CN111170731A - 一种锰锌高磁导率高居里温度高频材料及其制备方法 - Google Patents
一种锰锌高磁导率高居里温度高频材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种锰锌高磁导率高居里温度高频磁性材料及其制备方法。该磁性材料主成分包括52.67mol%~53.43mol%的Fe2O3,16.15mol%~17.3mol%的ZnO,其余为Mn3O4;辅助成分包括CaCO3、Bi2O3、Nb2O5、MoO3、SiO2中的三种或三种以上;所述磁性材料的居里温度Tc>180℃,初始磁导率(25℃,10kHz)μi>7000,磁导率(25℃,400kHz)μ>7000。本发明方法制备的磁性材料可以在既获得高磁导率和高居里温度的同时,还具备兼顾宽频特性要求,低频段和高频段的磁导率始终保持在较高的水平,有效扩展了材料的应用范围。
Description
技术领域
本发明涉及软磁铁氧体材料制备技术领域,尤其涉及一种锰锌高磁导率高居里温度高频材料及其制备方法。
背景技术
高磁导率锰锌铁氧体作为新时代的功能材料,主要应用于各类电子产品中,例如:通信设备,家用电器,计算机,汽车等。近年来,电子产品向轻,薄,短,小的方向发展,对软磁铁氧体材料的性能提出了更高的要求,其中高磁导率锰锌材料是随着市场发展最快,市场前景最好的材料之一。
随着科学技术的发展和人类室外活动范围的不断扩大,电子电力器件市场日益对软磁材料有更高的要求,既要求材料在室外工作时有较高的初始磁导率,又要求材料在工作时有稳定的宽频特性和较高的居里温度,而一般的高导材料很难兼顾高磁导率高居里温度和宽频特性要求,因此急需一种在常温和高温下具有高磁导率而且居里温度高的同时频率应用范围广泛的软磁材料。如公开号为CN108264340A的中国专利,公开了“一种高居里温度高磁导率锰锌铁氧体材料及其制备方法”,其获得了一种高磁导率、高居里温度、高饱和磁通密度的锰锌铁氧体磁性材料,虽然初始磁导率达到7000居里温度在200℃以上,但是没有提及频率性能,因而其应用范围有限。
发明内容
为了解决上述技术问题,本发明提出如下技术方案:
一种锰锌高磁导率高居里温度高频磁性材料,包括主成分和辅助成分,所述主成分包括Fe2O3、ZnO和Mn3O4,所述辅助成分包括CaCO3、Bi2O3、Nb2O5、MoO3、SiO2中的三种或三种以上;所述辅助成分的总重量为所述主成分总重量的0.11wt%~0.12wt%;所述磁性材料的居里温度Tc>180℃,初始磁导率(25℃,10kHz)μi>7000,磁导率(25℃,400kHz)μ>7000。
进一步地,所述主成分以各自氧化物计算分别为52.67mol%~53.43mol%的Fe2O3,16.15mol%~17.3mol%的ZnO,其余为Mn3O4。
进一步地,所述Fe2O3与ZnO摩尔百分数成分含量之比大于或等于3.04。
进一步地,所述材料的比损耗系数(25℃,10kHz)tanδ/μi≤4×10-6。
进一步地,所述主成分各组分原料纯度99wt%以上。
进一步地,基于所述总重量,所述辅助成分添加量范围为CaCO3:160ppm~220ppm,Bi2O3:500ppm~650ppm,Nb2O5:20ppm~80ppm,MoO3:200ppm~350ppm,SiO2:0ppm~80ppm。
一种锰锌高磁导率高居里温度高频磁性材料的制备方法,包括以下步骤:
(1)配料混合一磨:按主成分配比称量各主成分;取所述主成分重量100wt%~110wt%的去离子水、消泡剂与分散剂的混合物于砂磨机中混合,混合时间30min,转速1000r/min;
(2)预烧:将步骤(1)所得粉料置入马弗炉预烧,预烧温度800~850℃,预烧时间2个小时;
(3)配料混合二磨:将步骤(2)所得预烧料中添加辅助成分,加入粉料重量60wt%~70wt%的去离子水后进行球磨,球磨时间48min,得到球磨后的料浆;
