CN103360042A - 一种镍锌软磁铁氧体及其制备方法 - Google Patents
一种镍锌软磁铁氧体及其制备方法 Download PDFInfo
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Abstract
本发明提供了一种镍锌软磁铁氧体,包括主成分和辅助成分,所述主成分包括Fe2O3、NiO、ZnO和CuO,辅助成分包括Al2O3、V2O5和CaO;所述主成分中Fe2O3的含量为51~52mol%,NiO的含量为14.5~16mol%,ZnO的含量为15~18mol%,CuO的含量为14~18mol%。本发明通过对镍锌铁氧体各组分含量进行优化,并采用流延工艺成型坯片,烧结后制成厚度小于0.2mm的磁片,使磁片在厚度较薄的情况下仍可使天线模块具有较高的通讯距离。
Description
技术领域
本发明属于软磁材料技术领域,具体涉及一种镍锌软磁铁氧体。
背景技术
目前,手机等便携式信息终端向着小型化、紧凑型发展,金属元件高密度安装在小壳体内。因此,设置在便携式信息终端壳体内的非接触式IC标签用天线模块受到金属元件的影响,通讯性能较差,导致壳体内设置的天线模块比壳体外设置的天线模块通讯距离短。产生这种现象的原因是壳体内的金属部件在高频电磁场的作用下产生涡流效应,影响天线模块的通讯。
为了提高天线模块的通讯距离,需要在天线模块和金属部件之间增加磁芯部件,高导磁率的磁粉被用作磁芯部件的材料。其中由铁硅铝磁性合金制成的磁粉与有机物混合得到的磁片应用较广,同时铁氧体粉末的烧结物质也被用作磁芯材料,其磁导率比铁硅铝磁性合金更大。铁氧体材料由于其配方的不同磁性能差异很大,采用现有软磁铁氧体成分配方制备的磁片,虽然磁导率较大,但为了达到通讯距离的要求,磁片厚度一般偏厚,大于0.5mm,无法实现在磁片厚度较薄的情况下具有较高的磁导率,不能应对便携式信息终端小型化的趋势。
发明内容
为了解决现有技术中铁氧体磁片无法实现在厚度较薄的情况下具有较高的磁导率的问题,本发明提供了一种镍锌软磁铁氧体。
本发明的镍锌软磁铁氧体包括主成分和辅助成分,所述主成分包括Fe2O3、NiO、ZnO和CuO,辅助成分包括Al2O3、V2O5和CaO;所述主成分中Fe2O3的含量为51~52mol%,NiO的含量为14.5~16mol%,ZnO的含量为15~18mol%,CuO的含量为14~18mol%。
本发明的镍锌软磁铁氧体具有较高的Fe2O3含量,烧结过程中产生的Fe2+离子借助其正的磁晶各向异性常数补偿铁氧体的磁晶各向异性常数,达到提高磁导率的目的;而Fe2+的增加又会提高磁片电阻,导致磁损耗增加,本发明同时增加了CuO的含量,可以有效降低磁片电阻,从而降低磁损耗。而由于CuO含量的增加使烧结后晶粒异常长大,影响铁氧体的磁性能及机械性能,本发明添加了微量的Al2O3,有效地抑制了晶粒的长大。本发明还降低了ZnO的含量,有利于提高铁氧体的居里温度,提升产品性能。本发明还对NiO的含量进行了优化,具有较好的磁性能。辅助成分V2O5和CaO可以进入晶界,大大提高了铁氧体材料的晶界电阻率,有利于提高材料的品质因数。采用本发明的铁氧体材料配方经过流延成型工艺可以制成厚度小于0.2mm的磁片同时可以使天线模块具有良好的通讯距离,例如本发明的一个实施例,烧结后成品厚度为0.10±0.01mm的磁片,其通讯距离可达到67mm。
优选情况下,所述辅助成分中Al2O3的含量为0.1~1mol%、V2O5的含量为0.1~1mol%、CaO的含量为0.1~1mol%。所述辅助成分的含量不能太多,否则烧结后在磁片内形成气孔,影响磁片的磁性能和机械性能。
优选情况下,所述辅助成分还包括MnO2和Bi2O3,其中MnO2的含量为0.1~1mol%、Bi2O3的含量为0.1~1mol%。MnO2和Bi2O3在较低烧结温度下形成液相,提高磁片的致密度和机械强度,同时具有提高初始磁导率的作用。
优选情况下,所述辅助成分的总量为0.1~1mol%。辅助成分的含量必须控制在一定范围内,添加过多会影响磁片的机械强度和磁性能。
