CN111039669A - 高强度抗变形锰锌铁氧体及其制备方法 - Google Patents
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Abstract
本发明公开了一种高强度抗变形锰锌铁氧体及其制备方法,包括主成分和辅助成分;所述主成分以各自氧化物计算,包括69~71mol%的Fe2O3,7~15mol%的ZnO,其余为MnO,总量为100%;所述辅助组分的总重量为所述主成分总重量的0.15~0.5wt%,所述辅助成分包括CaCO3、TiO2、Nb2O5、Co2O3、B2O3、V2O5中的三种或三种以上。本发明通过特殊的掺杂工艺及烧结工艺曲线设计,使得所制备的锰锌铁氧体材料具有较高的磁导率特性,磁芯强度高,功耗低,且具有良好的温升特性,温度曲线平坦、高温功耗低,工作环境适应性强,可广泛应用于汽车电子领域,无线充电领域,通讯设备领域。
Description
技术领域
本发明涉及磁性材料领域,特别是涉及一种高强度抗变形锰锌铁氧体及其制备方法。
背景技术
随着汽车电子设备产业的高速发展,相关产品越来越趋于高效、低能耗、抗干扰方向,同时也给磁芯提出了新的要求。软磁铁氧体由于其成本方面的优势,越来越多的软磁用于替换传统磁芯,同时软磁具有良好的配合特性,也能帮助元器件实现更好的特性。
现有软磁磁芯存在磁滞密度低,磁芯强度不高等缺陷,不利于相关电子元气件更好的向高效、低能耗和抗干扰方向的发展。
发明内容
本发明主要解决的技术问题是提供一种高强度抗变形锰锌铁氧体及其制备方法,能够有效解决现有软磁磁芯存在的上述问题,为客户终端提供更好的元件解决方案。
为解决上述技术问题,本发明采用的一个技术方案是:提供一种高强度抗变形锰锌铁氧体,包括:主成分和辅助成分;所述主成分以各自氧化物计算,包括69~71mol%的Fe2O3,7~15mol%的ZnO,其余为MnO,总量为100%;所述辅助组分的总重量为所述主成分总重量的0.15~0.5wt%,所述辅助成分包括CaCO3、TiO2、Nb2O5、Co2O3、B2O3、V2O5中的三种或三种以上。
在本发明一个较佳实施例中,所述主组分的纯度为99.5wt%以上;其中,所述MnO的氧化物为Mn3O4,其比表面积为14~16 m2/g。
为解决上述技术问题,本发明采用的另一个技术方案是:提供一种高强度抗变形锰锌铁氧体的制备方法,包括如下步骤:
(1)配料混合:按配方量称取所述主成分中的各组分混合,然后称取占所述主成分总重量60~100%的去离子水及适量的消泡剂和分散剂于砂磨机中混合10~30min,加入适量的PVA水溶液后,喷雾造粒;
(2)预烧:将步骤(1)所得的粒料转入回转窑中进行预烧;
(3)粉碎:将步骤(2)所得的预烧料先置入振磨机内进行粗粉碎,再置于砂磨机内进行细粉碎;然后加入配方量的辅助成分及一定量的去离子水进行砂磨60~100min,得到砂磨后的料浆;
(4)喷雾造粒:将步骤(3)所得的料浆进行喷雾造粒,然后添加硬脂酸锌,混合整粒;
(5)毛坯成型:用步骤(4)所得的粉料进行压制成型为T25-15-10标准样品生坯或I84-15-5样品生坯;
(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钟罩炉内,采用平衡氧气氛进行烧结,得到所述高强度抗变形锰锌铁氧体。
在本发明一个较佳实施例中,所述步骤(2)中,所述预烧的工艺条件为:预烧温度900~1100℃,回转窑转速为3~5r/min,出料量350~550kg/h。
在本发明一个较佳实施例中,所述步骤(3)中,所述粗粉碎的时间10~40min;所述细粉碎的时间为60~90min,细粉碎后的物料粒径为1.0~1.2μm。
在本发明一个较佳实施例中,所述步骤(3)中,所述去离子水的加入量为细粉碎后所述粉料重量的50~100wt%。