(4)造粒:将步骤(3)所得的料浆烘干过筛后添加适量的胶水进行造粒;
(5)压制:用步骤(4)所得的粉料进行压制成型为标准样品生坯;
(6)烧结:将步骤(5)压制成型的样品生坯在平衡氧气氛中进行烧结,终烧温度控制在1350~1390℃。
其中,所述主成分包括Fe2O3、ZnO和Mn3O4,所述辅助成分包括CaCO3、Bi2O3、Nb2O5、MoO3、SiO2中的三种或三种以上;所述辅助成分的总重量为所述主成分总重量的0.11wt%~0.12wt%,所述磁性材料的居里温度Tc>180℃,初始磁导率(25℃,10kHz)μi>7000,磁导率(25℃,400kHz)μ>7000。
进一步地,所述主成分配比为52.67mol%~53.43mol%Fe2O3,16.15mol%~17.3mol%的ZnO,其余为Mn3O4。
进一步地,所述Fe2O3与ZnO摩尔百分数成分含量之比大于或等于3.04。
进一步地,所述材料的比损耗系数(25℃,10kHz)tanδ/μi≤4×10-6。
进一步地,所述主成分各组分原料纯度99wt%以上。
进一步地,所述辅助成分添加量范围为CaCO3:160ppm~220ppm,Bi2O3:500ppm~650ppm,Nb2O5:20ppm~80ppm,MoO3:200ppm~350ppm,SiO2:0ppm~80ppm。
进一步地,所述消泡剂为有机硅类消泡剂,如聚醚改性有机硅消泡剂或乳液型聚硅氧烷等;所述分散剂为柠檬酸盐类,十二烷基磺酸盐类,1-甲基戊醇等分散剂中的一种或多种。
进一步地,在所述步骤(3)中球磨后的浆料平均粒度控制在1±0.1μm。
进一步地,所述平衡氧分压按公式LogPO2=-A/T+B计算,确定氧含量:A取值10000~15000,B取值5~10。
本发明的有益效果是:
本发明方法制备的磁性材料可以在既获得高磁导率和高居里温度的同时,还具备兼顾高磁导率高居里温度和宽频特性要求,低频段和高频段的磁导率始终保持在较高的水平,该磁性材料在初始磁导率达到7000以上、居里温度达到180℃以上时,在10kHz-400kHz的频率范围内磁导率可以始终保持7000以上。
具体实施方式
以下为本发明的具体实施方式,对本发明的技术特征做进一步的说明,但是本发明并不限于这些实施例。
实施例1
一种MnZn高磁导率高居里温度高频材料的制备方法,具体步骤如下:
(1)配料混合一磨:按照53.43mol%的Fe2O3,16.15mol%的ZnO,其余为Mn3O4,计算重量,称量,加入去离子水及适量的分散剂,在砂磨机中混合,转速*时间为1000r*30min;
(2)预烧:将步骤(1)所得粉料烘干过筛粉碎后转入马弗炉预烧,预烧温度850℃,保温两个小时;
(3)配料混合二磨:将步骤(2)所得预烧料置于球磨机,添加辅助成分包括CaCO3:200ppm,Bi2O3:600ppm,Nb2O5:20ppm,MoO3:300ppm;加入去离子水后进行球磨,转速*时间为350r*48min,得到球磨后的料浆烘干过筛,平均粒度约1±0.1μm;
(4)造粒:将步骤(3)所得的粉料,添加适量的胶水造粒;
(6)烧结:将步骤(5)压制成型的样品生坯按一定的摆放方式排列后放入推板窑内,在平衡氧气氛下进行烧结:终烧温度为1385℃;降温过程采用平衡氧分压方式控制氧含量,按平衡氧分压公式LogPO2=-A/T+B(T为绝对温度)确定氧含量:A取值14540,B取值7.6。
实施例2
一种MnZn高磁导率高居里温度高频材料的制备方法,具体步骤如下:
(1)配料混合一磨:按照53.31mol%的Fe2O3,16.57mol%的ZnO,其余为Mn3O4,计算重量,称量,加入去离子水及适量的分散剂,在砂磨机中混合,转速*时间为1000r*30min;
(2)预烧:将步骤(1)所得粉料烘干过筛粉碎后转入马弗炉预烧,预烧温度850℃,保温两个小时;
