CN112979300A - 一种高频低损耗的钽掺杂锰锌铁氧体材料及其制备方法 - Google Patents

一种高频低损耗的钽掺杂锰锌铁氧体材料及其制备方法 Download PDF

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CN112979300A
CN112979300A CN202110206808.5A CN202110206808A CN112979300A CN 112979300 A CN112979300 A CN 112979300A CN 202110206808 A CN202110206808 A CN 202110206808A CN 112979300 A CN112979300 A CN 112979300A
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tantalum
oxide
manganese
zinc ferrite
ferrite material
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江昊杰
严鹏飞
严彪
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Tongji University
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Abstract

本发明涉及一种高频低损耗的钽掺杂锰锌铁氧体材料及其制备,钽掺杂锰锌铁氧体材料包括主料和掺杂料,主料包括氧化铁、氧化锰和氧化锌,氧化铁、氧化锰和氧化锌的质量比为(70~71):(21~22):(7~8),掺杂料包括钽。制备为:S1:将主料加入球磨机进行球磨,得到混合料A;S2:将混合料A进行预烧,然后冷却至室温得到预烧料B;S3:将预烧料B和掺杂料加入球磨机进行二次球磨,后烘干得到混合料C;S4:向混合料C中加入聚乙烯醇溶液混合进行喷雾造粒,后过筛得到粉末颗粒;S5:将粉末颗粒放入模具,压制成型,得到坯件;S6:将坯件在平衡气氛下进行烧结。与现有技术相比,本发明的材料成分均匀分布,晶界电阻率高,产品在MHz级的频率下的损耗进一步降低。

