CN106396657A - 一种宽频低损耗软磁铁氧体材料及其制备方法 - Google Patents

一种宽频低损耗软磁铁氧体材料及其制备方法 Download PDF

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CN106396657A
CN106396657A CN201610721539.5A CN201610721539A CN106396657A CN 106396657 A CN106396657 A CN 106396657A CN 201610721539 A CN201610721539 A CN 201610721539A CN 106396657 A CN106396657 A CN 106396657A
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王久如
徐升宝
商燕彬
李丛俊
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TIANCHANG ZHONGDE ELECTRONICS CO Ltd
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Abstract

本发明公开了一种宽频低损耗软磁铁氧体材料,由主料和辅料制成,主料和辅料的摩尔比为1:(0.1‑0.3),主料包括:氧化铁、氧化锰、氧化锌、氧化硅、余量为镍粉;以主料的重量为基准,辅料包括:碳酸钙、氧化锆、氧化铌、氧化锡、氧化钴、三氧化钼和氧化钙。本发明还提出上述一种宽频低损耗软磁铁氧体材料的制备方法。本发明制备得到的软磁铁氧体材料具有宽频低损的特性。

Description

一种宽频低损耗软磁铁氧体材料及其制备方法
技术领域
本发明涉及一种软磁铁氧体材料及其制备方法,尤其涉及一种宽频低损耗软磁铁氧体材料及其制备方法。
背景技术
随着数字通信技术和光纤通信技术的快速发展,传统的模拟通信设备不断地更新淘汰。在电子电路宽带变压器,综合业务数据网、局域网、广域网、背景照明等领域的脉冲变压器和光伏逆变器中共模滤波电感用的高磁导率铁氧体磁芯,由于变压器等朝着小型化发展,因此对铁氧体的磁特性提出了更高要求,特别是在当前电子信息时代,外界环境的各种电子干扰日益严重,需要铁氧体具有高起始磁导率、高饱和磁感应强度、高居里温度、高阻抗和宽频特性。
现有技术中的软磁铁氧体的居里温度和电损无法满足现有技术的需求,因此亟需设计一种宽频低损耗软磁铁氧体材料来解决现有技术中的问题。
发明内容
为解决背景技术中存在的技术问题,本发明提出一种宽频低损耗软磁铁氧体材料及其制备方法,制备得到的软磁铁氧体材料具有宽频低损的特性。
本发明提出的一种宽频低损耗软磁铁氧体材料,由主料和辅料制成,主料和辅料的摩尔比为1:(0.1-0.3),主料按摩尔百分比包括:氧化铁50.2-52.6mol%、氧化锰28.2-32.4mol%、氧化锌18.2-22.4mol%、氧化硅4.8-6.4mol%、余量为镍粉;以主料的重量为基准,辅料按重量百分比包括:碳酸钙0.02-0.08wt%、氧化锆0.03-0.05wt%、氧化铌0.020-0.040wt%、氧化锡0.15-0.18wt%、氧化钴0.38-0.45wt%、三氧化钼0.32-0.36wt%、氧化钙0.12-0.24wt%。
优选地,主料按摩尔百分比包括:氧化铁50.3-52.5mol%、氧化锰29.2-31.4mol%、氧化锌19.2-21.4mol%、氧化硅4.9-6.3mol%、余量为镍粉。
优选地,以主料的重量为基准,辅料按重量百分比包括:碳酸钙0.03-0.07wt%、氧化锆0.035-0.045wt%、氧化铌0.025-0.035wt%、氧化锡0.16-0.17wt%、氧化钴0.39-0.44wt%、三氧化钼0.33-0.35wt%、氧化钙0.14-0.22wt%。
