CN109553408A - 一种稀土掺杂锰锌铁氧体材料的制备方法 - Google Patents
一种稀土掺杂锰锌铁氧体材料的制备方法 Download PDFInfo
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Abstract
本发明涉及磁性材料技术领域,本发明公开了一种稀土掺杂锰锌铁氧体材料的制备方法,包括如下步骤:将主成分氧化锰、氧化锌、氧化铁加入球磨机球磨,得到混合料A;将混合料A进行预烧,然后冷却至室温,得到预烧料;将预烧料、氧化钒、五氧化二铌、氧化铋、氧化钼、五氧化二磷、氧化铜、复合稀土添加剂加入球磨机二次球磨,烘干,得到混合料B;所述复合稀土添加剂是由三氧化二铈、氧化钇、氧化镧组成;向混合料B中加入聚乙烯醇溶液混合造粒,然后过40‑80目筛,得到颗粒料;将颗粒料加入成型机中压制,得到坯件;烧结坯件,冷却后即可。本发明制备的稀土掺杂锰锌铁氧体材料具有较高的初始磁导率和饱和磁通密度。
Description
技术领域
本发明涉及磁性材料技术领域,尤其涉及一种稀土掺杂锰锌铁氧体材料的制备方法。
背景技术
软磁材料在工业中的应用始于十九世纪末,是伴随着电力电工及电讯技术的兴起而出现的,其应用范围极其广泛。软磁材料不仅应用于家电领域、信息化领域、汽车领域和其他配套领域,更主要的是软磁材料作为电子元器件生产的主要原材料为其带来了源源不断的需求。而随着电子行业的发展与应用领域的扩展,对磁性材料的要求也越来越高。现有技术中的软磁铁氧体的磁导率无法满足现有技术的需求,因此亟需设计一种高磁导率软磁铁氧体材料来解决现有技术中的问题。
发明内容
基于背景技术存在的问题,本发明提出了一种稀土掺杂锰锌铁氧体材料的制备方法,本发明制备的稀土掺杂锰锌铁氧体材料具有较高的初始磁导率和饱和磁通密度。
本发明提出了一种稀土掺杂锰锌铁氧体材料的制备方法,包括如下步骤:
S1、将主成分氧化锰、氧化锌、氧化铁加入球磨机球磨,得到混合料A;其中氧化锰、氧化锌、氧化铁的摩尔比为35-37:53-55:9-11;
S2、将混合料A进行预烧,然后冷却至室温,得到预烧料;
S3、将预烧料、氧化钒、五氧化二铌、氧化铋、氧化钼、五氧化二磷、氧化铜、复合稀土添加剂加入球磨机二次球磨,烘干,得到混合料B;所述复合稀土添加剂是由三氧化二铈、氧化钇、氧化镧组成;
S4、向混合料B中加入聚乙烯醇溶液混合造粒,然后过40-80目筛,得到颗粒料;混合料B与聚乙烯醇溶液的质量比为80-90:10-12;
S5、将颗粒料加入成型机中压制,得到坯件;
S6、将坯件在1350-1380℃的温度下烧结,冷却后即可。
优选地,S1中,球磨机转速为150-200r/min,球磨时间为4-6h。
优选地,S2中,预烧温度为860-880℃,预烧时间为60-90min。
优选地,S3中,预烧料、氧化钒、五氧化二铌、氧化铋、氧化钼、五氧化二磷、氧化铜、复合稀土添加剂的质量比为9800-10000:2-3:1-2:1-2:1.5-3:1.5-2.5:0.5-1.5:6-10。
优选地,S3中,所述复合稀土添加剂是由三氧化二铈、氧化钇、氧化镧按质量比3-4:4-5:6-8组成。
优选地,S3中,球磨机转速为150-200r/min,球磨时间为2-3h。
优选地,S4中,使用的是质量分数为8-10%的聚乙烯醇溶液。
优选地,S6中,保温时间4-5h。
