CN107481828A - 一种高矫顽力高磁能积铁氧体材料的生产方法 - Google Patents
一种高矫顽力高磁能积铁氧体材料的生产方法 Download PDFInfo
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Abstract
本发明公开了一种高矫顽力高磁能积铁氧体材料的生产方法,首先准备原料,选用粒度为0.7‑0.9m、粒度分布标准偏差δ=0.14‑0.16μm的铁红为原料,取得该铁红后经球磨研磨至0.4‑0.75μm粒径;然后混料,加入作为结晶粒度控制剂的0.1‑0.5%的SiO2、0.05‑0.2%的H3BO3,在1250‑1300℃温度下预烧;接着压制成型,在预烧后的磁粉中加入分散剂混炼,该分散剂采用1.3wt%的油酸二甲苯溶液作介质,桨料的平均粒径不大于0.65μm,将混炼后的浆料打入压机模穴压制成型;再将成型胚体送入烧结炉中,在1000℃以上温度烧结;最后将所得磁体充磁,检验成品。这种高矫顽力高磁能积铁氧体材料的生产方法可以利用中低档质量的预烧料制造高性能永磁铁氧体磁瓦和辐射取向磁环以及径向取向的极异方磁环,有效降低生产成本,有利于大规模推广。
Description
技术领域
本发明涉及一种铁氧体材料的生产方法。
背景技术
从1930年初永久磁石即为民生、国防工业上一项不可欠缺的材料。时至今日,信息及消费性电子产品的普及化,永久磁石的高性能化扮演着不可磨灭的角色。磁性材料是电子行业非常重要的材料,在家电、汽车、计算器、通讯、医疗、航天、军事等领域的应用十分广泛。经过年初永久磁石即为民生、国防工业上一项不可欠缺的材料。时至今日,信息及消费性电子产品的普及化,永久磁石的高性能化扮演着不可磨灭的角色。磁性材料是电子行业非常重要的材料,在家电、汽车、计算器、通讯、医疗、航天、军事等领域的应用十分广泛。经过20多年的建设和发展,我国已经形成了品种齐全的磁性材料体系,各主要门类磁性材料的产量均居世界第一位。目前我国磁性材料行业已经形成了一定数量的大规模骨干企业,产质量量和技术档次都有了较大幅度的提升,产品应用范围正逐步向高档领域扩展。中国的磁性材料工业凭借丰富的资源和劳动力的优势,以及巨大的国内外市场支持,将有一个稳定的发展时期。
随着汽车、电动单车、办公自动化设备、通讯、计算器、网络等家用电器与电子讯息产业的高速发展,日本著名的磁性材料企业走科技创新之路,立足于开发技术导向性磁性产品,与时俱进,瞄准市场,不断推展永磁铁氧体的高性能化,其主要技术手段就是采用La、Co组合搀杂来实现各种离子代换,形成了目前世界上性能较高的永磁铁氧体,最大磁能积已接近理论值,可满足摄像机、数码相机以及各类电机进一步小型化、高效化的需求。然而,这种铁氧体材料的生产方法需要采用高质量的预烧料,生产成本较高,难以大规模推广。
发明内容
本发明要解决的技术问题是提供一种高矫顽力高磁能积铁氧体材料的生产方法,以降低生产成本,可以大规模推广。
为了解决上述技术问题,本发明的一种高矫顽力高磁能积铁氧体材料的生产方法,包括以下步骤:
A)准备原料,选用粒度为0.7-0.9m、粒度分布标准偏差δ=0.14-0.16μm 的铁红为原料,取得该铁红后经球磨研磨至0.4-0.75μm粒径;
B)混料,加入作为结晶粒度控制剂的0.1-0.5%的SiO2 、0.05-0.2%的H3BO3,在1250-1300℃温度下预烧;
C)压制成型,在预烧后的磁粉中加入分散剂混炼,使分散剂与磁粉充分接触,减小磁粉的凝聚,从而提升配向度,该分散剂采用1.3wt%的油酸二甲苯溶液作介质,桨料的平均粒径不大于0.65μm,将混炼后的浆料打入压机模穴压制成型;
D)将成型胚体送入烧结炉中,在1000℃以上温度烧结;
E)将所得磁体充磁,检验成品。
所述步骤A中,球磨研磨采用分级研磨,通过球磨机干磨加风选分级来控制进料粗粉的粒度和粒度分布标准偏差并采用底部进料的连续砂磨机对粗颗粒长时间研磨。
所述步骤A中,研磨后的磁粉在600-900℃温度下热处理并采用磁选设备筛选磁粉。
所述步骤C中,混炼后的浆料在磁场下湿压成型,成型的同时施以磁场取向,上下冲模相距25mm时,磁场强度为15000奥斯特。
所述步骤D中,需要采用烧结炉回收热风把成型胚体烘干,然后在400-500℃温度下进行脱去分散剂处理。
所述骤D中烧结炉为全自动辊道推板电气隧道窑。
本发明的有益效果是:这种高矫顽力高磁能积铁氧体材料的生产方法,通过控制磁粉粒度和采用分散剂与磁粉混炼,可以利用中低档质量的预烧料制造高性能永磁铁氧体磁瓦和辐射取向磁环以及径向取向的极异方磁环,有效降低了生产成本,有利于大规模推广。