(3)配料混合二磨:将步骤(2)所得预烧料置于球磨机,添加辅助成分包括CaCO3:160ppm,Bi2O3:650ppm,Nb2O5:20ppm,MoO3:350ppm,SiO2:80ppm;加入去离子水后进行球磨,转速*时间为350r*48min,得到球磨后的料浆烘干过筛,平均粒度约1±0.1μm;
(4)造粒:将步骤(3)所得的粉料,添加适量的胶水造粒;
(6)烧结:将步骤(5)压制成型的样品生坯按一定的摆放方式排列后放入推板窑内,在平衡氧气氛下进行烧结:终烧温度为1385℃;降温过程采用平衡氧分压方式控制氧含量,按平衡氧分压公式LogPO2=-A/T+B(T为绝对温度)确定氧含量:A取值14540,B取值7.6。
实施例3
一种MnZn高磁导率高居里温度高频材料的制备方法,具体步骤如下:
(1)配料混合一磨:按照53.19mol%的Fe2O3,16.97mol%的ZnO,其余为Mn3O4,计算重量,称量,加入去离子水及适量的分散剂,在砂磨机中混合,转速*时间为1000r*30min;
(2)预烧:将步骤(1)所得粉料烘干过筛粉碎后转入马弗炉预烧,预烧温度850℃,保温两个小时;
(3)配料混合二磨:将步骤(2)所得预烧料置于球磨机,添加辅助成分包括CaCO3:200ppm,Bi2O3:500ppm,Nb2O5:80ppm,MoO3:200ppm;加入去离子水后进行球磨,转速*时间为350r*48min,得到球磨后的料浆烘干过筛,平均粒度约1±0.1μm;
(4)造粒:将步骤(3)所得的粉料,添加适量的胶水造粒;
(6)烧结:将步骤(5)压制成型的样品生坯按一定的摆放方式排列后放入推板窑内,在平衡氧气氛下进行烧结:终烧温度为1385℃;降温过程采用平衡氧分压方式控制氧含量,按平衡氧分压公式LogPO2=-A/T+B(T为绝对温度)确定氧含量:A取值14540,B取值7.6。
实施例4
一种MnZn高磁导率高居里温度高频材料的制备方法,具体步骤如下:
(1)配料混合一磨:按照52.67mol%的Fe2O3,17.3mol%的ZnO,其余为Mn3O4,计算重量,称量,加入去离子水及适量的分散剂,在砂磨机中混合,转速*时间为1000r*30min;
(2)预烧:将步骤(1)所得粉料烘干过筛粉碎后转入马弗炉预烧,预烧温度850℃,保温两个小时;
(3)配料混合二磨:将步骤(2)所得预烧料置于球磨机,添加辅助成分包括CaCO3:220ppm,Bi2O3:600ppm,Nb2O5:20ppm,MoO3:300ppm;加入去离子水后进行球磨,转速*时间为350r*48min,得到球磨后的料浆烘干过筛,平均粒度约1±0.1μm;
(4)造粒:将步骤(3)所得的粉料,添加适量的胶水造粒;
(6)烧结:将步骤(5)压制成型的样品生坯按一定的摆放方式排列后放入推板窑内,在平衡氧气氛下进行烧结:终烧温度为1385℃;降温过程采用平衡氧分压方式控制氧含量,按平衡氧分压公式LogPO2=-A/T+B(T为绝对温度)确定氧含量:A取值14540,B取值7.6。
对比例1
具体步骤如下:
(1)配料混合一磨:按照53.43mol%的Fe2O3,16.05mol%的ZnO,其余为Mn3O4,计算重量,称量,加入去离子水及适量的分散剂,在砂磨机中混合,转速*时间为1000r*30min;
(2)预烧:将步骤(1)所得粉料烘干过筛粉碎后转入马弗炉预烧,预烧温度850℃,保温两个小时;
(3)配料混合二磨:将步骤(2)所得预烧料置于球磨机,添加辅助成分包括CaCO3:200ppm,Bi2O3:600ppm,Nb2O5:20ppm,MoO3:300ppm;加入去离子水后进行球磨,转速*时间为350r*48min,得到球磨后的料浆烘干过筛,平均粒度约1±0.1μm;
(4)造粒:将步骤(3)所得的粉料,添加适量的胶水造粒;
(6)烧结:将步骤(5)压制成型的样品生坯按一定的摆放方式排列后放入推板窑内,在平衡氧气氛下进行烧结:终烧温度为1385℃;降温过程采用平衡氧分压方式控制氧含量,按平衡氧分压公式LogPO2=-A/T+B(T为绝对温度)确定氧含量:A取值14540,B取值7.6。