优选地,由主料和辅料制成,主料和辅料的摩尔比为1:(0.15-0.25),主料按摩尔百分比包括:氧化铁50.3-52.5mol%、氧化锰29.2-31.4mol%、氧化锌19.2-21.4mol%、氧化硅4.9-6.3mol%、余量为镍粉;以主料的重量为基准,辅料按重量百分比包括:碳酸钙0.03-0.07wt%、氧化锆0.035-0.045wt%、氧化铌0.020-0.040wt%、氧化锡0.15-0.18wt%、氧化钴0.38-0.45wt%、三氧化钼0.32-0.36wt%、氧化钙0.12-0.24wt%。
优选地,由主料和辅料制成,主料和辅料的摩尔比为1:0.2,主料按摩尔百分比包括:氧化铁51.4mol%、氧化锰30.3mol%、氧化锌20.3mol%、氧化硅5.6mol%、余量为镍粉;以主料的重量为基准,辅料按重量百分比包括:碳酸钙0.05wt%、氧化锆0.04wt%、氧化铌0.030wt%、氧化锡0.165wt%、氧化钴0.415wt%、三氧化钼0.34wt%、氧化钙0.36wt%。
本发明的一种宽频低损耗软磁铁氧体材料的制备方法,包括如下步骤:
S1、将主料进行湿式混合,一次球磨90-120min,然后喷雾干燥,进行预烧;
S2、向预烧主料中加入辅料、分散剂和消泡剂混合均匀,进行二次球磨1-3h,得到粒径为0.8-1.2微米的粉料;
S3、向S2得到的粉料中添加有机粘合剂混合均匀,喷雾造粒得颗粒料,将颗粒料于50-200MPa压制成生坯样品;
S4、将S3得到的生坯样品升温至1050-1150℃,保温20-60min;升温至1250-1350℃,保温10-30min,升温过程中,氧分压维持在2-4%;升温至1350-1450℃,保温1-3h,升温过程中,氧分压维持在12-18%;降温至900-1000℃,保温2-4h;降温至室温得到宽频低损耗软磁铁氧体材料。
优选地,S1中,预烧温度为800-900℃,预烧时间为2-4h。
本发明的一种宽频低损耗软磁铁氧体材料,由主料和辅料按一定比例制成,主料包括:氧化铁、氧化锰、氧化锌、氧化硅、余量为镍粉;以主料的重量为基准,辅料包括:碳酸钙、氧化锆、氧化铌、氧化锡、氧化钴、三氧化钼和氧化钙。将主料氧化铁、氧化锰、氧化锌、氧化硅和镍粉球磨后混合均匀,然后进行预烧处理,接着加入碳酸钙、氧化锆、氧化铌、氧化锡、氧化钴、三氧化钼和氧化钙进行二次球磨,混合均匀后,加入粘合剂制成粒状物料,最后进行烧结,从而制备得到宽频低损耗软磁铁氧体材料。本发明制备得到的软磁铁氧体材料具有宽频低损的特性。得到软磁铁氧体材料的初始磁导率为3200,100Kc,200mT条件下,25℃时,磁性损耗max为650KW/m3,80℃时,磁性损耗max为320KW/m3,100℃时,磁性损耗max为430KW/m3
具体实施方式
下面结合具体实施例对本发明做出详细说明,应当了解,实施例只用于说明本发明,而不是用于对本发明进行限定,任何在本发明基础上所做的修改、等同替换等均在本发明的保护范围内。
实施例1
本发明提出的一种宽频低损耗软磁铁氧体材料,由主料和辅料制成,主料和辅料的摩尔比为1:0.2,主料按摩尔百分比包括:氧化铁51.4mol%、氧化锰30.3mol%、氧化锌20.3mol%、氧化硅5.6mol%、余量为镍粉;以主料的重量为基准,辅料按重量百分比包括:碳酸钙0.05wt%、氧化锆0.04wt%、氧化铌0.030wt%、氧化锡0.165wt%、氧化钴0.415wt%、三氧化钼0.34wt%、氧化钙0.36wt%。
实施例2
本发明提出的一种宽频低损耗软磁铁氧体材料,由主料和辅料制成,主料和辅料的摩尔比为1:0.1,主料按摩尔百分比包括:氧化铁50.2mol%、氧化锰32.4mol%、氧化锌18.2mol%、氧化硅6.4mol%、余量为镍粉;以主料的重量为基准,辅料按重量百分比包括:碳酸钙0.02wt%、氧化锆0.05wt%、氧化铌0.020wt%、氧化锡0.18wt%、氧化钴0.38wt%、三氧化钼0.36wt%、氧化钙0.12wt%。
本发明的一种宽频低损耗软磁铁氧体材料的制备方法,包括如下步骤:
S1、将主料进行湿式混合,一次球磨90min,然后喷雾干燥,进行预烧,预烧温度为900℃,预烧时间为2h;
