CN105601263A - 一种高性能功率锰锌软磁铁氧体材料及其制备方法 - Google Patents
一种高性能功率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性能功率锰锌软磁铁氧体材料及其制备方法,包括主体体系和掺杂体系;所述主体体系和掺杂体系的质量比为30~38:1;所述制备方法为:(1)称料;(2)预烧;(3)混合研磨;(4)制浆;(5)压饼坯晾干;(6)二次预烧;(7)二次球磨;(8)干压成型;(9)烧结。本发明一种高性能功率锰锌软磁铁氧体材料及其制备方法,制备简便,容易实现,其通过科学的配方设计和合理的烧结工艺,使所制备的锰锌软磁铁氧体材料具备优异的饱和磁通密度和较低的功率损耗,适用于当前科技环境下的使用要求,市场前景广阔。
Description
技术领域
本发明涉及锰锌磁铁氧体材料领域,特别是涉及一种高性能功率锰锌软磁铁氧体材料及其制备方法。
背景技术
软磁材料在工业中的应用是伴随着电力电工及电讯技术的兴起而出现的,最早应用始于十九世纪末。软磁材料可应用于家电领域、信息化领域、汽车领域和其他配套领域。随着现代电子技术的快速发展,软磁材料中的高磁导率锰锌铁氧体得到飞速发展,应用范围由原来的脉冲变压器逐步扩大到电磁滤波器、扼流圈、感应器等领域,应用领域越来越广,其市场需求量逐年上升,产品种类也日益增多,成为磁性材料行业发展的一大亮点。
随着铁氧体材料应用范围的扩大及电子设备的发展,对铁氧体材料的性能要求也越来越高,如频率稳定性、温度稳定性、时间稳定性等,以满足电子行业发展的需求及应用环境变化对产品适应性能的挑战。
发明内容
本发明主要解决的技术问题是提供一种高性能功率锰锌软磁铁氧体材料及其制备方法,能够解决当前科技环境下对锰锌铁氧体材料性能的要求。
为解决上述技术问题,本发明采用的一个技术方案是:提供一种高性能功率锰锌软磁铁氧体材料,包括:主体体系和掺杂体系;所述主体体系和掺杂体系的质量比为30~38:1;所述主体体系由如下组分构成:精铁矿粉43~44.5mol%、Mn3O426.5~28.5mol%,其余为ZnO;所述掺杂体系包括CaCO3、ZrO2、MoO3、碳纳米管、Bi2O3、CaO、SnO和TiO2。
在本发明一个较佳实施例中,所述CaCO3、ZrO2、MoO3、碳纳米管、Bi2O3、CaO、SnO和TiO2的质量比为3~5:1~2:0.8~1.5:0.5~1.3:2~3:8~12:0.3~0.8:1~2.5。
为解决上述技术问题,本发明采用的另一个技术方案是:一种高性能功率锰锌软磁铁氧体材料及其制备方法,包括如下步骤:
(1)称料:按配方称取主体体系和掺杂体系的各组分备用;
(2)预烧:将步骤(1)中称取的主体体系的各组分加入马弗炉中,在一定条件下预烧;
(3)混合研磨:将步骤(2)中预烧后的主体体系转入球磨机内,先研磨30~60min,然后边研磨边缓慢加入步骤(1)中称好的掺杂体系,加毕,混合研磨1~3h;
(4)制浆:向步骤(3)中研磨后的混合物料中加入占物料总重量50%的水,搅拌形成混合液,再加入一定量分散剂溶液,搅拌混合成为浆料;
(5)压饼坯晾干:将步骤(4)中研磨后的混合浆料压滤制成坯块,然后将坯块晾晒5~9h;
(6)二次预烧:将步骤(5)中得到的坯块放入程序烧结炉内,采用平衡氧分压法预烧;
(7)二次球磨:将步骤(6)中得到的坯块放入球磨机内,研磨30~60min;
(8)干压成型:将步骤(7)中得到物料放入模具,干压成型;
(9)烧结:将步骤(8)中得到的坯块放入程序烧结炉内,采用平衡氧分压法烧结,制得高性能功率锰锌软磁铁氧体材料。
在本发明一个较佳实施例中,所述步骤(2)中,所述预烧工艺为:温度1000~1100℃,保温时间2~5h。
在本发明一个较佳实施例中,所述步骤(3)中,所述研磨速率为150~300r/min,所述掺杂体系的加入速率为3~10g/min。
在本发明一个较佳实施例中,所述步骤(4)中,所述分散剂为质量浓度为10~15%的PVA溶液,其加入量占所述物料总重量的3~5%。
在本发明一个较佳实施例中,所述步骤(6)中,所述预烧工艺条件为:氧气含量为0.10~0.18%,以100~200℃/min的速率从室温升温至850~1050℃,恒温保持30~60min,再以30~50℃/min的速率升温至1250℃,恒温烧结1~3h,然后以30~50℃/min的速率从1200℃降温至500℃,再关闭电源,随炉冷却至室温。
在本发明一个较佳实施例中,所述步骤(7)中,所述研磨速率为400~600r/min。
