CN108565109B - 一种软磁复合材料的制备方法 - Google Patents
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Abstract
本发明涉及一种软磁复合材料的制备方法。软磁复合材料以片状Fe、Fe‑Si、Fe‑Ni、Fe‑Ni‑Mo、Fe‑Si‑Al、非晶纳米晶软磁合金粉末为原材料;将钝化剂和软磁合金粉末混合,经搅拌、烘干,得到钝化粉;将钝化粉装入成型模具中,在压制过程中施加外磁场取向;磁场取向方式有2种:或沿磁环平面方向旋转样品或旋转磁场,或采用径向4磁极对样品进行对向交替充磁取向;采用B2O3、V2O5、Bi2O3、Na2CO3、Mn2O3、Sb2O3、CuO和低熔点玻璃粉等低熔点化合物将磁环表面包覆,经400~1000℃真空退火1~48h,使低熔点化合物经颗粒界面扩散至磁环内部,提高磁体电阻率,炉冷至室温,获得软磁复合材料。本发明的优点是:片状结构可有效降低涡流损耗,提高磁导率;经界面处渗透扩散得到的绝缘层非常薄,磁环磁导率高。
Description
技术领域
本发明涉及一种软磁复合材料的制备方法,属于磁性材料制备领域。
背景技术
软磁材料,指的是当磁化发生在Hc不大于1000A/m,这样的材料称为软磁体。典型的软磁材料,可以用最小的外磁场实现最大的磁化强度。软磁材料(soft magneticmaterial)具有低矫顽力和高磁导率的磁性材料。软磁材料易于磁化,也易于退磁,广泛用于电工设备和电子设备中。
软磁材料主要包括金属软磁和铁氧体软磁。金属软磁的优点是饱和磁化强度高,但电阻率低,因此高频涡流损耗高。软磁铁氧体饱和磁通密度低,磁导率低,居里温度低,中高频损耗低,成本低。前三个低是它的缺点,限制了它的使用范围,现在(21世纪初)正在努力改进。后两个低是它的优点,有利于进入高频市场,现在(21世纪初)正在努力扩展。
软磁复合材料是由铁磁性粉粒与绝缘介质混合压制而成的一种软磁材料。与传统的金属软磁合金和铁氧体材料相比,它有很多独特的优点:磁性金属粒子分散在非导体物件中,可以减少高频涡流损耗,提高应用频率;既可以采取热压法加工成粉芯,也可以利用现在(21世纪初)的塑料工程技术,注塑制造成复杂形状的磁体;具有密度小,重量轻,生产效率高,成本低,产品重复性和一致性好等优点。缺点是由于磁性粒子之间被非磁性体分开,磁路隔断,磁导率通常较低。
软磁复合材料的工作重点集中在磁性相成分设计、界面绝缘包覆和磁体工艺优化三个方面,以提高磁性能,改善磁通密度、磁导率和磁损耗特性。首先,磁性相成分设计主要从软磁合金自身出发,通过添加元素改善合金的磁导率、矫顽力及电阻率等特性。其次,界面绝缘包覆是软磁复合材料的研究重点,通过对软磁颗粒充分绝缘隔离,提高电阻率、降低涡流损耗;良好的包覆层应厚度薄以保证高磁导率,结构完整以保证充分的绝缘包覆;绝缘包覆材料既可以为无机物(玻璃粉、水玻璃、MgO、SiO2和Al2O3等)、有机物(环氧树脂、酚醛树脂和有机硅等),也可以为有机无机复合包覆。再次,工艺优化主要通过调整制备参数,优化材料微观结构,提升磁性能。
软磁复合材料磁性能虽不断提升,但自身结构导致材料磁导率低。基于两个因素:一、合金颗粒被非磁性绝缘层隔开,磁路隔断、磁阻高;二、非磁性界面导致磁化过程中合金颗粒内出现自由磁极,局域退磁场大。高磁阻与局域退磁场效应的共同作用导致磁导率降低、磁滞损耗增大。磁阻与磁路中非磁性绝缘层总厚度直接相关,而退磁场由合金颗粒形状决定,因此软磁复合材料的低磁导率是由自身结构所必然导致。如何通过优化组织结构以降低局域退磁场和磁阻,是提升材料磁导率降低损耗的关键。
中国专利2012104332238利用磁场使磁性颗粒沿磁场方向形成链状团簇,进行获得单向透光特性;中国专利2009101405358 、2016110014476、2016110015356、2016110017173采用片状软磁合金或铁氧体在聚合物或石蜡基体中磁场取向来获得复合材料,取向有序结构对材料的磁导率或损耗有一定优化,但基体中非磁性相含量依然过高,磁导率低、高频损耗高的缺点依然没有本质改善。
另一方面,现在的工艺是将绝缘介质与金属磁粉混合后压制成型。但绝缘介质与金属磁粉的包覆界面在压制过程中容易产生脱离,形成不均匀包覆,致使涡流损耗偏高。