本发明中,氧化钒的加入有助于在烧结过程中形成液相,增大液固反应面积,使反应速率加快,并使锰锌铁氧体晶粒均匀长大,从而增加锰锌铁氧体的磁导率和饱和磁感应强度;五氧化二铌的加入可以细化晶粒,使锰锌铁氧体晶粒均匀致密,还可以防止锌的挥发,进而提高锰锌铁氧体起始磁导率并降低损耗;加入适量的氧化铋有利于锰锌铁氧体晶粒的均匀长大,降低气孔率,增大密度,最终提高锰锌铁氧体起始磁导率;添加适量的氧化钼可以细化锰锌铁氧体晶粒,起到提高锰锌铁氧体的烧结密度和起始磁导率的作用;加入五氧化二磷可以增加晶界附近金属离子的空位,加速晶界的移动,并增大锰锌铁氧体晶粒尺寸和密度,进而起到增强锰锌铁氧体起始磁导率的作用;氧化铜可以降低烧结温度、增大晶格常数、促进晶粒长大,适量加入氧化铜可以降低锰锌铁氧体的气孔率并提高其电阻率和起始磁导率;随着氧化镧的加入,Ln3+少量取代Fe3+后,更有利于金属离子之间的超交换作用,从而提高铁氧体的起始磁导率以及饱和磁导率;加入三氧化二铈可以提高样品的烧结密度,减小气孔数量,进而提高铁氧体的起始磁导率以及饱和磁导率;加入适量的氧化钇可以减少样品的气孔数量,促进烧结过程中的固相反应,起到提高铁氧体的起始磁导率以及饱和磁导率的作用。在优选方案中本发明之所以将预烧温度限定在860-880℃,是因为合理的预烧温度,可以优化颗粒料的物理和化学性能、获得更好的成形密度和烧结密度、降低气孔率、均匀细化晶粒,从而降低损耗提高锰锌铁氧体材料的磁导率。
本发明通过添加适量的复合添加剂的方式来显著的改变锰锌铁氧体材料晶粒的晶界组成、离子价态以及微观结构,再结合合理的制备工艺,进而使制得的锰锌铁氧体材料的初始磁导率和饱和磁通密度等。
具体实施方式
下面结合具体实施例对本发明技术方案进行详细说明。
实施例1
一种稀土掺杂锰锌铁氧体材料的制备方法,包括如下步骤:
S1、将主成分氧化锰、氧化锌、氧化铁加入球磨机球磨,得到混合料A;其中氧化锰、氧化锌、氧化铁的摩尔比为35:55:9;
S2、将混合料A进行预烧,然后冷却至室温,得到预烧料;
S3、将预烧料、氧化钒、五氧化二铌、氧化铋、氧化钼、五氧化二磷、氧化铜、复合稀土添加剂加入球磨机二次球磨,烘干,得到混合料B;所述复合稀土添加剂是由三氧化二铈、氧化钇、氧化镧组成;
S4、向混合料B中加入聚乙烯醇溶液混合造粒,然后过40目筛,得到颗粒料;混合料B与聚乙烯醇溶液的质量比为90:10;
S5、将颗粒料加入成型机中压制,得到坯件;
S6、将坯件在1350℃的温度下烧结,冷却后即可。
实施例2
一种稀土掺杂锰锌铁氧体材料的制备方法,包括如下步骤:
S1、将主成分氧化锰、氧化锌、氧化铁加入球磨机球磨,得到混合料A;其中氧化锰、氧化锌、氧化铁的摩尔比为37:53:11;
S2、将混合料A进行预烧,然后冷却至室温,得到预烧料;
S3、将预烧料、氧化钒、五氧化二铌、氧化铋、氧化钼、五氧化二磷、氧化铜、复合稀土添加剂加入球磨机二次球磨,烘干,得到混合料B;所述复合稀土添加剂是由三氧化二铈、氧化钇、氧化镧组成;
S4、向混合料B中加入聚乙烯醇溶液混合造粒,然后过80目筛,得到颗粒料;混合料B与聚乙烯醇溶液的质量比为80:12;
S5、将颗粒料加入成型机中压制,得到坯件;
S6、将坯件在1380℃的温度下烧结,冷却后即可。
实施例3
一种稀土掺杂锰锌铁氧体材料的制备方法,包括如下步骤:
S1、将主成分氧化锰、氧化锌、氧化铁加入球磨机球磨,得到混合料A;其中氧化锰、氧化锌、氧化铁的摩尔比为35:55:9;球磨机转速为150r/min,球磨时间为6h;
S2、将混合料A进行预烧,然后冷却至室温,得到预烧料;预烧温度为860℃,预烧时间为90min;
S3、将预烧料、氧化钒、五氧化二铌、氧化铋、氧化钼、五氧化二磷、氧化铜、复合稀土添加剂加入球磨机二次球磨,烘干,得到混合料B;预烧料、氧化钒、五氧化二铌、氧化铋、氧化钼、五氧化二磷、氧化铜、复合稀土添加剂的质量比为9800:3:1:2:1.5:2.5:0.5:10;所述复合稀土添加剂是由三氧化二铈、氧化钇、氧化镧按质量比3:5:6组成;球磨机转速为150r/min,球磨时间为3h;