在本发明一个较佳实施例中,所述步骤(9)中,所述烧结工艺条件为:氧气含量为0.10~0.25%,以100~200℃/min的速率从室温升温至1200~1400℃,恒温保持30~40min,然后以30~50℃/min的速率从1400℃降温至500℃,再关闭电源,随炉冷却至室温。
本发明的有益效果是:本发明一种高性能功率锰锌软磁铁氧体材料及其制备方法,制备简便,容易实现,其通过科学的配方设计和合理的烧结工艺,使所制备的锰锌软磁铁氧体材料具备优异的饱和磁通密度和较低的功率损耗,适用于当前科技环境下的使用要求,市场前景广阔。
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:
实施例1
一种高性能功率锰锌软磁铁氧体材料,包括:主体体系和掺杂体系;所述主体体系和掺杂体系的质量比为38:1;所述主体体系由如下组分构成:精铁矿粉43mol%、Mn3O426.5mol%,其余为ZnO;所述掺杂体系包括质量比为5:2:1.5:1.3:3:12:0.8:2.5的CaCO3、ZrO2、MoO3、碳纳米管、Bi2O3、CaO、SnO和TiO2。
上述高性能功率锰锌软磁铁氧体材料的制备方法,包括如下步骤:
(1)称料:按配方称取主体体系和掺杂体系的各组分备用;
(2)预烧:将步骤(1)中称取的主体体系的各组分加入马弗炉中,在温度1100℃下预烧,保温时间5h;
(3)混合研磨:将步骤(2)中预烧后的主体体系转入球磨机内,研磨速率为300r/min,先研磨60min,然后边研磨边缓慢加入步骤(1)中称好的掺杂体系,所述掺杂体系的加入速率为3g/min,加毕,混合研磨1h;
(4)制浆:向步骤(3)中研磨后的混合物料中加入占物料总重量50%的水,搅拌形成混合液,再加入质量浓度为15%的PVA溶液的分散剂溶液,加入量占所述物料总重量的5%,搅拌混合成为浆料;
(5)压饼坯晾干:将步骤(4)中研磨后的混合浆料压滤制成坯块,然后将坯块晾晒5~9h;
(6)二次预烧:将步骤(5)中得到的坯块放入程序烧结炉内,采用平衡氧分压法预烧。条件为:氧气含量为0.18%,以200℃/min的速率从室温升温至1050℃,恒温保持30min,再以50℃/min的速率升温至1250℃,恒温烧结1h,然后以50℃/min的速率从1200℃降温至500℃,再关闭电源,随炉冷却至室温;
(7)二次球磨:将步骤(6)中得到的坯块放入球磨机内,研磨速率为400r/min,研磨60min;
(8)干压成型:将步骤(7)中得到物料放入模具,干压成型;
(9)烧结:将步骤(8)中得到的坯块放入程序烧结炉内,采用平衡氧分压法烧结,所述烧结工艺条件为:氧气含量为0.25%,以200℃/min的速率从室温升温至1400℃,恒温保持40min,然后以50℃/min的速率从1400℃降温至500℃,再关闭电源,随炉冷却至室温,制得高性能功率锰锌软磁铁氧体材料。
实施例2
一种高性能功率锰锌软磁铁氧体材料,包括:主体体系和掺杂体系;所述主体体系和掺杂体系的质量比为30:1;所述主体体系由如下组分构成:精铁矿粉44.5mol%、Mn3O428.5mol%,其余为ZnO;所述掺杂体系包括质量比为3:1:0.8:0.5:2:8:0.3:1的CaCO3、ZrO2、MoO3、碳纳米管、Bi2O3、CaO、SnO和TiO2。
上述高性能功率锰锌软磁铁氧体材料的制备方法,包括如下步骤:
(1)称料:按配方称取主体体系和掺杂体系的各组分备用;
(2)预烧:将步骤(1)中称取的主体体系的各组分加入马弗炉中,在温度1000℃下预烧,保温时间2h;
(3)混合研磨:将步骤(2)中预烧后的主体体系转入球磨机内,研磨速率为150r/min,先研磨30~60min,然后边研磨边缓慢加入步骤(1)中称好的掺杂体系,所述掺杂体系的加入速率为3g/min,加毕,混合研磨3h;
(4)制浆:向步骤(3)中研磨后的混合物料中加入占物料总重量50%的水,搅拌形成混合液,再加入质量浓度为10%的PVA溶液的分散剂溶液,加入量占所述物料总重量的3%,搅拌混合成为浆料;
(5)压饼坯晾干:将步骤(4)中研磨后的混合浆料压滤制成坯块,然后将坯块晾晒5~9h;
(6)二次预烧:将步骤(5)中得到的坯块放入程序烧结炉内,采用平衡氧分压法预烧。条件为:氧气含量为0.10%,以100℃/min的速率从室温升温至850℃,恒温保持30min,再以30℃/min的速率升温至1250℃,恒温烧结3h,然后以30℃/min的速率从1200℃降温至500℃,再关闭电源,随炉冷却至室温;