在本发明一个较佳实施例中,所述步骤(4)中,所述硬脂酸锌的加入量为所得粒料的0.01~0.02wt%。
在本发明一个较佳实施例中,所述步骤(5)中,所述生坯的压制密度为2 .95~3.15g/cm3。
在本发明一个较佳实施例中,所述步骤(6)中,所述烧结的工艺条件:在空气环境下,以5~10℃/min的速率从室温升高至900~1100℃,在此温度下加大空气的进气量,以3~5℃/min的升温速率继续升温至1360~1400℃,恒温烧结5~6h。
在本发明一个较佳实施例中,在900~1100℃下,所述空气的进气总量为1000~1500升/小时。
本发明的有益效果是:本发明一种高强度抗变形锰锌铁氧体,通过特殊的掺杂工艺及烧结工艺曲线设计,使得所制备的锰锌铁氧体材料具有较高的磁导率特性,磁芯强度高,功耗低,且具有良好的温升特性,温度曲线平坦、高温功耗低,工作环境适应性强,可广泛应用于汽车电子领域,无线充电领域,通讯设备领域,应用领域广泛,实用性强。
具体实施方式
下面对本发明的较佳实施例进行详细阐述,以使本发明的优点和特征能更易于被本领域技术人员理解,从而对本发明的保护范围做出更为清楚明确的界定。
本发明实施例包括:
本发明揭示了一种高强度抗变形锰锌铁氧体,包括:主成分和辅助成分。
其中,所述主成分以各自氧化物计算,包括69~71mol%的Fe2O3,7~15mol%的ZnO,其余为MnO,总量为100%。所述主组分的纯度为99.5wt%以上;其中,所述MnO的氧化物为Mn3O4,其比表面积为14~16 m2/g。通过高纯度的主成分的选用,能够有效保证成型的锰锌铁氧体的性能。
所述辅助组分的总重量为所述主成分总重量的0.15~0.5wt%。具体地,所述辅助成分包括CaCO3、TiO2、Nb2O5、Co2O3、B2O3、V2O5中的三种或三种以上。
其中,所述CaCO3在第二次粉碎时加入,烧结时往往不进入晶体内部而存在于晶界上,对生成大晶粒有抑止作用,同时对提高电阻率有比较明显的效果。
所述TiO2的少量加入,能够降低终烧温度并使功耗下降,由于它是四价元素,使二峰向低温方向移动。
所述Nb2O5的少量加入,可以使晶粒细化,提高Q值;在功率铁氧体中加入少量五氧化二铌,可使功耗下降并改善功耗频率特性;它还可以加在其他软磁铁氧体中,提高其磁特性。
所述Co2O3在软磁铁氧体中,能够改善磁导率的温度系数和提高Q值。
所述V2O5 又名钒酸酐,可由灼烧钒酸铵而得。在功率铁氧体中常加入适量五氧化二钒,可以提高密度、降低终烧温度,使材料的磁特性改善,并能增加机械强度和抗冷热冲击特性。
所述B2O3 又名硼酐,在锰锌铁氧体中作为助熔剂,可降低终烧温度和提高磁芯的密度。
实施例1
高强度抗变形锰锌铁氧体,包括:主成分和辅助成分;其中,所述主成分以各自氧化物计算,纯度为99.5wt%以上,包括69mol%的Fe2O3,15mol%的ZnO和16mol%的MnO。所述辅助组分的总重量为所述主成分总重量的0.15wt%。具体地,所述辅助成分包括质量比例为1:0.5:0.5:0.3的CaCO3、Nb2O5、B2O3和V2O5。
上述高强度抗变形锰锌铁氧体的制备方法,包括如下步骤:
(1)配料混合:按配方量称取所述主成分中的各组分混合,然后称取占所述主成分总重量60~100%的去离子水及占所述主成分总重量4%的消泡剂和4%的分散剂于砂磨机中混合10~30min,加入占所述主成分总重量8%的质量浓度为10%的PVA水溶液后,搅拌均匀,喷雾造粒;
(2)预烧:将步骤(1)所得的粒料转入回转窑中,以900℃的预烧温度,3r/min的回转窑转速,在出料量350kg/h的条件下进行预烧;
(3)粉碎:将步骤(2)所得的预烧料先置入振磨机内进行粗粉碎10~40min;,再置于砂磨机内进行细粉碎60~90min,使细粉碎后的物料粒径为1.0~1.2μm;然后加入配方量的辅助成分及占细粉碎后所述粉料重量的50wt%的去离子水进行砂磨60~100min,得到砂磨后的料浆;
