结
将步骤7所得坯件置于烧结炉内烧结，在1160℃保温1.5小时；
经以上工艺制备出的M型六角铁氧体材料，其性能指标如下：
实施例1～3测试结果如下：
实施例 4πMs(Gs) 4πM<sub>r</sub>(Gs) H<sub>cj</sub>(Oe) d(g/cm<sup>3</sup>)
1 4298 3428 2270 5.15
2 4361 3465 2220 5.17
3 4296 3408 2253 5.14

Claims (2)

1.本发明主要针对自偏置环行器用六角铁氧体材料高致密度和高矫顽力难以兼顾的问题，提供一种高矫顽力和高致密度的六角永磁铁氧体材料及其制备方法。
本发明的高矫顽力和高密度铁氧体材料制备方法包括以下步骤：
1)、配方
原材料选取按质量百分比，以氧化物计算，称取15.27wt％BaCO3、3.12wt％La2O3、80.07wt％Fe2O3、其余为CuO原料；
2)、一次球磨
将上述料粉在球磨机内混合均匀，球磨时间为10～12小时；
3)、预烧
将步骤2所得球磨料烘干，在1100℃预烧2～4小时；
4)、掺杂
将步骤3所得粉料按重量比加入以下掺杂剂：2.5％Bi2O3、2.0％CuO和0.10％～0.20％V2O5；
5)、二次球磨
将步骤4中得到的料粉在球磨机中球磨18小时；
6)、脱水
将步骤5中所得的球磨浆料经纱布脱水，料浆含水量控制在15～30％之间；
7)、成型
将步骤6所得脱水浆料在磁场成型机下压制成型，成型磁场强度为1.2～1.8T,成型压力为80～120MPa；
8)、烧结
将步骤7所得坯件置于烧结炉内烧结，在1160℃保温1～1.5小时；
9)、测试
将步骤8所得样品进行磁性能测试。
采用美国LakeShore 8604型振动样品磁强计测试样品的矫顽力Hc、饱和磁化强度4πMs、剩余磁化强度4πMr以及剩磁比Mr/Ms等静磁性能。
2.根据权利要求1所述的U型六角铁氧体的制备方法，其特征在于，步骤4中所述的掺杂剂为0.10％-0.20％V2O5。
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