本发明还提供了一种镍锌软磁铁氧体的制备方法,包括以下步骤:
S1:按各金属氧化物的组分含量称取原料,进行湿法球磨;
S2:将湿法球磨后得到的粉末烘干;
S3:将经步骤S2烘干后的粉末预烧结;
S4:将经步骤S3预烧结的原料进行二次球磨,得到具有一定粒径的粉末材料;
S5:将步骤S4制得的粉末材料与有机体系混合后流延成型,制得铁氧体坯片;
S6:将步骤S5制得的铁氧体坯片进行叠压;
S7:烧结经步骤S6叠压后的坯片。
本发明采用流延工艺成型铁氧体坯片,可制备出厚度小于0.1mm的磁片,铁氧体粉末颗粒在浆料中均匀分布,保证磁片具有较高的均匀性和磁导率。
优选情况下,本发明的镍锌软磁铁氧体包括主成分和辅助成分,所述主成分包括Fe2O3、NiO、ZnO和CuO,辅助成分包括Al2O3、V2O5和CaO;所述主成分中Fe2O3的含量为51~52mol%,NiO的含量为14.5~16mol%,ZnO的含量为15~18mol%,CuO的含量为14~18mol%。
本发明的镍锌铁氧体的制备方法,通过优化配方中各种金属氧化物的组分含量,使磁片在较薄的情况下天线模块仍具有较高的通讯距离。具体为,Fe2O3含量的增加,在烧结过程中产生的Fe2+离子具有正的磁晶各向异性常数,提高了铁氧体的磁晶各向异性常数,从而提高了磁导率;而Fe2+的增加又会提高磁片电阻,导致磁损耗增加,因此本发明同时增加了CuO的含量,可以有效的降低磁片电阻,从而降低了磁损耗。而由于CuO含量的增加使烧结后晶粒异常长大,影响铁氧体的磁性能及机械性能,本发明添加了微量的Al2O3,有效地抑制了晶粒的长大。本发明还降低了ZnO的含量,有利于提高铁氧体的居里温度,提升产品性能。本发明还对NiO的含量进行了优化,具有较好的磁性能。辅助成分V2O5和CaO可以进入晶界,大大提高了铁氧体材料的晶界电阻率,有利于提高材料的品质因数。采用本发明的铁氧体材料配方经过流延成型工艺并高温烧结可以制成厚度小于0.2mm同时可以使天线模块具有良好的通讯距离的磁片。
优选情况下,本发明的镍锌铁氧体的制备方法所添加的辅助成分Al2O3的含量为0.1~1mol%、V2O5的含量为0.1~1mol%、CaO的含量为0.1~1mol%。所述辅助成分的含量不能太多,否则烧结后再磁片内形成气孔,影响磁片的磁性能和机械性能。
优选情况下,本发明的镍锌铁氧体的制备方法所添加的辅助成分还包括MnO2和Bi2O3,其中MnO2的含量为0.1~1mol%、Bi2O3的含量为0.1~1mol%。MnO2和Bi2O3在较低烧结温度下形成液相,提高磁片的致密度和机械强度,同时具有提高初始磁导率的作用。
优选情况下,本发明的镍锌铁氧体的制备方法所添加的辅助成分的总量为0.1~1mol%。辅助成分的含量必须控制在一定范围内,添加过多会影响磁片的机械强度和磁性能,添加过少由起不到相应的作用。
优选情况下,本发明的镍锌铁氧体的制备方法还包括对叠压后的磁片采用半切割工艺进行划片处理,划片处理可以防止坯片烧结过程中的翘曲现象,也有利于后续产品的组装。
附图说明
图1 为本发明的镍锌软磁铁氧体的制备工艺流程图。
具体实施方式
为了使本发明所解决的技术问题、技术方案及有益效果更加清楚明白,以下结合附图及实施例,对本发明作进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。
本发明提供了一种镍锌铁氧体,包括主成分和辅助成分,主成分包括Fe2O3、NiO、ZnO和CuO,辅助成分包括Al2O3、V2O5、CaO、MnO2、Bi2O3。所述主成分的含量为Fe2O3为51~52mol%、NiO为14.5~16mol%、ZnO为15~18mol%、CuO为14~18mol%,辅助成分中Al2O3为0.1~1mol%、V2O5为0.1~1mol%、CaO为0.1~1mol%、MnO2为0.1~1mol%、Bi2O3为0.1~1mol%,且辅助成分的总量为0.1~1mol%。
