CN106396662A - 一种低损耗MnZn铁氧体及其烧结工艺 - Google Patents
一种低损耗MnZn铁氧体及其烧结工艺 Download PDFInfo
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Abstract
本发明公开了一种低损耗MnZn铁氧体及其烧结工艺。它主要由主配方和子配方两部分组成,所述的主配方包括Fe2O3、ZnO和MnO,其中:Fe2O3为52.7‑52.9mol%,ZnO为9.2‑11.2mol%,其余为MnO;所述的子配方包括SnO2、CaCO3、ZrO2和Nb2O5,将低损耗MnZn铁氧体放入钟罩炉中烧结,通过对升温段的升温速度、保温段的保温温度以及降温段的氧气含量控制,使得晶粒均匀生长,减少内应力。本发明的有益效果是:通过CaCO3、ZrO2和Nb2O5三者的联合添加,提高晶界的电阻率,同时细化晶粒,使得晶粒均匀生长;通过加入SnO2提高晶粒内部的电阻率;通过对升温段的升温速度、保温段的保温温度以及降温段的氧气含量控制,使得晶粒均匀生长,减少内应力。
Description
技术领域
本发明涉及软磁铁氧体材料相关技术领域,尤其是指一种低损耗MnZn铁氧体及其烧结工艺。
背景技术
MnZn铁氧体广泛应用于电子、通讯领域作为电源变压器材料。传统开关电源的输出功率与材料直接相关的参数就是材料的饱和磁通密度。高饱和磁通密度的材料可以使开关电源更加小型化、薄型化。材料的功率损耗会影响电能的转化效率,越低功率损耗,器件的转化效率越高。
目前国际上100℃时损耗最低的软磁MnZn铁氧体材料为TDK公司的PC47,但是随着电子元器件的小型和高效化的发展,要求进一步降低工作温度点的损耗。
国内外软磁铁氧体生产厂家,都为此进行大量的研制和量产,但是还没有厂家公开生产100℃损耗低于250kW/m3的铁氧体。
发明内容
本发明是为了克服现有技术中存在上述的不足,提供了一种降低涡流损耗和磁滞损耗的低损耗MnZn铁氧体及其烧结工艺。
为了实现上述目的,本发明采用以下技术方案:
一种低损耗MnZn铁氧体,主要由主配方和子配方两部分组成,所述的主配方包括Fe2O3、ZnO和MnO,其中:Fe2O3为52.7-52.9mol%,ZnO为9.2-11.2mol%,其余为MnO;所述的子配方包括SnO2、CaCO3、ZrO2和Nb2O5。
通过CaCO3、ZrO2和Nb2O5三者的联合添加,提高晶界的电阻率,同时细化晶粒,使得晶粒均匀生长,通过加入SnO2提高晶粒内部的电阻率,从而降低了涡流损耗和磁滞损耗。
作为优选,所述的子配方是按主配方的总重量百分比进行添加的,其中:SnO2为0.07-0.15wt%,CaCO3为0.06-0.08wt%,ZrO2为0.03-0.04wt%,Nb2O5为0.01-0.02wt%。
本发明还提供了一种低损耗MnZn铁氧体的烧结工艺,将低损耗MnZn铁氧体放入钟罩炉中烧结,通过对升温段的升温速度、保温段的保温温度以及降温段的氧气含量控制,使得晶粒均匀生长,减少内应力,具体操作步骤如下:
(1)升温段:由900℃升温到保温段的保温温度时,升温速度控制在1℃/分钟;
(2)保温段:保温温度为1290℃-1300℃,保温时间为180分钟-300分钟;
(3)降温段:在氮气保护下冷却,注重1250℃-1050℃的氧气含量控制,其中:1250℃的氧气含量在2%-4%,1200℃的氧气含量在1%-2%,1150℃的氧气含量在0.8%-0.25%,1050℃的氧气含量在0.2%-0.15%。
本发明的有益效果是:通过CaCO3、ZrO2和Nb2O5三者的联合添加,提高晶界的电阻率,同时细化晶粒,使得晶粒均匀生长;通过加入SnO2提高晶粒内部的电阻率;通过对升温段的升温速度、保温段的保温温度以及降温段的氧气含量控制,使得晶粒均匀生长,减少内应力。
具体实施方式
下面结合具体实施方式对本发明做进一步的描述。
实施例1:
将52.7mol%的Fe2O3和9.2mol%的ZnO,其余为MnO的量,按料球水的比例为1∶4∶0.45的比例进行混合,在砂磨中砂磨1小时,然后喷雾造粒,在回转窑中进行预烧,将0.06wt%的CaCO3,0.04wt%的ZrO2,0.01wt%的Nb2O5和0.08wt%的SnO2按预烧料的质量加入到预烧料中,在砂磨机中砂磨160分钟,喷雾造粒。在一定压力下压制成标环。放入钟罩炉中烧结,烧结温度为1300℃,保温300分钟。然后在氮气保护下冷却至室温。
对比例1:
将53.2mol%的Fe2O3和9.2mol%的ZnO,其余为MnO的量,按料球水的比例为1∶4∶0.45的比例进行混合,在砂磨中砂磨1小时,然后喷雾造粒,在回转窑中进行预烧,将0.06wt%的CaCO3,0.04wt%的ZrO2,0.01wt%的Nb2O5和0.08wt%的SnO2按预烧料的质量加入到预烧料中,在砂磨机中砂磨160分钟,喷雾造粒。在一定压力下压制成标环。放入钟罩炉中烧结,烧结温度为1300℃,保温300分钟。然后在氮气保护下冷却至室温。