S4、向混合料B中加入质量分数为8%的聚乙烯醇溶液混合造粒,然后过40目筛,得到颗粒料;混合料B与聚乙烯醇溶液的质量比为90:10;
S5、将颗粒料加入成型机中压制,得到坯件;
S6、将坯件在1350℃的温度下烧结,保温时间4h,冷却后即可。
实施例4
一种稀土掺杂锰锌铁氧体材料的制备方法,包括如下步骤:
S1、将主成分氧化锰、氧化锌、氧化铁加入球磨机球磨,得到混合料A;其中氧化锰、氧化锌、氧化铁的摩尔比为37:53:11;球磨机转速为200r/min,球磨时间为4h;
S2、将混合料A进行预烧,然后冷却至室温,得到预烧料;预烧温度为880℃,预烧时间为60min;
S3、将预烧料、氧化钒、五氧化二铌、氧化铋、氧化钼、五氧化二磷、氧化铜、复合稀土添加剂加入球磨机二次球磨,烘干,得到混合料B;预烧料、氧化钒、五氧化二铌、氧化铋、氧化钼、五氧化二磷、氧化铜、复合稀土添加剂的质量比为10000:2:2:1:3:1.5:1.5:6;所述复合稀土添加剂是由三氧化二铈、氧化钇、氧化镧按质量比4:4:8组成;球磨机转速为200r/min,球磨时间为2h;
S4、向混合料B中加入质量分数为10%的聚乙烯醇溶液混合造粒,然后过80目筛,得到颗粒料;混合料B与聚乙烯醇溶液的质量比为80:12;
S5、将颗粒料加入成型机中压制,得到坯件;
S6、将坯件在1380℃的温度下烧结,保温时间5h,冷却后即可。
实验例
检测实施例1-4制备的稀土掺杂锰锌铁氧体材料的初始磁导率和饱和磁通密度,实验结果如表1所示:
表1
由表1可知,本发明制备的稀土掺杂锰锌铁氧体材料具有较高的初始磁导率和饱和磁通密度。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (8)
1.一种稀土掺杂锰锌铁氧体材料的制备方法,其特征在于,包括如下步骤:
S1、将主成分氧化锰、氧化锌、氧化铁加入球磨机球磨,得到混合料A;其中氧化锰、氧化锌、氧化铁的摩尔比为35-37:53-55:9-11;
S2、将混合料A进行预烧,然后冷却至室温,得到预烧料;
S3、将预烧料、氧化钒、五氧化二铌、氧化铋、氧化钼、五氧化二磷、氧化铜、复合稀土添加剂加入球磨机二次球磨,烘干,得到混合料B;所述复合稀土添加剂是由三氧化二铈、氧化钇、氧化镧组成;
S4、向混合料B中加入聚乙烯醇溶液混合造粒,然后过40-80目筛,得到颗粒料;混合料B与聚乙烯醇溶液的质量比为80-90:10-12;
S5、将颗粒料加入成型机中压制,得到坯件;
S6、将坯件在1350-1380℃的温度下烧结,冷却后即可。
2.根据权利要求1所述的制备方法,其特征在于,S1中,球磨机转速为150-200r/min,球磨时间为4-6h。
3.根据权利要求1或2所述的制备方法,其特征在于,S2中,预烧温度为860-880℃,预烧时间为60-90min。
4.根据权利要求1-3任一项所述的制备方法,其特征在于,S3中,预烧料、氧化钒、五氧化二铌、氧化铋、氧化钼、五氧化二磷、氧化铜、复合稀土添加剂的质量比为9800-10000:2-3:1-2:1-2:1.5-3:1.5-2.5:0.5-1.5:6-10。
5.根据权利要求1-4任一项所述的制备方法,其特征在于,S3中,所述复合稀土添加剂是由三氧化二铈、氧化钇、氧化镧按质量比3-4:4-5:6-8组成。
6.根据权利要求1-5任一项所述的制备方法,其特征在于,S3中,球磨机转速为150-200r/min,球磨时间为2-3h。
7.根据权利要求1-6任一项所述的制备方法,其特征在于,S4中,使用的是质量分数为8-10%的聚乙烯醇溶液。
8.根据权利要求1-7任一项所述的制备方法,其特征在于,S6中,保温时间4-5h。
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