CN111116191A - 一种高磁导率低损耗锰锌软磁铁氧体材料及其制备方法 - Google Patents
一种高磁导率低损耗锰锌软磁铁氧体材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种高磁导率低损耗锰锌软磁铁氧体材料及其制备方法,该铁氧体材料的原料包括主料和添加剂,主料包括Fe2O3、MnO、ZnO,其中,按摩尔百分比计,Fe2O3为51.8‑52.4%、ZnO为22.4‑22.8%、余量为MnO;添加剂包括V2O5、Bi2O3、Y2O3、TiO2、CaCO3、SiO2,其中,按主料的总重量计,添加剂的组成为:V2O5:200‑500ppm、Bi2O3:400‑800ppm、Y2O3:1000‑1500ppm、TiO2:1000‑1500ppm、CaCO3:500‑1000ppm、SiO2:500‑1000ppm。本发明制得的锰锌软磁铁氧体材料的磁导率高、饱和磁感应强度高、损耗低,具有优良的电磁性能。
Description
技术领域
本发明涉及铁氧体材料技术领域,尤其涉及一种高磁导率低损耗锰锌软磁铁氧体材料及其制备方法。
背景技术
随着电子仪器、设备的体积趋向小型化,对电子元器件的性能要求也逐渐提升。磁导率是软磁铁氧体材料的重要参数之一,当材料磁导率高时,较少的线圈匝数就可以获得规定的电感量,从而能有效减少变压器的电阻及其引起的损耗,而且能有效减少变压器的体积,有利于电子设备的轻量化。因此,如何制备具有高磁导率、低损耗的锰锌软磁铁氧体,成为近年来的一个研究重点。
发明内容
基于背景技术存在的技术问题,本发明提出了一种高磁导率低损耗锰锌软磁铁氧体材料及其制备方法。
本发明提出的一种高磁导率低损耗锰锌软磁铁氧体材料,其原料包括主料和添加剂,所述主料包括Fe2O3、MnO、ZnO,其中,按摩尔百分比计,Fe2O3为51.8-52.4%、ZnO为22.4-22.8%、余量为MnO;所述添加剂包括V2O5、Bi2O3、Y2O3、TiO2、CaCO3、SiO2,其中,按主料的总重量计,添加剂的组成为:V2O5:200-500ppm、Bi2O3:400-800ppm、Y2O3:1000-1500ppm、TiO2:1000-1500ppm、CaCO3:500-1000ppm、SiO2:500-1000ppm。
优选地,所述主料中,按摩尔百分比计,Fe2O3为52.2%、ZnO为22.6%、余量为MnO。
优选地,按主料的总重量计,添加剂的组成为:V2O5:400ppm、Bi2O3:600ppm、Y2O3:1200ppm、TiO2:1200ppm、CaCO3:600ppm、SiO2:600ppm。
一种所述的高磁导率低损耗锰锌软磁铁氧体材料的制备方法,包括下述步骤:
S1、将Fe2O3、MnO、ZnO混合均匀,得到主料,将所述主料经过一次球磨后烘干,经过预烧处理、破碎,得到预烧料;
S2、将V2O5、Bi2O3、Y2O3、TiO2、CaCO3、SiO2混合均匀,得到添加剂,将所述添加剂与所述预烧料混合均匀,经过二次球磨后烘干,得到混合料;
S3、将所述混合料与聚乙烯醇水溶液混合均匀,得到混合浆料;
S4、将所述混合浆料进行喷雾造粒,得到颗粒料;
S5、将所述颗粒料压制成型,然后进行烧结,冷却后得到铁氧体材料。
优选地,所述步骤S1中,预烧处理的温度为820-860℃,时间为1.5-2.5h。
优选地,所述步骤S1中,一次球磨的球料比为(2-3):1,球磨时间为5-8h;所述步骤S2中,二次球磨的球料比为(4-5):1,球磨时间为8-12h。
优选地,所述混合料与聚乙烯醇水溶液的质量比为10-15%;所述聚乙烯醇水溶液的质量分数为5-10%。
优选地,所述步骤S4中,压制成型的压力为10-12MPa。
优选地,所述步骤S5中,烧结的具体方法为:先以200-220℃/h的升温速率升温至600-640℃,保温1-1.5h,然后以280-300℃/h的升温速率升温至1000-1050℃,保温0.5-1h,再以120-140℃/h的升温速率升温至1400-1420℃,保温烧结1.5-2.5h,即可。
本发明的有益效果如下:
本发明的原料中,以适量的V2O5、Bi2O3、Y2O3、TiO2、CaCO3、SiO2复配作为添加剂,其中V2O5、Bi2O3能够促进材料中晶粒的快速生长,并且增加烧结中材料的密度,从而提高材料的磁导率;Y2O3能够增大晶格常数,促进晶粒生长,从而提高饱和磁感应强度和磁导率;TiO2能够固溶于晶格中,提高晶粒内部的电阻率,降低涡流损耗;CaCO3、SiO2能够形成CaSiO3相,在晶粒边界析出,提高晶界电阻率,从而降低涡流损耗;Y2O3、CaCO3、SiO2还能够起到协同作用,形成钇硅酸盐相分布在晶界间,能够充填气孔,提高材料的致密性,从而提高材料的磁导率,降低损耗。本发明还通过选择合适的预烧温度、成型压力以及烧结温度曲线,提高了材料微观结构的晶粒均匀性以及致密性,进一步提升材料的饱和磁感应强度、磁导率,降低损耗。通过上述配方和工艺的选择,本发明提供的锰锌软磁铁氧体材料具有磁导率高、饱和磁感应强度高、损耗低的优点,具有优良的电磁性能。
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
一种高磁导率低损耗锰锌软磁铁氧体材料,其原料包括主料和添加剂,主料包括Fe2O3、MnO、ZnO,其中,按摩尔百分比计,Fe2O3为51.8%、ZnO为22.4%、余量为MnO;其中,按主料的总重量计,添加剂的组成为:V2O5:500ppm、Bi2O3:800ppm、Y2O3:1500ppm、TiO2:1500ppm、CaCO3:1000ppm、SiO2:1000ppm。
高磁导率低损耗锰锌软磁铁氧体材料的制备方法包括下述步骤:
S1、将Fe2O3、MnO、ZnO混合均匀,得到主料,将主料经过一次球磨后烘干,其中一次球磨的球料比为2:1,球磨时间为5h,然后在820℃预烧处理1.5h,经过破碎,得到预烧料;
S2、将V2O5、Bi2O3、Y2O3、TiO2、CaCO3、SiO2混合均匀,得到添加剂,将所述添加剂与所述预烧料混合均匀,经过二次球磨后烘干,其中二次球磨的球料比为4:1,球磨时间为8h,得到混合料;
S3、将所述混合料与质量分数为5%的聚乙烯醇水溶液混合均匀,得到混合浆料,其中混合料与聚乙烯醇水溶液的质量比为10%;
S4、将所述混合浆料进行喷雾造粒,得到颗粒料;
S5、将所述颗粒料在10MPa条件下压制成型,然后以200℃/h的升温速率升温至600℃,保温1h,然后以280℃/h的升温速率升温至1000℃,保温0.5h,再以120℃/h的升温速率升温至1400℃,保温烧结1.5h,冷却后得到铁氧体材料。
实施例2
一种高磁导率低损耗锰锌软磁铁氧体材料,其原料包括主料和添加剂,主料包括Fe2O3、MnO、ZnO,其中,按摩尔百分比计,Fe2O3为52.4%、ZnO为22.8%、余量为MnO;其中,按主料的总重量计,添加剂的组成为:V2O5:200ppm、Bi2O3:400ppm、Y2O3:1000ppm、TiO2:1000ppm、CaCO3:500ppm、SiO2:500ppm。
高磁导率低损耗锰锌软磁铁氧体材料的制备方法包括下述步骤:
S1、将Fe2O3、MnO、ZnO混合均匀,得到主料,将主料经过一次球磨后烘干,其中一次球磨的球料比为3:1,球磨时间为8h,然后在860℃预烧处理2.5h,经过破碎,得到预烧料;
S2、将V2O5、Bi2O3、Y2O3、TiO2、CaCO3、SiO2混合均匀,得到添加剂,将所述添加剂与所述预烧料混合均匀,经过二次球磨后烘干,其中二次球磨的球料比为5:1,球磨时间为12h,得到混合料;
S3、将所述混合料与质量分数为10%的聚乙烯醇水溶液混合均匀,得到混合浆料,其中混合料与聚乙烯醇水溶液的质量比为15%;
S4、将所述混合浆料进行喷雾造粒,得到颗粒料;
S5、将所述颗粒料在12MPa条件下压制成型,然后以220℃/h的升温速率升温至640℃,保温1.5h,然后以300℃/h的升温速率升温至1050℃,保温1h,再以140℃/h的升温速率升温至1420℃,保温烧结2.5h,冷却后得到铁氧体材料。
实施例3
一种高磁导率低损耗锰锌软磁铁氧体材料,其原料包括主料和添加剂,主料包括Fe2O3、MnO、ZnO,其中,按摩尔百分比计,Fe2O3为52.2%、ZnO为22.6%、余量为MnO;按主料的总重量计,添加剂的组成为:V2O5:400ppm、Bi2O3:600ppm、Y2O3:1200ppm、TiO2:1200ppm、CaCO3:600ppm、SiO2:600ppm。
高磁导率低损耗锰锌软磁铁氧体材料的制备方法包括下述步骤:
S1、将Fe2O3、MnO、ZnO混合均匀,得到主料,将主料经过一次球磨后烘干,其中一次球磨的球料比为2.5:1,球磨时间为6h,然后在850℃预烧处理2h,经过破碎,得到预烧料;