对比例2
具体步骤如下:
(1)配料混合一磨:按照53.53mol%的Fe2O3,15.15mol%的ZnO,其余为Mn3O4,计算重量,称量,加入去离子水及适量的分散剂,在砂磨机中混合,转速*时间为1000r*30min;
(2)预烧:将步骤(1)所得粉料烘干过筛粉碎后转入马弗炉预烧,预烧温度850℃,保温两个小时;
(3)配料混合二磨:将步骤(2)所得预烧料置于球磨机,添加辅助成分包括CaCO3:200ppm,Bi2O3:600ppm,Nb2O5:20ppm,MoO3:300ppm;加入去离子水后进行球磨,转速*时间为350r*48min,得到球磨后的料浆烘干过筛,平均粒度约1±0.1μm;
(4)造粒:将步骤(3)所得的粉料,添加适量的胶水造粒;
(6)烧结:将步骤(5)压制成型的样品生坯按一定的摆放方式排列后放入推板窑内,在平衡氧气氛下进行烧结:终烧温度为1385℃;降温过程采用平衡氧分压方式控制氧含量,按平衡氧分压公式LogPO2=-A/T+B(T为绝对温度)确定氧含量:A取值14540,B取值7.6。
对比例3
具体步骤如下:
(1)配料混合一磨:按照52.67mol%的Fe2O3,17.4mol%的ZnO,其余为Mn3O4,计算重量,称量,加入去离子水及适量的分散剂,在砂磨机中混合,转速*时间为1000r*30min;
(2)预烧:将步骤(1)所得粉料烘干过筛粉碎后转入马弗炉预烧,预烧温度850℃,保温两个小时;
(3)配料混合二磨:将步骤(2)所得预烧料置于球磨机,添加辅助成分包括CaCO3:200ppm,Bi2O3:600ppm,Nb2O5:20ppm,MoO3:300ppm;加入去离子水后进行球磨,转速*时间为350r*48min,得到球磨后的料浆烘干过筛,平均粒度约1±0.1μm;
(4)造粒:将步骤(3)所得的粉料,添加适量的胶水造粒;
(6)烧结:将步骤(5)压制成型的样品生坯按一定的摆放方式排列后放入推板窑内,在平衡氧气氛下进行烧结:终烧温度为1385℃;降温过程采用平衡氧分压方式控制氧含量,按平衡氧分压公式LogPO2=-A/T+B(T为绝对温度)确定氧含量:A取值14540,B取值7.6。
对比例4
具体步骤如下:
(1)配料混合一磨:按照52.57mol%的Fe2O3,17.3mol%的ZnO,其余为Mn3O4,计算重量,称量,加入去离子水及适量的分散剂,在砂磨机中混合,转速*时间为1000r*30min;
(2)预烧:将步骤(1)所得粉料烘干过筛粉碎后转入马弗炉预烧,预烧温度850℃,保温两个小时;
(3)配料混合二磨:将步骤(2)所得预烧料置于球磨机,添加辅助成分包括CaCO3:200ppm,Bi2O3:600ppm,Nb2O5:20ppm,MoO3:300ppm;加入去离子水后进行球磨,转速*时间为350r*48min,得到球磨后的料浆烘干过筛,平均粒度约1±0.1μm;
(4)造粒:将步骤(3)所得的粉料,添加适量的胶水造粒;
(6)烧结:将步骤(5)压制成型的样品生坯按一定的摆放方式排列后放入推板窑内,在平衡氧气氛下进行烧结:终烧温度为1385℃;降温过程采用平衡氧分压方式控制氧含量,按平衡氧分压公式LogPO2=-A/T+B(T为绝对温度)确定氧含量:A取值14540,B取值7.6。
采用Agilent-4284A精密LCR仪测量常温下样品的频率特性电感量L计算样品的初始磁导率μi,采用1061A型号精密LCR仪器测量样品温度特性电感量L计算样品的磁导率μ,测试结果如表1所示。
表1
表1所示实例中实施例1-4主成分均在本发明限定范围之内,材料性能指标完全达标。对比例1-2为Fe2O3或者ZnO含量超出本发明限定范围,导致磁晶各向异性常数补偿点偏离常温,所以二峰温度明显偏离常温,常温初始磁导率显著降低;对比例3-4因为铁锌比的改变,导致样品居里温度偏低,即使其它性能符合要求,也没有实际意义。