如图1所示,本发明镍锌铁氧体的制备工艺流程为:
S1:按照配比称取氧化物原料,进行湿法球磨4~12小时,球磨机的转速为200~400r/min。
S2:烘干经湿法球磨后的粉末,在40~120℃温度下,烘干2~8小时。
S3:对烘干后的粉末进行预烧结,以1~5℃/min的升温速率升温至1000~1100℃,保温1~4h后随炉冷却。
S4:二次球磨,将预烧结后的材料以300~500r/min的转速再次球磨8~14h,控制球磨后的粉末粒径为2~5μm。
S5:流延成型,将步骤S4中制得的粉末与行业内公知的有机体系混合制成浆料,并将浆料进行球磨、脱泡处理,然后通过流延工艺制成厚度为0.05~0.08mm的铁氧体坯片。所述有机体系中溶剂为乙醇与甲苯体系的混合物,粘结剂为聚乙烯醇缩丁醛,增塑剂为邻苯二甲酸二丁酯。
S6:将流延成型后的坯片进行烘干和裁切,之后将两层坯片以5~50MPa的压力保压0.5~5min进行叠压。优选情况下,对叠压后的坯片采用半切割工艺进行划片处理,在坯片表层形成连续的(0.5~3mm)×(0.5~3mm)的方格结构,划片深度为磁片厚度的1/3~1/2。
S7:成品烧结,以0.5~3℃的升温速率,在250℃保温20~100min; 600℃保温20~100min;900℃保温20~100min;最高温度1050℃~1150℃下保温60~180min;然后随炉冷却,制得本发明的镍锌软磁铁氧体磁片。
本发明的镍锌软磁铁氧体具有较高的Fe2O3含量,烧结过程中产生的Fe2+离子借助其正的磁晶各向异性常数补偿铁氧体的磁晶各向异性常数,达到提高磁导率的目的;而Fe2+的增加又会提高磁片电阻,导致磁损耗增加,本发明同时增加了CuO的含量,可以有效降低磁片电阻,从而降低磁损耗。而由于CuO含量的增加使烧结后晶粒异常长大,影响铁氧体的磁性能及机械性能,本发明添加了微量的Al2O3,有效地抑制了晶粒的长大。本发明还降低了ZnO的含量,有利于提高铁氧体的居里温度,提升产品性能。本发明还对NiO的含量进行了优化,具有较好的磁性能。辅助成分V2O5和CaO可以进入晶界,大大提高了铁氧体材料的晶界电阻率,有利于提高材料的品质因数。采用本发明的铁氧体材料配方经过流延成型工艺可以制成厚度小于0.1mm的磁片,同时具有该磁片的天线模块通讯距离良好。
以下结合具体实施例,对本发明做进一步详细说明:
实施例1:
主成分中Fe2O3为51.5mol%、NiO为14.5mol%、ZnO为16mol%、CuO为17mol%,辅助成分中Al2O3为0.4mol%、V2O5为0.2mol%、CaO为0.15mol%、MnO2为0.1mol%、Bi2O3为0.15mol%。
制备工艺流程为:
(1)、按上述配比称取金属氧化物原料,以200r/min的转速湿法球磨12h。
(2)、在120℃下对湿法球磨后的粉末烘干4h。
(3)、以2℃/min的升温速率升温至1050℃对金属粉末进行预烧结,保温2h后,随炉冷却。
(4)、以400r/min的转速二次球磨10h。
(5)、流延成型,所用的有机体系中溶剂为乙醇和甲苯体系的混合物,粘结剂为聚乙烯醇缩丁醛,增塑剂为邻苯二甲酸二丁酯,制成厚度为0.08mm的坯片。
(6)、叠压,两层坯片之间以30MPa的压力保压5min。
(7)、对叠压后的坯片采用半切割工艺进行划片处理,采用热切机在坯片表面形成连续的2mm×2mm的方格结构,切割深度为坯片厚度的1/3。
(8)、成品烧结,以1℃的升温速率,升温至250℃保温60min,600℃保温60min,900℃保温30min,最高温度为1050℃,保温120min,之后随炉冷却。烧结后制得的成品厚度为0.10±0.01mm。
实施例2:
本实施例中主成分Fe2O3为52mol%、NiO为14.5 mol%、ZnO为15mol%、CuO为17.5mol%,辅助成分中Al2O3为0.4mol%、V2O5为0.2mol%、CaO为0.15mol%、MnO2为0.1mol%、Bi2O3为0.15mol%。
制备工艺与实施例1相同。