(4)喷雾造粒:将步骤(3)所得的料浆进行喷雾造粒,然后添加占所得粒料0.01wt%的硬脂酸锌,混合整粒;
(5)毛坯成型:用步骤(4)所得的粉料进行压制成型为T25-15-10标准样品生坯或I84-15-5样品生坯;
(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钟罩炉内,采用平衡氧气氛进行烧结,得到所述高强度抗变形锰锌铁氧体。
所述烧结的工艺条件为:在空气环境下,以5℃/min的速率从室温升高至900℃,在此温度下加大空气的进气量,使进气总量为1000升/小时,并以3℃/min的升温速率继续升温至1360±5℃,恒温烧结6h。
上述方法制备得到的高强度抗变形锰锌铁氧体,经测试,其性能如下:
初始磁导率μi=3400±25% (1.0KHz,0.3V, 25±3℃);
适合工作温度:-30℃~160℃;
功耗: 25℃、100℃下均小于450kW/m3;120℃下小于500kW/m3 (100KHZ,200mT)
饱和磁通密度:Bs>510mT (1194A/m,25±3℃)
磁芯强度特性: F>100N。
实施例2
高强度抗变形锰锌铁氧体,包括:主成分和辅助成分;其中,所述主成分以各自氧化物计算,纯度为99.5wt%以上,包括71mol%的Fe2O3,7mol%的ZnO和22mol%的MnO。所述辅助组分的总重量为所述主成分总重量的0.15wt%。具体地,所述辅助成分包括质量比例为1:0.5:0.5:0.3的CaCO3、Co2O3、B2O3和V2O5。
上述高强度抗变形锰锌铁氧体的制备方法,包括如下步骤:
(1)配料混合:按配方量称取所述主成分中的各组分混合,然后称取占所述主成分总重量60~100%的去离子水及占所述主成分总重量3%的消泡剂和5%的分散剂于砂磨机中混合10~30min,加入占所述主成分总重量10%的质量浓度为15%的PVA水溶液后,搅拌均匀,喷雾造粒;
(2)预烧:将步骤(1)所得的粒料转入回转窑中,以1100℃的预烧温度, 5r/min的回转窑转速,在出料量550kg/h的条件下进行预烧;
(3)粉碎:将步骤(2)所得的预烧料先置入振磨机内进行粗粉碎10~40min;;再置于砂磨机内进行细粉碎60~90min,使细粉碎后的物料粒径为1.0~1.2μm;然后加入配方量的辅助成分及占细粉碎后所述粉料重量的100wt%的去离子水进行砂磨60~100min,得到砂磨后的料浆;
(4)喷雾造粒:将步骤(3)所得的料浆进行喷雾造粒,然后添加占所得粒料0.02wt%的硬脂酸锌,混合整粒;
(5)毛坯成型:用步骤(4)所得的粉料进行压制成型为T25-15-10标准样品生坯或I84-15-5样品生坯;
(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钟罩炉内,采用平衡氧气氛进行烧结,得到所述高强度抗变形锰锌铁氧体。
所述烧结的工艺条件:在空气环境下,以10℃/min的速率从室温升高至1100℃,在此温度下加大空气的进气量,使进气总量为1500升/小时,以5℃/min的升温速率继续升温至1400±5℃,恒温烧结5h。
上述方法制备得到的高强度抗变形锰锌铁氧体,经测试,其性能如下:
初始磁导率μi=3450±25% (1.0KHz,0.3V, 25±3℃);
适合工作温度:-30℃~160℃;
功耗: 25℃、100℃下均小于450kW/m3;120℃下小于500kW/m3 (100KHZ,200mT)
饱和磁通密度:Bs>530mT (1194A/m,25±3℃)
磁芯强度特性: F>120N。