(7)二次球磨:将步骤(6)中得到的坯块放入球磨机内,研磨速率为600r/min,研磨30min;
(8)干压成型:将步骤(7)中得到物料放入模具,干压成型;
(9)烧结:将步骤(8)中得到的坯块放入程序烧结炉内,采用平衡氧分压法烧结,所述烧结工艺条件为:氧气含量为0.10%,以100℃/min的速率从室温升温至1200℃,恒温保持30min,然后以30℃/min的速率从1400℃降温至500℃,再关闭电源,随炉冷却至室温,制得高性能功率锰锌软磁铁氧体材料。
上述方法制得的锰锌铁氧铁,经检测,其在25℃时的饱和磁通密度为880~1000mT,100℃的饱和磁通密度为850~1000mT;100℃,100kHz,200mT条件下的功率损耗小于220kW/m3。
以上所述仅为本发明的实施例,并非因此限制本发明的专利范围,凡是利用本发明说明书内容所作的等效结构或等效流程变换,或直接或间接运用在其他相关的技术领域,均同理包括在本发明的专利保护范围内。
Claims (9)
1.一种高性能功率锰锌软磁铁氧体材料,其特征在于,包括:主体体系和掺杂体系;所述主体体系和掺杂体系的质量比为30~38:1;所述主体体系由如下组分构成:精铁矿粉43~44.5mol%、Mn3O426.5~28.5mol%,其余为ZnO;所述掺杂体系包括CaCO3、ZrO2、MoO3、碳纳米管、Bi2O3、CaO、SnO和TiO2。
2.根据权利要求1所述的高性能功率锰锌软磁铁氧体材料,其特征在于,所述CaCO3、ZrO2、MoO3、碳纳米管、Bi2O3、CaO、SnO和TiO2的质量比为3~5:1~2:0.8~1.5:0.5~1.3:2~3:8~12:0.3~0.8:1~2.5。
3.一种如权利要求1或2所述的高性能功率锰锌软磁铁氧体材料制备方法,其特征在于,包括如下步骤:
(1)称料:按配方称取主体体系和掺杂体系的各组分备用;
(2)预烧:将步骤(1)中称取的主体体系的各组分加入马弗炉中,在一定条件下预烧;
(3)混合研磨:将步骤(2)中预烧后的主体体系转入球磨机内,先研磨30~60min,然后边研磨边缓慢加入步骤(1)中称好的掺杂体系,加毕,混合研磨1~3h;
(4)制浆:向步骤(3)中研磨后的混合物料中加入占物料总重量50%的水,搅拌形成混合液,再加入一定量分散剂溶液,搅拌混合成为浆料;
(5)压饼坯晾干:将步骤(4)中研磨后的混合浆料压滤制成坯块,然后将坯块晾晒5~9h;
(6)二次预烧:将步骤(5)中得到的坯块放入程序烧结炉内,采用平衡氧分压法预烧;
(7)二次球磨:将步骤(6)中得到的坯块放入球磨机内,研磨30~60min;
(8)干压成型:将步骤(7)中得到物料放入模具,干压成型;
(9)烧结:将步骤(8)中得到的坯块放入程序烧结炉内,采用平衡氧分压法烧结,制得高性能功率锰锌软磁铁氧体材料。
4.根据权利要求3所述的高性能功率锰锌软磁铁氧体材料制备方法,其特征在于,所述步骤(2)中,所述预烧工艺为:温度1000~1100℃,保温时间2~5h。
5.根据权利要求3所述的高性能功率锰锌软磁铁氧体材料制备方法,其特征在于,所述步骤(3)中,所述研磨速率为150~300r/min,所述掺杂体系的加入速率为3~10g/min。
6.根据权利要求3所述的高性能功率锰锌软磁铁氧体材料制备方法,其特征在于,所述步骤(4)中,所述分散剂为质量浓度为10~15%的PVA溶液,其加入量占所述物料总重量的3~5%。
7.根据权利要求3所述的高性能功率锰锌软磁铁氧体材料制备方法,其特征在于,所述步骤(6)中,所述预烧工艺条件为:氧气含量为0.10~0.18%,以100~200℃/min的速率从室温升温至850~1050℃,恒温保持30~60min,再以30~50℃/min的速率升温至1250℃,恒温烧结1~3h,然后以30~50℃/min的速率从1200℃降温至500℃,再关闭电源,随炉冷却至室温。
8.根据权利要求3所述的高性能功率锰锌软磁铁氧体材料制备方法,其特征在于,所述步骤(7)中,所述研磨速率为400~600r/min。
9.根据权利要求3所述的高性能功率锰锌软磁铁氧体材料制备方法,其特征在于,所述步骤(9)中,所述烧结工艺条件为:氧气含量为0.10~0.25%,以100~200℃/min的速率从室温升温至1200~1400℃,恒温保持30~40min,然后以30~50℃/min的速率从1400℃降温至500℃,再关闭电源,随炉冷却至室温。
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