CN115611624B - 一种宽温高Tc高磁导率锰锌铁氧体材料及其制备方法 - Google Patents
一种宽温高Tc高磁导率锰锌铁氧体材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种宽温高Tc高磁导率锰锌铁氧体材料及其制备方法,宽温高Tc高磁导率锰锌铁氧体材料至少包括FeFe2O4、MnFe2O4、ZnFe2O4三种单元铁氧体固溶形成的复合铁氧体材料,三种单元铁氧体的含量以百分比计算,分别为α、β、γ,满足数量关系:5.78%≤α≤7.33%,30.49%≤γ≤34.43%,且α+β+γ=1。本发明中的设计方法及制造工艺制备出的宽温高Tc高磁导率锰锌铁氧体材料,其起始磁导率μi≥7000(25℃,10kHz),居里温度Tc>170℃,同时在20℃~100℃的宽温度范围内,起始磁导率最小值μi_min≥6000,制得的材料克服了现有7K高磁导率锰锌铁氧体材料的不足,是一种宽温高Tc高磁导率锰锌铁氧体材料,适合推广应用。
Description
技术领域
本发明涉及锰锌铁氧体材料技术领域,具体涉及宽温高Tc高磁导率锰锌铁氧体材料及其制备方法。特别是在宽温度范围内有高磁导率的锰锌铁氧体材料,属于氧化物制备磁性材料领域。
背景技术
当前全球电子信息产业,新型照明技术、电子产品数字化等方面的飞速发展,向材料工业不断提出更高更新的需求,高磁导率软磁材料也面临同样的挑战。为了满足电子变压器等电子器件的平面化、片式化及轻量化的发展需求,需要提高铁氧体材料的磁导率;同时,为了让电子器件更好的适应其应用于环境温差大的场合,在满足高性能要求的基础上,必然要求铁氧体材料具有高的温度稳定性。因此,开发出具有宽温高Tc高磁导率的锰锌铁氧体材料是十分重要的。
目前,针对高磁导率锰锌铁氧体材料,国内外都开发出了不同牌号的铁氧体材料。Ferroxcube也开发的3E25、3E26、3E27、3E65等,日本TDK公司很早就开发的HP5、DN70等,中国台湾越峰也开发出A05、A07等;以及以横店东磁和天通为代表的内资企业也开发出了R5K、R7K、TSR7、等都是磁导率高于5000低于10000的高磁导率材料。在同时兼顾高磁导率、居里温度的条件下,磁导率为7000左右的高导材料受到广泛的重视和应用。传统的7000高导材料难以适应环境温差较大的场合,因此急需开发出一款居里温度达到170℃以上的材料,它的磁导率的温度特性良好,其起始磁导率在极大的温度范围内稳定在7000左右。这种宽温高Tc高磁导率铁氧体材料将在汽车电子等恶劣工况下具有显著的竞争优势,市场前景广阔。
综上所述,开发出的铁氧体材料在在宽温度范围内有高磁导率的锰锌铁氧体材料,同时又有成本优势,将在市场上具有很大的竞争优势,也是亟需要解决的问题。
发明内容
为了解决上述技术问题,本发明采用了以下技术方案:
采用本发明中的设计方法及制造工艺制备出的宽温高Tc高磁导率锰锌铁氧体材料,其起始磁导率μi≥7000(25℃,10kHz),居里温度Tc>170℃,同时在20℃~100℃的宽温度范围内,起始磁导率最小值μi_min≥6000。
一种宽温高Tc高磁导率锰锌铁氧体材料,
宽温高Tc高磁导率锰锌铁氧体材料至少包括FeFe2O4、MnFe2O4、ZnFe2O4三种单元铁氧体固溶形成的复合铁氧体材料,三种单元铁氧体的含量以百分比计算,分别为α、β、γ,满足数量关系:5.78%≤α≤7.33%,30.49%≤γ≤34.43%,且α+β+γ=1。
作为本方案的进一步改进,铁氧体材料由Fe2O3、MnO、ZnO为原料制备而成,含量以mol%计算,含量分别为a%、b%、c%,a+b+c=100,且有公式Tc=9.40a-3.40b-11.93c-15.3,Tc>170℃。
作为本方案的进一步改进,还包括添加剂组合物,所述添加剂组合物为BiVO4、LiCoO2、TiO2、CaCO3中的任意3种或者3种以上组分。
作为本方案的进一步改进,添加剂组合为BiVO4和LiCoO2和TiO2,
其中,BiVO4含量为200~500ppm,LiCoO2含量为300~800ppm,TiO2含量为200~500ppm。
作为本方案的进一步改进,添加剂组合为BiVO4和LiCoO2,
其中,BiVO4含量为200~500ppm,LiCoO2含量为300~800ppm。
一种宽温高Tc高磁导率锰锌铁氧体材料的制备方法,宽温高Tc高磁导率锰锌铁氧体材料包括下列步骤:
(1)原料混合:根据单元铁氧体含量百分比计算出三种主原料的投料量,称量好后使用振磨机混合,使三种原材料分布均匀;
(2)预烧:混合好的原料进入回转窑预烧,清除原料内的酸根离子和其他杂质,并初步反应生成铁氧体;
(3)砂磨:将预烧后的粉料加入添加剂组合、纯水、PVA、消泡剂后进行砂磨,粉料砂磨粒径控制在0.7~1.2μm;
(4)喷雾造粒:将砂磨后的浆料在喷雾塔中进行喷雾造粒;
(5)将喷雾造粒的粉料使用成型机压制成生坯,在钟罩窑中使用1340℃~1360℃之间的温度烧结7~10小时,降温过程中气氛使用平衡方程进行设定,冷却后即得到所述的软磁铁氧体材料。
作为本方案的进一步改进,所述步骤(5)中的烧结时间为8小时。
作为本方案的进一步改进,所述步骤(5)中的烧结温度为1360℃。
与现有技术相比,本发明具备下述有益效果:
本发明从铁氧体的化学组成出发,通过对组成铁氧体材料的单元铁氧体的数量和比例、添加剂组合、居里温度Tc、工艺条件等方面控制,实现了材料的高Tc、高磁导率特性和温度稳定性;
为了提高磁导率和改善温度特性,添加剂组合中一般都会选用低熔点的助熔剂和形成高阻晶界的CaCO3等等。在本发明专利中,结合传统的添加剂理论上,选用了BiVO4和LiCoO2作为必用的添加剂,上述添加剂的添加显著改善了磁导率和温度特性,BiVO4的熔点只有500℃,在烧结的过程中形成液相,可以促进晶粒均匀长大,提高磁导率;LiCoO2作为添加剂可以和主配方中的Fe2O3反应生成Li0.5Fe0.5Fe2O4和CoFe2O4,Li0.5Fe0.5Fe2O4可以进一步提升居里温度,而CoFe2O4拥有很大的磁晶各向异性常数K1,可以进一步有效补偿铁氧体的磁晶各向异性常数K1,调整磁导率的温度特性和二峰位置,可以大幅改善磁导率的温度特性;
通过选用BiVO4和LiCoO2作为必用的添加剂,本发明制备了一种宽温高Tc高磁导率锰锌铁氧体材料,该铁氧体电磁性能的测试条件如下:起始磁导率μi:B<0.25mT;饱和磁通密度Bs:1kHz/1194A*m-1,单位为mT。其起始磁导率μi≥7000(25℃,10kHz),居里温度Tc>170℃,同时在20℃~100℃的宽温度范围内,起始磁导率最小值μi_min≥6000。综上,制得的材料克服了现有7K高磁导率锰锌铁氧体材料的不足,是一种宽温高Tc高磁导率锰锌铁氧体材料,适合推广应用。
附图说明
附图1为本发明中实施例中制备的宽温高Tc高磁导率锰锌铁氧体材料,典型的磁导率温度曲线。
具体实施方式
为了使本发明的目的、技术方案和优点更加清楚,以下结合实施例对本发明作进一步说明:
实施例1~4:
铁氧体材料内FeFe2O4、MnFe2O4、ZnFe2O4三种单元铁氧体含量α、β、γ,且满足6.30%≤α≤6.82%,31.45%≤γ≤33.44%,添加剂组合为0.04wt%BiVO4、0.06wt%LiCoO2、0.02% CaCO3,α、β、γ及Tc的具体值见表-1中所示。铁氧体材料的具体制备方法如下:
(1)原料混合:根据三种单元铁氧体含量百分比计算出三种主原料的投料量,称量好后使用振磨机混合,使三种原材料分布均匀;
(2)预烧:混合好的原料进入回转窑预烧,清除原料内的酸根离子和其他杂质,并初步反应生成铁氧体;
(3)砂磨:将预烧后的粉料加入添加剂组合、纯水、PVA、消泡剂后进行砂磨,粉料砂磨粒径控制在0.7~1.1μm;
(4)喷雾造粒:将砂磨后的浆料在喷雾塔中进行喷雾造粒;
(5)将喷雾造粒的粉料使用成型机压制成生坯,在钟罩窑中使1360℃温度烧结8小时,降温过程中气氛使用平衡方程进行设定,冷却后即得到所述的软磁铁氧体材料。
实施例1~4的具体配方见表-1中所示。
实施例1~4样品的主要技术指标见表-2中所示。
对比例1~4:
对比例1~4中均有配方参数超出本发明前述给定的范围。其中,对比例1~2中α值超出本发明前述给定的范围,对比例3~4中γ值超出本发明前述给定的范围,并且对比例1、对比例4的Tc均超出了本发明前述给定的范围。对比例1~4的添加剂组合和制备工艺与实施例1-4完全相同。
对比例1~4样品的主要技术指标见表-2所示。
表-1实施例1~4及对比例1~4组分配方
表-2实施例1~4及对比例1~4样品的主要技术指标
实施例5~8:
实施例5~8的铁氧体材料内FeFe2O4、MnFe2O4、ZnFe2O4三种单元铁氧体含量完全相同,α、γ的值分别为α=6.56%,γ=32.46%,添加剂组合见表-3中所示,制备工艺与实施例1~4完全相同。