实施例3:
本实施例主成分Fe2O3为51mol%、NiO为14.5mol%、ZnO为17mol%、CuO为16.5mol%,辅助成分Al2O3为0.4mol%、V2O5为0.2mol%、CaO为0.15mol%、MnO2为0.1mol%、Bi2O3为0.15mol%。
制备工艺与实施例1相同。
实施例4:
本实施例主成分Fe2O3为51.5mol%、NiO为15.5mol%、ZnO为18mol%、CuO为14mol%,辅助成分Al2O3为0.4mol%、V2O5为0.2mol%、CaO为0.15mol%、MnO2为0.1mol%、Bi2O3为0.15mol%。
制备工艺与实施例1相同。
实施例5:
本实施例中主成分Fe2O3为51.5mol%、NiO为14.5mol%、ZnO为16mol%、CuO为17mol%,辅助成分中Al2O3为0.4mol%、V2O5为0.2mol%、CaO为0.15mol%、MnO2为0.1mol%、Bi2O3为0.15mol%。
制备工艺中流延成型制成的坯片厚度为0.05mm,烧结后成品磁片的厚度为0.065±0.01mm,其他工艺与实施例1相同。
对比例1:
Fe-Si-Al磁性合金,其中含Fe85wt%、Si9.5wt%和Al5.5wt%。
制备工艺如下:
(1)片状粉料制备:称取氧化物原料,进行湿法球磨12h,转速为500r/min,球料比为5:1。
(2)将球磨后的粉料在80℃下烘干2h。
(3)流延成型,将行业内熟知的有机体系与粉料混合后流延成厚度为0.1mm的坯片。
(4)叠压,四层坯片采用20MPa的压力,在120℃的温度下保压4min。
成品厚度为0.20±0.01mm。
对比例2:
镍锌铁氧体,其成分中Fe2O3为49.3mol%、NiO为28.9mol%、ZnO为12.6mol%、CuO为9.2mol%。辅助成分中Al2O3为0.4mol%、V2O5为0.2mol%、CaO为0.15mol%、MnO2为0.1mol%、Bi2O3为0.15mol%。
制备工艺与实施例1相同。
对上述实施例和对比例中的磁片及包含磁片的天线模块进行以下测试:
1、复数磁导率测试:
采用美国Aglient公司生产E4991阻抗分析仪及磁导率测量专用夹具16454A,把被测材料制成三维圆环体,将该圆环体看做一个单匝线圈,通过测量该线圈的阻抗可得到圆环线圈电感的大小,继而计算出被测材料磁导率的大小,并给出1M到1G 频率下复数磁导率的变化趋势,由于本实验应用范围在13.56MHz,所以数据点取13.56MHz的复数磁导率。
2、天线特性测试:
采用美国Aglient公司生产E4991阻抗分析仪测试标准天线匹配磁片后在13.56MHz频率下的L、R、Q值。
3、天线通讯距离测试
自制通讯距离测试仪,该测试仪包括可以上下移动的夹具、带有近距离通讯功能的的手机和标准卡。手机固定在夹具上,移动夹具靠近标准卡,当手机和标准卡之间达到一定距离时会实现通讯并产生提示信号,该最远距离即为天线通讯距离。
表1:实施例和对比例性能测试
从表1中可以看出,本发明的镍锌软磁铁氧体在辅助成分含量相同的情况下,随着主成分中各组分含量的不同,磁芯的性能也不同。其中实施例1的效果最佳,磁芯材料具有较高的品质因数,即具有较高的磁导率和较低的磁损耗,在磁片厚度为0.10±0.01mm情况下,天线模块的通讯距离可达到67mm。
实施例5中的镍锌铁氧体磁芯材料其各组分含量与实施例1相同,制成的磁片厚度比实施例1更薄,天线模块的通讯距离有所下降。
本发明的各实施例相对于对比例1中铁硅铝磁性合金的各方面性能具有明显优势,而对比例2中的镍锌铁氧体磁芯虽然成分与本发明相同,但各成分的含量不在本发明的优选范围内,磁芯的品质因数和天线模块的通讯距离较差。
Claims (10)
1.一种镍锌软磁铁氧体,其特征在于,包括主成分和辅助成分,所述主成分包括Fe2O3、NiO、ZnO和CuO,辅助成分包括Al2O3、V2O5和CaO;所述主成分中Fe2O3的含量为51~52mol%,NiO的含量为14.5~16mol%,ZnO的含量为15~18mol%,CuO的含量为14~18mol%。