将实施例1和比较例1的两组样环进行测试,具体数据见表1。
表1实施例1和对比例1样环性能对比
由表1可得,在比较例1中由于主配方中Fe2O3的含量过高,使得整体损耗偏高。
实施例2
将52.8mol%的Fe2O3和10.2mol%的ZnO,其余为MnO的量,按料球水的比例为1∶4∶0.45的比例进行混合,在砂磨机中砂磨1小时,然后喷雾造粒,在回转窑中进行预烧,将0.06wt%的CaCO3,0.04wt%的ZrO2,0.01wt%的Nb2O5和0.09wt%的SnO2按预烧料的质量加入到预烧料中,在砂磨机中砂磨160分钟,喷雾造粒。在一定压力下压制成标环。放入钟罩炉中烧结,烧结温度为1300℃,保温300分钟。然后在氮气保护下冷却至室温。
比较例2
将52.8mol%的Fe2O3和10.2mol%的ZnO,其余为MnO的量,按料球水的比例为1∶4∶0.45的比例进行混合,在砂磨机中砂磨1小时,然后喷雾造粒,在回转窑中进行预烧,将0.06wt%的CaCO3,0.04wt%的ZrO2,0.01wt%的Nb2O5按预烧料的质量加入到预烧料中,在砂磨机中砂磨160分钟,喷雾造粒。在一定压力下压制成标环。放入钟罩炉中烧结,烧结温度为1300℃,保温300分钟。然后在氮气保护下冷却至室温。
将实施例2和比较例2的两组样环进行测试,具体数据见表2。
表2实施例2和对比例2样环性能对比
由表2可得,在比较例2中由于子配方中未加入SnO2,使得涡流损耗增加,整体损耗偏高。
实施例3:
将52.9mol%的Fe2O3和11.2mol%的ZnO,其余为MnO的量,按料球水的比例为1∶4∶0.45的比例进行混合,在砂磨机中砂磨1小时,然后喷雾造粒,在回转窑中进行预烧,将0.08wt%的CaCO3,0.03wt%的ZrO2,0.01wt%的Nb2O5和0.1wt%的SnO2按预烧料的质量加入到预烧料中,在砂磨机中砂磨160分钟,喷雾造粒。在一定压力下压制成标环。放入钟罩炉中烧结,由900℃升温到1300℃时,升温速度控制在1℃/分钟;保温温度为1300℃,保温300分钟;然后在氮气保护下冷却,在降温段1250℃时氧气含量在4%,1200℃时氧气含量在1.5%,1150℃时氧气含量为0.5%,1050℃时氧气含量为0.15%。
比较例3
将52.9mol%的Fe2O3和11.2mol%的ZnO,其余为MnO的量,按料球水的比例为1∶4∶0.45的比例进行混合,在砂磨机中砂磨1小时,然后喷雾造粒,在回转窑中进行预烧,将0.08wt%的CaCO3,0.03wt%的ZrO2,0.01wt%的Nb2O5和0.1wt%的SnO2按预烧料的质量加入到预烧料中,在砂磨机中砂磨160分钟,喷雾造粒。在一定压力下压制成标环。放入钟罩炉中烧结由900℃升温到1300℃时,升温速度控制在1℃/分钟;保温温度为1300℃,保温300分钟;然后在氮气保护下冷却,在降温段1250℃时氧气含量在4%,1200℃时氧气含量在1.5%,1150℃时氧气含量为1%,1050℃时氧气含量为0.5%。
将实施例3和比较例3的两组样环进行测试,具体数据见表3。
表3实施例3和对比例3样环性能对比
由表3可得,在比较例3中由于烧结工艺的降温段中1150℃和1050℃的氧气含量过高,出现了一定程度的氧化,使得损耗增加。
Claims (3)
1.一种低损耗MnZn铁氧体,其特征是,主要由主配方和子配方两部分组成,所述的主配方包括Fe2O3、ZnO和MnO,其中:Fe2O3为52.7-52.9mol%,ZnO为9.2-11.2mol%,其余为MnO;所述的子配方包括SnO2、CaCO3、ZrO2和Nb2O5。
2.根据权利要求1所述的一种低损耗MnZn铁氧体,其特征是,所述的子配方是按主配方的总重量百分比进行添加的,其中:SnO2为0.07-0.15wt%,CaCO3为0.06-0.08wt%,ZrO2为0.03-0.04wt%,Nb2O5为0.01-0.02wt%。
3.根据权利要求1或2所述的一种低损耗MnZn铁氧体的烧结工艺,其特征是,将低损耗MnZn铁氧体放入钟罩炉中烧结,通过对升温段的升温速度、保温段的保温温度以及降温段的氧气含量控制,使得晶粒均匀生长,减少内应力,具体操作步骤如下:
(1)升温段:由900℃升温到保温段的保温温度时,升温速度控制在1℃/分钟;
(2)保温段:保温温度为1290℃-1300℃,保温时间为180分钟-300分钟;
(3)降温段:在氮气保护下冷却,注重1250℃-1050℃的氧气含量控制,其中:1250℃时氧气含量在2%-4%,1200℃时氧气含量在1%-2%,1150℃时氧气含量在0.8%-0.25%,1050℃时氧气含量在0.2%-0.15%。
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