CN112614689A - 一种提高粘结永磁铁氧体磁粉各向异性的方法 - Google Patents

一种提高粘结永磁铁氧体磁粉各向异性的方法 Download PDF

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CN112614689A
CN112614689A CN202011558311.1A CN202011558311A CN112614689A CN 112614689 A CN112614689 A CN 112614689A CN 202011558311 A CN202011558311 A CN 202011558311A CN 112614689 A CN112614689 A CN 112614689A
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李昕
裴晓东
骆艳华
汪祥
鲍维东
张倩倩
张金艳
鲍思凯
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Sinosteel Nanjing New Material Research Institute Co Ltd
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    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
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    • H01F41/02Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
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Abstract

本发明公布了一种提高粘结永磁铁氧体磁粉各向异性的方法,步骤为:将粘结磁粉添加助熔剂后加入球磨罐中,加水球磨,出料后滤干,将含水磁粉加入压机中,人工施加磁场将磁粉充磁取向后,再加压压制成圆形毛坯。将毛坯放入马弗炉中二次烧结,待炉内冷却后,取出磁块,加润滑剂放入振动粉碎机中粗破碎后,在加入到球磨罐中破碎,磁粉出罐后,用清水洗涤三次。烘干后过筛分散,放入马弗炉中回火,得各向异性粘结永磁铁氧体磁粉。本发明的方法施加外磁场充磁取向后,再进行二次烧结,促进磁粉晶粒沿磁场取向方向二次生长,提高磁粉各向异性,从而提升磁粉磁性能。