针对软磁复合材料存在的问题,本申请采用片状合金磁粉压制过程中经磁场取向成型、绝缘介质磁体表面涂覆、真空退火使绝缘介质产生界面扩散的工艺方法,提高磁体电阻率。
发明内容
本发明的目的在于提供一种软磁复合材料的制备方法。
本发明的具体制备步骤为:
1)原材料准备
所采用的片状软磁合金粉末为:Fe、Fe-Si、Fe-Ni、Fe-Ni-Mo、Fe-Si-Al、非晶纳米晶合金;
所述的片状软磁合金粉末优选采用球磨法制备;
2)软磁合金粉末的钝化
将钝化剂和软磁合金粉末混合,经搅拌、烘干,得到钝化粉;
3)磁场取向成型
在磁环成型过程中,利用磁场对片状软磁合金粉末取向,获得高度有序取向的各向异性磁环;
所述磁场强度为0.1~10T;
磁场取向方式优选为:成型过程中施加磁场,磁场方向平行于磁环平面,同时沿磁环平面方向旋转样品或旋转磁场,实现片状合金颗粒的完全有序取向;
磁场取向方式优选为:成型过程中,采用径向4磁极对样品进行对向交替充磁取向,实现片状合金颗粒的完全有序取向;
4)表面包覆、界面扩散
采用低熔点化合物将磁环表面包覆,再采用真空退火工艺,使低熔点化合物经颗粒界面扩散至磁环内部,提高磁体电阻率,炉冷至室温,获得软磁复合材料;
所述的低熔点化合物包括:B2O3、V2O5、Bi2O3、Na2CO3、Mn2O3、Sb2O3、CuO和低熔点玻璃粉;
所述的真空退火温度为400~1000℃,退火时间为1~48h。
本发明的优点是:
1、片状结构可有效降低涡流损耗,提高磁导率;
2、无需在磁环压制成型之前加入绝缘介质,避免了压制过程中绝缘介质分布不均;
3、通过真空退火在磁体内部界面处渗透扩散得到的绝缘层非常薄,避免了传统工艺中绝缘层导致磁体磁导率大幅降低的问题。
具体实施方式
下面结合实施例对本发明进行详细描述,以便更好地理解本发明的目的、特点和优点。虽然本发明是结合该具体的实施例进行描述,但并不意味着本发明局限于所描述的具体实施例。相反,对可以包括在本发明权利要求中所限定的保护范围内的实施方式进行的替代、改进和等同的实施方式,都属于本发明的保护范围。对于未特别标注的工艺参数,可按常规技术进行。
实施例1:
1)原材料准备
通过湿法球磨工艺获得片状Fe粉;
2)软磁合金粉末的钝化
将钝化剂和片状Fe粉混合,经搅拌、烘干,得到钝化粉;
3)磁场取向成型
在磁环成型过程中,利用磁场对片状Fe粉取向,获得高度有序取向的各向异性磁环;磁场强度为0.1T;
磁场取向方式为:成型过程中施加磁场,磁场方向平行于磁环平面,同时沿磁环平面方向旋转样品或旋转磁场,实现片状合金颗粒的完全有序取向;
4)表面包覆、界面扩散
采用Sb2O3将磁环表面包覆,在600℃真空退火24h,使Sb2O3经颗粒界面扩散至磁环内部,提高磁体电阻率,炉冷至室温,获得软磁复合材料。
实施例2:
1)原材料准备
通过湿法球磨工艺获得片状Fe-Si粉末;
2)软磁合金粉末的钝化
将钝化剂和片状Fe-Si粉混合,经搅拌、烘干,得到钝化粉;
3)磁场取向成型
在磁环成型过程中,利用磁场对片状Fe-Si粉取向,获得高度有序取向的各向异性磁环;磁场强度为0.5T;
磁场取向方式为:成型过程中,采用径向4磁极对样品进行对向交替充磁取向,实现片状合金颗粒的完全有序取向;
4)表面包覆、界面扩散
采用Bi2O3将磁环表面包覆,在700℃真空退火12h,使Bi2O3经颗粒界面扩散至磁环内部,提高磁体电阻率,炉冷至室温,获得软磁复合材料。
实施例3:
1)原材料准备
通过湿法球磨工艺获得片状Fe-Ni粉末;
2)软磁合金粉末的钝化
将钝化剂和片状Fe-Ni粉混合,经搅拌、烘干,得到钝化粉;
3)磁场取向成型
在磁环成型过程中,利用磁场对片状Fe-Ni粉取向,获得高度有序取向的各向异性磁环;磁场强度为1T;
磁场取向方式为:成型过程中施加磁场,磁场方向平行于磁环平面,同时沿磁环平面方向旋转样品或旋转磁场,实现片状合金颗粒的完全有序取向;
4)表面包覆、界面扩散
采用Na2CO3将磁环表面包覆,在800℃真空退火8h,使Na2CO3经颗粒界面扩散至磁环内部,提高磁体电阻率,炉冷至室温,获得软磁复合材料。
实施例4:
1)原材料准备
通过湿法球磨工艺获得片状Fe-Ni-Mo粉末;
2)软磁合金粉末的钝化
将钝化剂和片状Fe-Ni-Mo粉混合,经搅拌、烘干,得到钝化粉;