实施例5~8样品的主要技术指标见表-4中所示。
对比例5~8:
对比例5~8中的三种单元铁氧体含量与实施例5~8完全相同,但是添加剂组合中BiVO4和LiCoO2分别超出本发明前述给定的范围,添加剂组合见表-3所示,制备工艺与实施例5~8也完全相同。
对比例5~8样品的主要技术指标见表-4中所示。
实施例9~10:
实施例9~10的铁氧体材料内FeFe2O4、MnFe2O4、ZnFe2O4三种单元铁氧体含量完全相同,α、γ的值分别为α=6.56%,γ=32.46%,添加剂组合中只有TiO2含量不同,如表-3所示,制备工艺与实施例1~4完全相同。
实施例9~10样品的主要技术指标见表-4中所示。
对比例9~10:
对比例9~10中的三种单元铁氧体含量与实施例9~10也完全相同,但是添加剂组合中TiO2超出本发明前述给定的范围,添加剂组合见表-3所示,制备工艺与实施例9~10也完全相同。
对比例9~10样品的主要技术指标见表-4中所示。
表-3实施例5~10及对比例5~10组分配方
表-4实施例5~10及对比例5~10样品的主要技术指标
可以看出,本发明专利制备了一种宽温高Tc高磁导率锰锌铁氧体材料,其起始磁导率μi≥7000(25℃,10kHz),居里温度Tc>170℃,同时在20℃~100℃的宽温度范围内,起始磁导率最小值μi_min≥6000。
在本发明专利中,结合传统的添加剂理论上,选用了BiVO4和LiCoO2作为必用的添加剂,上述添加剂的添加显著改善了磁导率和温度特性,BiVO4的熔点只有500℃,在烧结的过程中形成液相,可以促进晶粒均匀长大,提高磁导率;LiCoO2作为添加剂可以和主配方中的Fe2O3反应生成Li0.5Fe0.5Fe2O4和CoFe2O4,Li0.5Fe0.5Fe2O4可以进一步提升居里温度,而CoFe2O4拥有很大的磁晶各向异性常数K1,可以进一步有效补偿铁氧体的磁晶各向异性常数K1,调整磁导率的温度特性和二峰位置,可以大幅改善磁导率的温度特性。
以上所述仅为本发明的优选实施方式,并非因此限制本发明的专利范围,凡是利用本发明所作的等效变换,均在本发明的专利保护范围内。
Claims (5)
1.一种宽温高Tc高磁导率锰锌铁氧体材料,其特征在于:
宽温高Tc高磁导率锰锌铁氧体材料至少包括FeFe2O4、MnFe2O4、ZnFe2O4三种单元铁氧体固溶形成的复合铁氧体材料,三种单元铁氧体的含量以百分比计算,分别为α、β、γ,满足数量关系:5.78%≤α≤7.33%,30.49%≤γ≤34.43%,且α+β+γ=1;
还包括添加剂组合物,添加剂组合为BiVO4和LiCoO2和TiO2,
其中,BiVO4含量为200~500ppm,LiCoO2含量为300~800ppm,TiO2含量为200~500ppm。
2.根据权利要求1所要求的宽温高Tc高磁导率锰锌铁氧体材料,其特征在于:铁氧体材料由Fe2O3、MnO、ZnO为原料制备而成,含量以mol%计算,含量分别为a%、b%、c%,a+b+c=100,且有公式Tc=9.40a-3.40b-11.93c-15.3,Tc>170℃。
3.一种权利要求1或2任一项所述宽温高Tc高磁导率锰锌铁氧体材料的制备方法,其特
征在于:宽温高Tc高磁导率锰锌铁氧体材料包括下列步骤:
(1)原料混合:根据单元铁氧体含量百分比计算出三种主原料的投料量,称量好后使用
振磨机混合,使三种原材料分布均匀;
(2)预烧:混合好的原料进入回转窑预烧,清除原料内的酸根离子和其他杂质,并初步
反应生成铁氧体;
(3)砂磨:将预烧后的粉料加入添加剂组合、纯水、PVA、消泡剂后进行砂磨,粉料砂磨粒径控制在0.7~1.2μm;
(4)喷雾造粒:将砂磨后的浆料在喷雾塔中进行喷雾造粒;
(5)将喷雾造粒的粉料使用成型机压制成生坯,在钟罩窑中使用1340℃~1360℃之间
的温度烧结7~10小时,降温过程中气氛使用平衡方程进行设定,冷却后即得到铁氧体材料。
4.根据权利要求3所要求的宽温高Tc高磁导率锰锌铁氧体材料的制备方法,其特征在
于:所述步骤(5)中的烧结时间为8小时。
5.根据权利要求4所要求的宽温高Tc高磁导率锰锌铁氧体材料的制备方法,其特征在
于:所述步骤(5)中的烧结温度为1360℃。
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