Description

一种提高粘结永磁铁氧体磁粉各向异性的方法
技术领域
本发明涉及磁性材料生产方法,具体涉及一种提高粘结永磁铁氧体磁粉各向异性的方法。
背景技术
注塑铁氧体是指用铁氧体磁粉和树脂混合后,通过注射成型工艺成型的磁体。特点是既可以轴向单极充磁,也可径向多级充磁,还可以轴向径向复合充磁。产品外观光洁无瑕疵,尺寸精度高,一致性好,无需后续加工,性能稳定,抗震耐冲击,产品可复杂化,是精密微电机及自动化行业不可缺少的信号源和恒磁源,具有其他磁体无法替代和比拟的优越性。
粘结永磁铁氧体磁粉为注塑铁氧体的主要原料之一,目前已经有了成熟的制备方法,在很多专利中都有论述(CN101894648A,粘结铁氧体磁粉及其制备方法及粘结磁体;CN107399964,一种粘结铁氧体磁粉的制备方法)。但传统工艺方法中制备的永磁铁氧体磁粉均为各向同性磁粉,其磁粉磁性能提升有限。而各向异性磁粉的磁性能优于各向同性磁粉,通过提高磁粉的各向异性可以显著提高磁粉的磁性能,尤其是磁粉的剩磁可以得到大幅度提高。
发明内容
为了解决上述不足,本发明提供了一种提高粘结永磁铁氧体磁粉各向异性的方法,所述的制备方法包括以下步骤:1)将粘结磁粉添加助熔剂后加入球磨罐中,加水球磨,出料后滤干,将含水磁粉加入压机中,先充磁取向后,加压压制成圆形毛坯;
2)将毛坯放入马弗炉中二次烧结,待炉内冷却后,取出磁块,加润滑剂放入振动粉碎机中粗破碎后,再加入到球磨罐中破碎,磁粉出罐后,用清水洗涤三次;
3)烘干后过筛分散,再放入马弗炉中回火,得各向异性粘结永磁铁氧体磁粉。
进一步地,添加的助熔剂为氯化钠、氧化铋和硼酸中的一种或混合物,助熔剂的添加量为0.1-1%。
进一步地,磁粉添加助熔剂后再球磨,磁粉的球磨时间为10-13h,磁粉的粒径控制在0.8-2 μm。
进一步地,球磨后的磁粉滤干后,加入压机中,先充磁取向后,再加压压制成圆形毛坯,压机的充磁磁场强度为8000-10000Oe。
进一步地,压制成的毛坯进行二次烧结,二次烧结的温度为1180-1220℃,保温时间为 1-3h。
进一步地,毛坯烧结结束后,加润滑剂放入振动粉碎机中粗破碎后,再加入到球磨罐中细磨,振动粉碎时间为4-8min,球磨破碎时间为2-4h。
进一步地,球磨结束后,将磁粉过筛分散,放入马弗炉中回火,回火温度为900-930℃,回火时间为1h。
与现有技术相比,本发明的优点为:相比于其他制备粘结铁氧体磁粉的方法,本发明的粘结磁粉经过施加外磁场充磁取向后,再进行二次烧结,促进磁粉晶粒沿磁场取向方向二次生长,提高磁粉各向异性,从而提升磁粉磁性能;同时本方法简单易行,过程方便控制,可以大幅度提升粘结永磁铁氧体磁粉的磁性能。
附图说明
图1为实施例和对比例的XRD对比示意图;
图中四条线,从上到下依次是;实施例1,实施例2,对比例1,对比例2。
具体实施方式
为了使审查员能够进一步了解本发明的步骤、特征以及其它目的,现结合所附较佳实施例详细说明如下,本实施仅用于说明本发明的技术方案,并非限定发明。
本发明提供了一种提高粘结永磁铁氧体磁粉各向异性的方法,所述的制备方法包括以下步骤:1)将粘结磁粉添加助熔剂后加入球磨罐中,加水球磨,出料后滤干,将含水磁粉加入压机中,先充磁取向后,加压压制成圆形毛坯;
2)将毛坯放入马弗炉中二次烧结,待炉内冷却后,取出磁块,加润滑剂放入振动粉碎机中粗破碎后,再加入到球磨罐中破碎,磁粉出罐后,用清水洗涤三次;
3)烘干后过筛分散,再放入马弗炉中回火,得各向异性粘结永磁铁氧体磁粉。
上述添加的助熔剂为氯化钠、氧化铋和硼酸中的一种或混合物,助熔剂的添加量为 0.1-1%。
上述磁粉添加助熔剂后再球磨,磁粉的球磨时间为10-13h,磁粉的粒径控制在0.8-2μm。
上述球磨后的磁粉滤干后,加入压机中,先充磁取向后,再加压压制成圆形毛坯,压机的充磁磁场强度为8000-10000Oe。
上述压制成的毛坯进行二次烧结,二次烧结的温度为1180-1220℃,保温时间为1-3h。
上述毛坯烧结结束后,加润滑剂放入振动粉碎机中粗破碎后,再加入到球磨罐中细磨,振动粉碎时间为4-8min,球磨破碎时间为2-4h。
上述球磨结束后,将磁粉过筛分散,放入马弗炉中回火,回火温度为900-930℃,回火时间为1h。
实施例1
将1503.2g铁红、216.2g碳酸锶和3.6g碳酸钡放入砂磨机中,加水均匀混磨2h,出料后烘干,造球预烧。升温至1320℃,烧结2h制备成锶铁氧体预烧料。
往预烧料中添加0.5%氧化铋和0.3%氯化钠后,加入球磨罐中,加水球磨13h,出料后滤干,将含水磁粉加入压机中,在10000Oe磁场下充磁取向后,加压压制成圆形毛坯。将毛坯放入马弗炉中,1200℃下二次烧结,待炉内冷却后,取出磁块,加0.33%葡萄糖酸钙,放入振动粉碎机中粗破碎6min后,再加入到球磨罐中细磨3h,待磁粉出罐后,用清水洗涤三次。烘干后过筛分散,放入马弗炉中920℃回火1h,得各向异性粘结永磁铁氧体磁粉。
实施例2
将1336.5g铁红、216.2g碳酸锶和3.6g碳酸钡放入砂磨机中,加水均匀混磨2h,出料后烘干,造球预烧。升温至1320℃,烧结2h制备成锶铁氧体预烧料。
往预烧料中添加0.55%氧化铋和0.35%氯化钠后,加入球磨罐中,加水球磨13h,出料后滤干,将含水磁粉加入压机中,在8500Oe磁场下充磁取向后,加压压制成圆形毛坯。将毛坯放入马弗炉中,1200℃下二次烧结,待炉内冷却后,取出磁块,加0.33%葡萄糖酸钙,放入振动粉碎机中粗破碎4min后,再加入到球磨罐中细磨13h,待磁粉出罐后,用清水洗涤三次。烘干后过筛分散,放入马弗炉中930℃回火1h,得各向异性粘结永磁铁氧体磁粉。
对比例1
将1503.2g铁红、216.2g碳酸锶和3.6g碳酸钡放入砂磨机中,加水均匀混磨2h,出料后烘干,造球预烧。升温至1320℃,烧结2h制备成锶铁氧体预烧料。将冷却后的预烧料,加0.33%葡萄糖酸钙,放入振动粉碎机中粗破碎6min后,再加入到球磨罐中细磨3h,待磁粉出罐后,用清水洗涤三次。烘干后过筛分散,放入马弗炉中920℃回火1h,得粘结永磁铁氧体磁粉。
对比例2
将1336.5g铁红、216.2g碳酸锶和3.6g碳酸钡放入砂磨机中,加水均匀混磨2h,出料后烘干,造球预烧。升温至1320℃,烧结2h制备成锶铁氧体预烧料。将冷却后的预烧料,加0.33%葡萄糖酸钙,放入振动粉碎机中粗破碎4min后,再加入到球磨罐中细磨3h,待磁粉出罐后,用清水洗涤三次。烘干后过筛分散,放入马弗炉中930℃回火,得粘结永磁铁氧体磁粉。
将制备的永磁铁氧体磁粉检测XRD图,结果见附图1。经分析,充磁取向复烧后的磁粉,出现了明显的(008)面峰位,表明磁粉晶粒在易磁化的C轴出现异常生长,这有利于磁粉的磁性能提升。
检测磁粉的压坯磁性能,具体方法为:称取石蜡1.4g,磁粉20g。将石蜡熔化后,加入磁粉搅拌均匀后,称取混合样7g,用压片机在7Mpa压力下,保压10s压制成直径20mm 的圆形坯体,用B-H仪检测坯体磁性能。
表1是各实施例与对比例压坯磁性能一览表。从中可见经过充磁取向的粘结永磁铁氧体磁粉,其压坯磁性能,尤其是剩磁有了显著的提高。
表1.实施例与对比例压坯磁性能一览表
Figure BDA0002859458590000041
需要声明,上述具体实施方式意在证明本发明所提供制备方法的实际应用,不限定为对本发明的保护范围。本领域的技术人员在本发明的精神和原理内,可以进行各种修改、替换或改进。本发明的保护范围以所附的权利要求书为准。