S2、向预烧主料中加入辅料、分散剂和消泡剂混合均匀,进行二次球磨3h,得到粒径为0.8微米的粉料;
S3、向S2得到的粉料中添加有机粘合剂混合均匀,喷雾造粒得颗粒料,将颗粒料于200MPa压制成生坯样品;
S4、将S3得到的生坯样品升温至1050℃,保温60min;升温至1250℃,保温30min,升温过程中,氧分压维持在2%;升温至1450℃,保温1h,升温过程中,氧分压维持在18%;降温至900℃,保温4h;降温至室温得到宽频低损耗软磁铁氧体材料。
实施例3
本发明提出的一种宽频低损耗软磁铁氧体材料,由主料和辅料制成,主料和辅料的摩尔比为1:0.3,主料按摩尔百分比包括:氧化铁52.6mol%、氧化锰28.2mol%、氧化锌22.4mol%、氧化硅4.8mol%、余量为镍粉;以主料的重量为基准,辅料按重量百分比包括:碳酸钙0.08wt%、氧化锆0.03wt%、氧化铌0.040wt%、氧化锡0.15wt%、氧化钴0.45wt%、三氧化钼0.32wt%、氧化钙0.24wt%。
本发明的一种宽频低损耗软磁铁氧体材料的制备方法,包括如下步骤:
S1、将主料进行湿式混合,一次球磨120min,然后喷雾干燥,进行预烧,预烧温度为800℃,预烧时间为4h;
S2、向预烧主料中加入辅料、分散剂和消泡剂混合均匀,进行二次球磨3h,得到粒径为0.8微米的粉料;
S3、向S2得到的粉料中添加有机粘合剂混合均匀,喷雾造粒得颗粒料,将颗粒料于200MPa压制成生坯样品;
S4、将S3得到的生坯样品升温至1050℃,保温60min;升温至1250℃,保温30min,升温过程中,氧分压维持在2%;升温至1450℃,保温1h,升温过程中,氧分压维持在18%;降温至900℃,保温4h;降温至室温得到宽频低损耗软磁铁氧体材料。
实施例4
本发明提出的一种宽频低损耗软磁铁氧体材料,由主料和辅料制成,主料和辅料的摩尔比为1:0.15,主料按摩尔百分比包括:氧化铁52.5mol%、氧化锰31.4mol%、氧化锌19.2mol%、氧化硅6.3mol%、余量为镍粉;以主料的重量为基准,辅料按重量百分比包括:碳酸钙0.03wt%、氧化锆0.045wt%、氧化铌0.020wt%、氧化锡0.18wt%、氧化钴0.38wt%、三氧化钼0.36wt%、氧化钙0.12wt%。
本发明的一种宽频低损耗软磁铁氧体材料的制备方法,包括如下步骤:
S1、将主料进行湿式混合,一次球磨95min,然后喷雾干燥,进行预烧,预烧温度为880℃,预烧时间为2.5h;
S2、向预烧主料中加入辅料、分散剂和消泡剂混合均匀,进行二次球磨2.5h,得到粒径为0.9微米的粉料;
S3、向S2得到的粉料中添加有机粘合剂混合均匀,喷雾造粒得颗粒料,将颗粒料于150MPa压制成生坯样品;
S4、将S3得到的生坯样品升温至1080℃,保温55min;升温至1280℃,保温25min,升温过程中,氧分压维持在2.5%;升温至1420℃,保温1.5h,升温过程中,氧分压维持在17%;降温至920℃,保温3.5h;降温至室温得到宽频低损耗软磁铁氧体材料。
实施例5
本发明提出的一种宽频低损耗软磁铁氧体材料,由主料和辅料制成,主料和辅料的摩尔比为1:0.25,主料按摩尔百分比包括:氧化铁52.5mol%、氧化锰29.2mol%、氧化锌21.4mol%、氧化硅4.9mol%、余量为镍粉;以主料的重量为基准,辅料按重量百分比包括:碳酸钙0.07wt%、氧化锆0.035wt%、氧化铌0.040wt%、氧化锡0.15wt%、氧化钴0.45wt%、三氧化钼0.32wt%、氧化钙0.24wt%。
本发明的一种宽频低损耗软磁铁氧体材料的制备方法,包括如下步骤:
S1、将主料进行湿式混合,一次球磨115min,然后喷雾干燥,进行预烧,预烧温度为820℃,预烧时间为3.5h;
S2、向预烧主料中加入辅料、分散剂和消泡剂混合均匀,进行二次球磨1.5h,得到粒径为1.1微米的粉料;
S3、向S2得到的粉料中添加有机粘合剂混合均匀,喷雾造粒得颗粒料,将颗粒料于100MPa压制成生坯样品;