以上所述的仅是本发明的一些实施方式。对于本领域的普通技术人员来说,在不脱离本发明创造构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。
Claims (10)
1.一种锰锌高磁导率高居里温度高频磁性材料,其特征在于,包括主成分和辅助成分,所述主成分包括Fe2O3、ZnO和Mn3O4,所述辅助成分包括CaCO3、Bi2O3、Nb2O5、MoO3、SiO2中的三种或三种以上;所述辅助成分的总重量为所述主成分总重量的0.11wt%~0.12wt%;所述磁性材料的居里温度Tc>180℃,初始磁导率(25℃,10kHz)μi>7000,磁导率(25℃,400kHz)μ>7000。
2.根据权利要求1所述的锰锌高磁导率高居里温度高频磁性材料,其特征在于,所述主成分以各自氧化物计算分别为52.67mol%~53.43mol%的Fe2O3,16.15mol%~17.3mol%的ZnO,其余为Mn3O4;所述Fe2O3与ZnO摩尔百分数成分含量之比大于或等于3.04。
3.根据权利要求1-2任一项所述的锰锌高磁导率高居里温度高频磁性材料,其特征在于,所述材料的比损耗系数(25℃,10kHz)tanδ/μi≤4×10-6。
4.根据权利要求1-3任一项所述的锰锌高磁导率高居里温度高频磁性材料,其特征在于,所述主成分各组分原料纯度99wt%以上。
5.根据权利要求1所述的锰锌高磁导率高居里温度高频磁性材料,其特征在于,基于所述总重量,所述辅助成分添加量范围为CaCO3:160ppm~220ppm,Bi2O3:500ppm~650ppm,Nb2O5:20ppm~80ppm,MoO3:200ppm~350ppm,SiO2:0ppm~80ppm。
6.一种权利要求1-5所述锰锌高磁导率高居里温度高频磁性材料的制备方法,包括以下步骤:
(1)配料混合一磨:按主成分配比称量Fe2O3、ZnO和Mn3O4;取所述主成分重量100wt%~110wt%的去离子水、消泡剂与分散剂的混合物于砂磨机中混合,混合时间30min,转速1000r/min;
(2)预烧:将步骤(1)所得粉料置入马弗炉预烧,预烧温度800~850℃,预烧时间2个小时;
(3)配料混合二磨:将步骤(2)所得预烧料中添加辅助成分,加入粉料重量60wt%~70wt%的去离子水后进行球磨,球磨时间48min,得到球磨后的料浆;
(4)造粒:将步骤(3)所得的料浆烘干过筛后添加适量的胶水进行造粒;
(5)压制:用步骤(4)所得的粉料进行压制成型为标准样品生坯;
(6)烧结:将步骤(5)压制成型的样品生坯在平衡氧气氛中进行烧结,终烧温度控制在1350~1390℃。
7.根据权利要求6所述的锰锌高磁导率高居里温度高频磁性材料的制备方法,其特征在于:所述主成分配比为以各自氧化物计算52.67mol%~53.43mol%Fe2O3,16.15mol%~17.3mol%的ZnO,其余为Mn3O4;所述辅助成分包括碳酸钙CaCO3、氧化铋Bi2O3、五氧化二铌Nb2O5、氧化钼MoO3、二氧化硅SiO2中的三种或三种以上。
8.根据权利要求6所述的锰锌高磁导率高居里温度高频磁性材料的制备方法,其特征在于:所述消泡剂为有机硅类消泡剂;所述分散剂选自柠檬酸盐、十二烷基磺酸盐,1-甲基戊醇中的一种或多种。
9.根据权利要求6所述的锰锌高磁导率高居里温度高频磁性材料的制备方法,其特征在于:在所述步骤(3)中球磨后的浆料平均粒度控制在1±0.1μm。
10.根据权利要求6所述的锰锌高磁导率高居里温度高频磁性材料的制备方法,其特征在于:所述平衡氧分压按公式LogPO2=-A/T+B计算,确定氧含量:A取值10000~15000,B取值5~10。
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