Claims (8)

1.一种提高粘结永磁铁氧体磁粉各向异性的方法,其特征在于,步骤为:
1)将粘结磁粉添加助熔剂后加入球磨罐中,加水球磨,出料后滤干,将含水磁粉加入压机中,先充磁取向后,加压压制成圆形毛坯;
2)将毛坯放入马弗炉中二次烧结,待炉内冷却后,取出磁块,加润滑剂放入振动粉碎机中粗破碎后,再加入到球磨罐中破碎,磁粉出罐后,用清水洗涤三次;
3)烘干后过筛分散,再放入马弗炉中回火,得各向异性粘结永磁铁氧体磁粉。
2.根据权利要求1所述的一种提高粘结永磁铁氧体磁粉各向异性的方法,其特征在于,添加的助熔剂为氯化钠、氧化铋和硼酸中的一种或混合物,助熔剂的添加量为0.1-1%。
3.根据权利要求1所述的一种提高粘结永磁铁氧体磁粉各向异性的方法,其特征在于,磁粉添加助熔剂后再球磨,磁粉的球磨时间为10-13h,磁粉的粒径控制在0.8-2μm。
4.根据权利要求1所述的一种提高粘结永磁铁氧体磁粉各向异性的方法,其特征在于,球磨后的磁粉滤干后,加入压机中,先充磁取向后,再加压压制成圆形毛坯,压机的充磁磁场强度为8000-10000Oe。
5.根据权利要求1所述的一种提高粘结永磁铁氧体磁粉各向异性的方法,其特征在于,压制成的毛坯进行二次烧结,二次烧结的温度为1180-1220℃,保温时间为1-3h。
6.根据权利要求1所述的一种提高粘结永磁铁氧体磁粉各向异性的方法,其特征在于,所述的润滑剂为葡萄糖酸钙。
7.根据权利要求1所述的一种提高粘结永磁铁氧体磁粉各向异性的方法,其特征在于,毛坯烧结结束后,加润滑剂放入振动粉碎机中粗破碎后,再加入到球磨罐中细磨,振动粉碎时间为4-8min,球磨破碎时间为2-4h。
8.根据权利要求1所述的提高粘结永磁铁氧体磁粉各向异性的方法,其特征在于,球磨结束后,将磁粉过筛分散,放入马弗炉中回火,回火温度为900-930℃,回火时间为1h。
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