3)磁场取向成型
在磁环成型过程中,利用磁场对片状Fe-Ni-Mo粉取向,获得高度有序取向的各向异性磁环;磁场强度为2T;
磁场取向方式为:成型过程中,采用径向4磁极对样品进行对向交替充磁取向,实现片状合金颗粒的完全有序取向;
4)表面包覆、界面扩散
采用CuO将磁环表面包覆,在1000℃真空退火1h,使CuO经颗粒界面扩散至磁环内部,提高磁体电阻率,炉冷至室温,获得软磁复合材料。
实施例5:
1)原材料准备
通过湿法球磨工艺获得片状Fe-Si-Al粉末;
2)软磁合金粉末的钝化
将钝化剂和片状Fe-Si-Al粉混合,经搅拌、烘干,得到钝化粉;
3)磁场取向成型
在磁环成型过程中,利用磁场对片状Fe-Si-Al粉取向,获得高度有序取向的各向异性磁环;磁场强度为10T;
磁场取向方式为:成型过程中施加磁场,磁场方向平行于磁环平面,同时沿磁环平面方向旋转样品或旋转磁场,实现片状合金颗粒的完全有序取向;
4)表面包覆、界面扩散
采用Mn2O3将磁环表面包覆,在900℃真空退火6h,使Mn2O3经颗粒界面扩散至磁环内部,提高磁体电阻率,炉冷至室温,获得软磁复合材料。
实施例6:
1)原材料准备
通过湿法球磨工艺获得片状非晶粉末;
2)软磁合金粉末的钝化
将钝化剂和片状非晶粉混合,经搅拌、烘干,得到钝化粉;
3)磁场取向成型
在磁环成型过程中,利用磁场对片状非晶粉取向,获得高度有序取向的各向异性磁环;磁场强度为5T;
磁场取向方式为:成型过程中,采用径向4磁极对样品进行对向交替充磁取向,实现片状合金颗粒的完全有序取向;
4)表面包覆、界面扩散
采用B2O3将磁环表面包覆,在400℃真空退火48h,使B2O3经颗粒界面扩散至磁环内部,提高磁体电阻率,炉冷至室温,获得软磁复合材料。
实施例7:
1)原材料准备
通过湿法球磨工艺获得片状纳米晶粉末;
2)软磁合金粉末的钝化
将钝化剂和片状纳米晶粉混合,经搅拌、烘干,得到钝化粉;
3)磁场取向成型
在磁环成型过程中,利用磁场对片状纳米晶粉取向,获得高度有序取向的各向异性磁环;磁场强度为0.5T;
磁场取向方式为:成型过程中施加磁场,磁场方向平行于磁环平面,同时沿磁环平面方向旋转样品或旋转磁场,实现片状合金颗粒的完全有序取向;
4)表面包覆、界面扩散
采用V2O5将磁环表面包覆,在500℃真空退火36h,使V2O5经颗粒界面扩散至磁环内部,提高磁体电阻率,炉冷至室温,获得软磁复合材料。
实施例8:
1)原材料准备
通过湿法球磨工艺获得片状Fe粉末;
2)软磁合金粉末的钝化
将钝化剂和片状Fe粉混合,经搅拌、烘干,得到钝化粉;
3)磁场取向成型
在磁环成型过程中,利用磁场对片状Fe粉取向,获得高度有序取向的各向异性磁环;磁场强度为1T;
4)表面包覆、界面扩散
采用低熔点玻璃粉将磁环表面包覆,在650℃真空退火16h,使低熔点玻璃粉经颗粒界面扩散至磁环内部,提高磁体电阻率,炉冷至室温,获得软磁复合材料。
Claims (1)
1.一种软磁复合材料的制备方法,其特征在于具体步骤为:
1)原材料准备
所采用的片状软磁合金粉末为:Fe、Fe-Si、Fe-Ni、Fe-Ni-Mo、Fe-Si-Al;
所述的片状软磁合金粉末优选采用球磨法制备;
2)软磁合金粉末的钝化
将钝化剂和软磁合金粉末混合,经搅拌、烘干,得到钝化粉;
3)磁场取向成型
在磁环成型过程中,利用磁场对片状软磁合金粉末取向,获得高度有序取向的各向异性磁环;
所述磁场强度为0.1~10T;
磁场取向方式优选为:成型过程中施加磁场,磁场方向平行于磁环平面,同时沿磁环平面方向旋转样品或旋转磁场,实现片状合金颗粒的完全有序取向;
磁场取向方式优选为:成型过程中,采用径向4磁极对样品进行对向交替充磁取向,实现片状合金颗粒的完全有序取向;
4)表面包覆、界面扩散
采用低熔点化合物将磁环表面包覆,再采用真空退火工艺,使低熔点化合物经颗粒界面扩散至磁环内部,提高磁体电阻率,炉冷至室温,获得软磁复合材料;
所述的低熔点化合物包括:B2O3、V2O5、Bi2O3、Na2CO3、Mn2O3、Sb2O3、CuO和低熔点玻璃粉;
所述的真空退火温度为400~1000℃,退火时间为1~48h。
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