S4、将S3得到的生坯样品升温至1120℃,保温25min;升温至1320℃,保温15min,升温过程中,氧分压维持在3.5%;升温至1380℃,保温2.5h,升温过程中,氧分压维持在13%;降温至980℃,保温2.5h;降温至室温得到宽频低损耗软磁铁氧体材料。
对实施例1-实施例5中得到的宽频低损耗软磁铁氧体材料进行性能测试,得到的特性如表1所示。
表1:
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 (7)

1.一种宽频低损耗软磁铁氧体材料,其特征在于,由主料和辅料制成,主料和辅料的摩尔比为1:(0.1-0.3),主料按摩尔百分比包括:氧化铁50.2-52.6mol%、氧化锰28.2-32.4mol%、氧化锌18.2-22.4mol%、氧化硅4.8-6.4mol%、余量为镍粉;以主料的重量为基准,辅料按重量百分比包括:碳酸钙0.02-0.08wt%、氧化锆0.03-0.05wt%、氧化铌0.020-0.040wt%、氧化锡0.15-0.18wt%、氧化钴0.38-0.45wt%、三氧化钼0.32-0.36wt%、氧化钙0.12-0.24wt%。
2.根据权利要求1所述的宽频低损耗软磁铁氧体材料,其特征在于,主料按摩尔百分比包括:氧化铁50.3-52.5mol%、氧化锰29.2-31.4mol%、氧化锌19.2-21.4mol%、氧化硅4.9-6.3mol%、余量为镍粉。
3.根据权利要求1或2所述的宽频低损耗软磁铁氧体材料,其特征在于,以主料的重量为基准,辅料按重量百分比包括:碳酸钙0.03-0.07wt%、氧化锆0.035-0.045wt%、氧化铌0.025-0.035wt%、氧化锡0.16-0.17wt%、氧化钴0.39-0.44wt%、三氧化钼0.33-0.35wt%、氧化钙0.14-0.22wt%。
4.根据权利要求1-3任一项所述的宽频低损耗软磁铁氧体材料,其特征在于,由主料和辅料制成,主料和辅料的摩尔比为1:(0.15-0.25),主料按摩尔百分比包括:氧化铁50.3-52.5mol%、氧化锰29.2-31.4mol%、氧化锌19.2-21.4mol%、氧化硅4.9-6.3mol%、余量为镍粉;以主料的重量为基准,辅料按重量百分比包括:碳酸钙0.03-0.07wt%、氧化锆0.035-0.045wt%、氧化铌0.020-0.040wt%、氧化锡0.15-0.18wt%、氧化钴0.38-0.45wt%、三氧化钼0.32-0.36wt%、氧化钙0.12-0.24wt%。
5.根据权利要求1-4任一项所述的宽频低损耗软磁铁氧体材料,其特征在于,由主料和辅料制成,主料和辅料的摩尔比为1:0.2,主料按摩尔百分比包括:氧化铁51.4mol%、氧化锰30.3mol%、氧化锌20.3mol%、氧化硅5.6mol%、余量为镍粉;以主料的重量为基准,辅料按重量百分比包括:碳酸钙0.05wt%、氧化锆0.04wt%、氧化铌0.030wt%、氧化锡0.165wt%、氧化钴0.415wt%、三氧化钼0.34wt%、氧化钙0.36wt%。
6.一种权利要求1-4任一项所述的宽频低损耗软磁铁氧体材料的制备方法,其特征在于,包括如下步骤:
S1、将主料进行湿式混合,一次球磨90-120min,然后喷雾干燥,进行预烧;
S2、向预烧主料中加入辅料、分散剂和消泡剂混合均匀,进行二次球磨1-3h,得到粒径为0.8-1.2微米的粉料;
S3、向S2得到的粉料中添加有机粘合剂混合均匀,喷雾造粒得颗粒料,将颗粒料于50-200MPa压制成生坯样品;
S4、将S3得到的生坯样品升温至1050-1150℃,保温20-60min;升温至1250-1350℃,保温10-30min,升温过程中,氧分压维持在2-4%;升温至1350-1450℃,保温1-3h,升温过程中,氧分压维持在12-18%;降温至900-1000℃,保温2-4h;降温至室温得到宽频低损耗软磁铁氧体材料。
7.根据权利要求6所述的宽频低损耗软磁铁氧体材料的制备方法,其特征在于,S1中,预烧温度为800-900℃,预烧时间为2-4h。
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