S2、将V2O5、Bi2O3、Y2O3、TiO2、CaCO3、SiO2混合均匀,得到添加剂,将所述添加剂与所述预烧料混合均匀,经过二次球磨后烘干,其中二次球磨的球料比为4.5:1,球磨时间为10h,得到混合料;
S3、将所述混合料与质量分数为7.5%的聚乙烯醇水溶液混合均匀,得到混合浆料,其中混合料与聚乙烯醇水溶液的质量比为12%;
S4、将所述混合浆料进行喷雾造粒,得到颗粒料;
S5、将所述颗粒料在11MPa条件下压制成型,然后以210℃/h的升温速率升温至620℃,保温1.2h,然后以290℃/h的升温速率升温至1020℃,保温0.6h,再以130℃/h的升温速率升温至1410℃,保温烧结2h,冷却后得到铁氧体材料。
经测试,实施例1-3制得的铁氧体材料在25℃,1.2kA/m条件下的饱和磁感应强度Bs≥450mT,10kHZ条件下的磁导率μi≥13000,10kHZ条件下的比损耗因子tanδ/μi≤1.5×10-6,具有磁导率高、饱和磁感应强度高、损耗低的电磁特性。
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 (9)
1.一种高磁导率低损耗锰锌软磁铁氧体材料,其特征在于,其原料包括主料和添加剂,所述主料包括Fe2O3、MnO、ZnO,其中,按摩尔百分比计,Fe2O3为51.8-52.4%、ZnO为22.4-22.8%、余量为MnO;所述添加剂包括V2O5、Bi2O3、Y2O3、TiO2、CaCO3、SiO2,其中,按主料的总重量计,添加剂的组成为:V2O5:200-500ppm、Bi2O3:400-800ppm、Y2O3:1000-1500ppm、TiO2:1000-1500ppm、CaCO3:500-1000ppm、SiO2:500-1000ppm。
2.根据权利要求1所述的高磁导率低损耗锰锌软磁铁氧体材料,其特征在于,所述主料中,按摩尔百分比计,Fe2O3为52.2%、ZnO为22.6%、余量为MnO。
3.根据权利要求1或2所述的种高磁导率低损耗锰锌软磁铁氧体材料,其特征在于,按主料的总重量计,添加剂的组成为:V2O5:400ppm、Bi2O3:600ppm、Y2O3:1200ppm、TiO2:1200ppm、CaCO3:600ppm、SiO2:600ppm。
4.一种如权利要求1-3任一项所述的高磁导率低损耗锰锌软磁铁氧体材料的制备方法,其特征在于,包括下述步骤:
S1、将Fe2O3、MnO、ZnO混合均匀,得到主料,将所述主料经过一次球磨后烘干,经过预烧处理、破碎,得到预烧料;
S2、将V2O5、Bi2O3、Y2O3、TiO2、CaCO3、SiO2混合均匀,得到添加剂,将所述添加剂与所述预烧料混合均匀,经过二次球磨后烘干,得到混合料;
S3、将所述混合料与聚乙烯醇水溶液混合均匀,得到混合浆料;
S4、将所述混合浆料进行喷雾造粒,得到颗粒料;
S5、将所述颗粒料压制成型,然后进行烧结,冷却后得到铁氧体材料。
5.根据权利要求4所述的高磁导率低损耗锰锌软磁铁氧体材料的制备方法,其特征在于,所述步骤S1中,预烧处理的温度为820-860℃,时间为1.5-2.5h。
6.根据权利要求4或5所述的高磁导率低损耗锰锌软磁铁氧体材料的制备方法,其特征在于,所述步骤S1中,一次球磨的球料比为(2-3):1,球磨时间为5-8h;所述步骤S2中,二次球磨的球料比为(4-5):1,球磨时间为8-12h。
7.根据权利要求4-6任一项所述的高磁导率低损耗锰锌软磁铁氧体材料的制备方法,其特征在于,所述混合料与聚乙烯醇水溶液的质量比为10-15%;所述聚乙烯醇水溶液的质量分数为5-10%。
8.根据权利要求4-7任一项所述的高磁导率低损耗锰锌软磁铁氧体材料的制备方法,其特征在于,所述步骤S4中,压制成型的压力为10-12MPa。
9.根据权利要求4-8任一项所述的高磁导率低损耗锰锌软磁铁氧体材料的制备方法,其特征在于,所述步骤S5中,烧结的具体方法为:先以200-220℃/h的升温速率升温至600-640℃,保温1-1.5h,然后以280-300℃/h的升温速率升温至1000-1050℃,保温0.5-1h,再以120-140℃/h的升温速率升温至1400-1420℃,保温烧结1.5-2.5h,即可。
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