具体实施方式
本发明的一种高矫顽力高磁能积铁氧体材料的生产方法,包括以下步骤:
A)准备原料,选用粒度为0.7-0.9m、粒度分布标准偏差δ=0.14-0.16μm 的铁红为原料,取得该铁红后经球磨研磨至0.4-0.75μm粒径;
B)混料,加入作为结晶粒度控制剂的0.1-0.5%的SiO2 、0.05-0.2%的H3BO3,在1250-1300℃温度下预烧,利用此预烧料可以生产Br>0.42(4200G),Hcj>278kA/m(3500Oe)的烧结永磁铁氧体。
C)压制成型,在预烧后的磁粉中加入分散剂混炼,使分散剂与磁粉充分接触,减小磁粉的凝聚,从而提升配向度,该分散剂采用1.3wt%的油酸二甲苯溶液作介质,桨料的平均粒径不大于0.65μm,将混炼后的浆料打入压机模穴压制成型;
D)将成型胚体送入烧结炉中,在1000℃以上温度烧结;
E)将所得磁体充磁,检验成品。
所述步骤A中,球磨研磨采用分级研磨,通过球磨机干磨加风选分级来控制进料粗粉的粒度和粒度分布标准偏差并采用底部进料的连续砂磨机对粗颗粒长时间研磨。此技术可以有效控制粒度分布标准偏差δ=0.14-0.16μm ,使永磁铁氧体的剩磁和矫顽力提升4%。
所述步骤A中,研磨后的磁粉在600-900℃温度下热处理并采用磁选设备筛选磁粉,热处理后的Fe及Fe2+氧化成Fe3+,便于将无磁的磁粉除掉。利用此方法可以有效控制铁氧体晶粒分布,提升单畴颗粒的存在率。
所述步骤C中,混炼后的浆料在磁场下湿压成型,成型的同时施以磁场取向,上下冲模相距25mm时,磁场强度为15000奥斯特。所述步骤D中,需要采用烧结炉回收热风把成型胚体烘干,然后在400-500℃温度下进行脱去分散剂处理。
高性能产品对烧结温度和烧结气氛都有特别的要求。在烧结过程中,特别在高温1000℃以上,窑炉中的含氧量与升温速率、高温区的温度及保温时间、降温速率对产品磁性能有着直接的影响。若烧结温度太低或保温时间过短,则固相响应不完全,晶体生长不完全,气孔多,产品的磁性能就不好。若烧结温度过高或保温时间过长,则会导致异常晶粒生长,使产品磁性能恶化。只有当烧结温度适当时,晶粒细而均匀,气孔呈球形,产品密度高,性能就高。所述骤D中烧结炉为全自动辊道推板电气隧道窑,控温精度高,而且烧结气氛易控制,满足高性能连续大生产技术条件。
以上所述仅为本发明的优先实施方式,只要以基本相同手段实现本发明目的的技术方案都属于本发明的保护范围之内。
Claims (6)
1.一种高矫顽力高磁能积铁氧体材料的生产方法,其特征在于包括以下步骤:
A)准备原料,选用粒度为0.7-0.9m、粒度分布标准偏差δ=0.14-0.16μm 的铁红为原料,取得该铁红后经球磨研磨至0.4-0.75μm粒径;
B)混料,加入作为结晶粒度控制剂的0.1-0.5%的SiO2 、0.05-0.2%的H3BO3,在1250-1300℃温度下预烧;
C)压制成型,在预烧后的磁粉中加入分散剂混炼,使分散剂与磁粉充分接触,减小磁粉的凝聚,从而提升配向度,该分散剂采用1.3wt%的油酸二甲苯溶液作介质,桨料的平均粒径不大于0.65μm,将混炼后的浆料打入压机模穴压制成型;
D)将成型胚体送入烧结炉中,在1000℃以上温度烧结;
E)将所得磁体充磁,检验成品。
2.根据权利要求1所述的高矫顽力高磁能积铁氧体材料的生产方法,其特征在于:所述步骤A中,球磨研磨采用分级研磨,通过球磨机干磨加风选分级来控制进料粗粉的粒度和粒度分布标准偏差并采用底部进料的连续砂磨机对粗颗粒长时间研磨。
3.根据权利要求2所述的高矫顽力高磁能积铁氧体材料的生产方法,其特征在于:所述步骤A中,研磨后的磁粉在600-900℃温度下热处理并采用磁选设备筛选磁粉。
4.根据权利要求1所述的高矫顽力高磁能积铁氧体材料的生产方法,其特征在于:所述步骤C中,混炼后的浆料在磁场下湿压成型,成型的同时施以磁场取向,上下冲模相距25mm时,磁场强度为15000奥斯特。
5.根据权利要求4所述的高矫顽力高磁能积铁氧体材料的生产方法,其特征在于:所述步骤D中,需要采用烧结炉回收热风把成型胚体烘干,然后在400-500℃温度下进行脱去分散剂处理。
6.根据权利要求4所述的高矫顽力高磁能积铁氧体材料的生产方法,其特征在于:所述骤D中烧结炉为全自动辊道推板电气隧道窑。
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