2.根据权利要求1所述的镍锌软磁铁氧体,其特征在于,所述辅助成分中Al2O3的含量为0.1~1mol%、V2O5的含量为0.1~1mol%、CaO的含量为0.1~1mol%。
3.根据权利要求1所述的镍锌软磁铁氧体,其特征在于,所述辅助成分还包括MnO2和Bi2O3,其中MnO2的含量为0.1~1mol%、Bi2O3的含量为0.1~1mol%。
4.根据权利要求1至3中任意一项所述的镍锌软磁铁氧体,其特征在于,所述辅助成分的总量为0.1~1mol%。
5.一种镍锌软磁铁氧体的制备方法,其特征在于,包括以下步骤:
S1:按各金属氧化物的组分含量称取原料,进行湿法球磨;
S2:将湿法球磨后得到的粉末烘干;
S3:将经步骤S2烘干后的粉末预烧结;
S4:将经步骤S3预烧结的原料进行二次球磨,得到具有一定粒径的粉末材料;
S5:将步骤S4制得的粉末材料与有机体系混合后流延成型,制得铁氧体坯片;
S6:将步骤S5制得的铁氧体坯片进行叠压;
S7:烧结经步骤S6叠压后的坯片。
6.根据权利要求5所述的镍锌软磁铁氧体的制备方法,其特征在于,所述镍锌软磁铁氧体包括主成分和辅助成分,所述主成分包括Fe2O3、NiO、ZnO和CuO,辅助成分包括Al2O3、V2O5和CaO;所述主成分中Fe2O3的含量为51~52mol%,NiO的含量为14.5~16mol%,ZnO的含量为15~18mol%,CuO的含量为14~18mol%。
7.根据权利要求6所述的镍锌软磁铁氧体的制备方法,其特征在于,所述辅助成分中Al2O3的含量为0.1~1mol%、V2O5的含量为0.1~1mol%、CaO的含量为0.1~1mol%。
8.根据权利要求7所述的镍锌软磁铁氧体的制备方法,其特征在于,所述辅助成分还包括MnO2和Bi2O3,其中MnO2的含量为0.1~1mol%、Bi2O3的含量为0.1~1mol%。
9.根据权利要求6至8中任意一项所述的镍锌软磁铁氧体的制备方法,其特征在于,所述辅助成分的总量为0.1~1mol%。
10.根据权利要求5所述的镍锌软磁铁氧体的制备方法,其特征在于,所述步骤S6之后还包括对叠压后的铁氧体坯片进行划片处理。
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CN104051114A (zh) * | 2014-06-24 | 2014-09-17 | 铜陵三佳变压器有限责任公司 | 一种变压器用铬基铁氧体磁芯材料 |
CN104844184A (zh) * | 2015-04-27 | 2015-08-19 | 厦门大学 | 一种低磁导率温度系数近场通讯磁片及其制备方法 |
CN106242545A (zh) * | 2016-07-13 | 2016-12-21 | 深圳顺络电子股份有限公司 | 一种非磁性铁氧体、叠层电子器件及其制备方法 |
CN106242545B (zh) * | 2016-07-13 | 2019-01-18 | 深圳顺络电子股份有限公司 | 一种非磁性铁氧体、叠层电子器件及其制备方法 |
CN107230541A (zh) * | 2017-06-08 | 2017-10-03 | 东莞信柏结构陶瓷股份有限公司 | 磁性材料及其制备方法 |
CN108154989A (zh) * | 2017-12-25 | 2018-06-12 | 日照亿鑫电子材料有限公司 | 一种钛基稀土铁磁芯材料 |
CN109231978A (zh) * | 2018-08-20 | 2019-01-18 | 浙江大学 | 一种高频高磁导率铁氧体片及其制备方法 |
CN112830776A (zh) * | 2021-03-25 | 2021-05-25 | 电子科技大学 | 一种u型六角铁氧体材料及其制备方法 |
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