本发明通过特殊的掺杂工艺及烧结工艺曲线设计,在常温条件下具备较高的磁导率特性(μi=3400±25%),磁芯功耗低,且具有良好的温升特性,温度曲线平坦、高温功耗低,工作环境适应性强。
该材料要求较高的磁芯强度特性以满足车载器件要求。
本发明的制备方法可批量生产功率型锰锌铁氧体,可广泛应用于汽车电子领域,无线充电领域,通讯设备领域,应用领域广泛,实用性强。
以上所述仅为本发明的优选实施例而已,并不用于限制本发明,对于本领域的技术人员来说,本发明可以有各种更改和变化。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.一种高强度抗变形锰锌铁氧体,其特征在于,包括:主成分和辅助成分;所述主成分以各自氧化物计算,包括69~71mol%的Fe2O3,7~15mol%的ZnO,其余为MnO,总量为100%;所述辅助组分的总重量为所述主成分总重量的0.15~0.5wt%,所述辅助成分包括CaCO3、TiO2、Nb2O5、Co2O3、B2O3、V2O5中的三种或三种以上。
2.根据权利要求1所述的高强度抗变形锰锌铁氧体,其特征在于,所述主组分的纯度为99.5wt%以上;其中,所述MnO的氧化物为Mn3O4,其比表面积为14~16 m2/g。
3.一种高强度抗变形锰锌铁氧体的制备方法,其特征在于,包括如下步骤:
(1)配料混合:按配方量称取所述主成分中的各组分混合,然后称取占所述主成分总重量60~100%的去离子水及适量的消泡剂和分散剂于砂磨机中混合10~30min,加入适量的PVA水溶液后,喷雾造粒;
(2)预烧:将步骤(1)所得的粒料转入回转窑中进行预烧;
(3)粉碎:将步骤(2)所得的预烧料先置入振磨机内进行粗粉碎,再置于砂磨机内进行细粉碎;然后加入配方量的辅助成分及一定量的去离子水进行砂磨60~100min,得到砂磨后的料浆;
(4)喷雾造粒:将步骤(3)所得的料浆进行喷雾造粒,然后添加硬脂酸锌,混合整粒;
(5)毛坯成型:用步骤(4)所得的粉料进行压制成型为T25-15-10标准样品生坯或I84-15-5样品生坯;
(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钟罩炉内,采用平衡氧气氛进行烧结,得到所述高强度抗变形锰锌铁氧体。
4.根据权利要求3所述的高强度抗变形锰锌铁氧体的制备方法,其特征在于,所述步骤(2)中,所述预烧的工艺条件为:预烧温度900~1100℃,回转窑转速为3~5r/min,出料量350~550kg/h。
5.根据权利要求3所述的高强度抗变形锰锌铁氧体的制备方法,其特征在于,所述步骤(3)中,所述粗粉碎的时间10~40min;所述细粉碎的时间为60~90min,细粉碎后的物料粒径为1.0~1.2μm。
6.根据权利要求3所述的高强度抗变形锰锌铁氧体的制备方法,其特征在于,所述步骤(3)中,所述去离子水的加入量为细粉碎后所述粉料重量的50~100wt%。
7.根据权利要求3所述的高强度抗变形锰锌铁氧体的制备方法,其特征在于,所述步骤(4)中,所述硬脂酸锌的加入量为所得粒料的0.01~0.02wt%。
8.根据权利要求3所述的高强度抗变形锰锌铁氧体的制备方法,其特征在于,所述步骤(5)中,所述生坯的压制密度为2 .95~3.15g/cm3。
9.根据权利要求3所述的高强度抗变形锰锌铁氧体的制备方法,其特征在于,所述步骤(6)中,所述烧结的工艺条件:在空气环境下,以5~10℃/min的速率从室温升高至900~1100℃,在此温度下加大空气的进气量,以3~5℃/min的升温速率继续升温至1360~1400℃,恒温烧结5~6h。
10.根据权利要求9所述的高强度抗变形锰锌铁氧体的制备方法,其特征在于,在900~1100℃下,所述空气的进气总量为1000~1500升/小时。
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