Description

一种高频低损耗的钽掺杂锰锌铁氧体材料及其制备方法
技术领域
本发明属于磁性材料技术领域,尤其是涉及一种高频低损耗的钽掺杂锰锌铁氧体材料及其制备方法。
背景技术
锰锌铁氧体作为软磁材料的一种,广泛应用于电力工业设备、家电仪器及信息化技术领域等,是目前产量最大、用量也最大的一种软磁材料,在兆赫兹级别的电子元器件中有着不可替代的作用。随着5G通信技术,物联网技术的迅猛发展,电子元器件也向着小型化、高效化、低损化的方向迈进,对磁性材料的要求也越来越高。在电力电工及通信技术领域,低损耗永远是一个努力追求的目标。现有技术中的软磁铁氧体的高频损耗量无法满足现有技术的需求。因此,亟需设计一种高频低损耗的软磁铁氧体材料来解决现有技术中的问题。
电源系统向轻、薄、小和高效率方向发展,要求电子元器件承载更大的功率密度,磁心材料亟需进一步提高饱和磁通密度。
专利CN101183585A公开了一种锰锌MnZn铁氧体材料及磁芯以及磁芯制造方法,所述的锰锌MnZn软磁铁氧体材料,其主成分为49.5~53.8mol%的氧化铁Fe2O3、34.6~39.8mol%的氧化锰MnO和8.5~13.8mol%的氧化锌ZnO,在主成分中还需添加以重量计100~600ppm的第一副组分和以重量计50~3000ppm的第二副组分,第一副组分是指二氧化硅SiO2、五氧化二钽Ta2O5中的至少一种,第二副组分是指三氧化二铋Bi2O3、五氧化二铌Nb2O5、三氧化钨WO3中的至少一种。该锰锌MnZn铁氧体材料中含有的是五氧化二钽,而非单质钽,且该材料使用频率范围较低,仅在25kHz左右,远低于本发明中的MHz级,且其起始磁导率并不高。
专利CN111470857A公开了一种高频锰锌铁氧体材料及其制备方法。所述高频锰锌铁氧体材料的基体原料组成以Fe2O3、MnO和ZnO的总量为100mol%计,Fe2O3的含量为amol%,ZnO的含量为b mol%,余量为MnO,其中52≤a≤55,0<b≤12;所述高频锰锌铁氧体材料中还含有添加物,添加物含量以基体原料的总质量为100wt%计包括:钇铁石榴石100~1000ppm和钛酸钡100~1000ppm,所述添加物中还含有:二氧化锡500~5000ppm、五氧化二钒100~1000ppm和五氧化二钽50~500ppm。该锰锌铁氧体材料中含有的是五氧化二钽,而非单质钽,且该材料磁芯的磁导率与本发明相当,但其在500kHz下的损耗在650kW/m3左右,损耗较高,仍有较大提升空间。
综合上述专利,均未提及所研发锰锌铁氧体的饱和磁感应强度,而在控制降低损耗的同时,保持较高的饱和磁感应强度(>0.5T)也是电子元器件小型化的重要目标。
发明内容
本发明的目的就是为了解决上述问题而提供一种高频低损耗的钽掺杂锰锌铁氧体材料及其制备方法。
本发明的目的通过以下技术方案实现:
一种高频低损耗的钽掺杂锰锌铁氧体材料,包括主料和掺杂料,所述主料包括氧化铁、氧化锰和氧化锌,所述氧化铁、氧化锰和氧化锌的质量比为(70~71):(21~22):(7~8),所述掺杂料包括第一副成分,所述第一副成分为单质钽。钽掺杂锰锌铁氧体材料具有不低的起始磁导率(1600~2500)、较高的饱和磁通密度(0.50~0.52T)、较适宜的居里温度(220~260℃)以及较低的高频损耗(338~380kW/m3)。
所述掺杂料中还包括第二副成分,所述第二副成分选自五氧化二钒、五氧化二铌、氧化铋、氧化钴、氧化钼、五氧化二磷或碳酸钙中的一种或多种混合。
所述材料中,以材料原料的总质量为100wt%计,掺杂料的总量为100~2350PPM。
所述材料中,以材料原料的总质量为100wt%计,第一副成分的含量为100~350PPM,优选为150~300PPM。
所述材料中,以材料原料的总质量为100wt%计,第二副成分的总量为500~2000PPM,优选为800~1600PPM,进一步优选为1000~1300PPM。具体地,五氧化二钒、五氧化二铌、氧化铋、氧化钴、氧化钼、五氧化二磷和碳酸钙的含量分别为100~300PPM(优选为100~200PPM)、100~300PPM(优选为100~150PPM)、100~200PPM(优选为100~150PPM)、200~400PPM(优选为200~300PPM)、300~500PPM(优选为250~300PPM)、50~150PPM(优选为50~70PPM)、150~250PPM(优选为150~200PPM)。
一种如上述所述的钽掺杂锰锌铁氧体材料的制备方法,所述制备方法具体包括以下步骤:
S1:将氧化铁、氧化锰和氧化锌加入球磨机进行球磨,得到混合料A;
S2:将混合料A进行预烧,然后冷却至室温得到预烧料B;
S3:将预烧料B和掺杂料加入球磨机进行二次球磨,之后烘干,得到混合料C;
S4:向混合料C中加入聚乙烯醇溶液混合进行喷雾造粒,然后过筛得到粉末颗粒,其中,聚乙烯醇起粘接剂的作用,经烧结后不再留存于材料中;
S5:将粉末颗粒放入模具,进行压制成型,得到坯件;
S6:将坯件在平衡气氛下进行烧结,即得到所述钽掺杂锰锌铁氧体材料。
步骤S1中,球磨机的转速为200~250r/min,优选为200~220r/min,球磨时间为2~7h。充分的球磨可以使主料间相互挤压破碎,使得粉末颗粒形成较高的表面能,使得在后续预烧过程中形成部分铁氧体相,改善后续烧结的变形异常。
步骤S2中,在空气气氛下进行预烧,预烧温度为850~900℃,预烧时间为50~90min,优选为60~70min。
步骤S3中,球磨机的转速为200~250r/min,优选为200~210r/min,球磨时间为6~8h,优选为6~7h,置于真空烘箱中进行烘干,烘干的温度为70~80℃,烘干的时间为20~24h,优选为24h,目测粉末无明显团聚为好。
步骤S4中,混合料C与适量聚乙烯醇溶液混合造粒后过100~120目筛,优选为100目筛。
步骤S5中,利用恒载荷压力机进行压制成型,恒载荷压力机施加的载荷为400~500MPa,优选为400~450MPa,保压340~380s,优选为360s。
步骤S6中,烧结过程具体为:先在真空条件下以2℃/min的速度升温至400℃,再以5℃/min的速度升温至600℃,随后在高纯氮气氛下以3℃/min的速度升温至1200℃,之后充入空气调整至5%氧分压,以1℃/min的速度升温至1200~1315℃,优选为1270~1300℃,保温4~6h,优选为5h,最后在平衡条件下以5℃/min的速度降温至室温,冷却过程中通高纯氮。
本发明中,过铁配方的主料可以保证较高的饱和磁感应强度以及较高的居里温度。五氧化二钒、五氧化二铌、氧化铋、氧化钴、氧化钼、五氧化二磷、碳酸钙等是常规添加的掺杂小料。五氧化二钒、氧化铋、氧化钼等低熔点物质在烧结时易形成液相,降低烧结温度,能够提升烧结密度和减少气孔率,使晶粒更加均匀,能够有效地改善饱和磁感应强度和损耗;五氧化二铌能够抑制晶粒的异常生长,使晶粒均匀;氧化钴固溶于晶格改善电磁性能;五氧化二磷、碳酸钙主要存在于晶界起到改善微结构和增大材料电阻率的作用。适量的掺杂料可以帮助铁氧体在烧结过程中形成尺寸合适,大小均匀的晶粒(约为10~20μm),排出气孔,提高密度(约为4.8~5.0g/cm3),在晶界沉积的同时提高材料电阻率。此外,本发明独特添加的单质钽,在晶粒边界以类似屏障作用阻挡无机非金属元素进入晶粒,使掺杂元素聚集于晶界,并且均匀分布,提高晶界电阻率,使得产品在MHz级的频率下的损耗进一步降低。
具体实施方式
下面结合具体实施例对本发明进行详细说明,但绝不是对本发明的限制。
一种高频低损耗的钽掺杂锰锌铁氧体材料,包括主料和掺杂料,主料包括氧化铁、氧化锰和氧化锌,氧化铁、氧化锰和氧化锌的质量比为(70~71):(21~22):(7~8),以材料原料的总质量为100wt%计,掺杂料的含量为500~2350PPM。
掺杂料包括第一副成分,第一副成分为单质钽,以材料原料的总质量为100wt%计,单质钽的含量为100~350PPM。
掺杂料中还包括第二副成分,第二副成分选自五氧化二钒、五氧化二铌、氧化铋、氧化钴、氧化钼、五氧化二磷或碳酸钙中的一种或多种混合。以材料原料的总质量为100wt%计,第二副成分的含量为500~2000PPM,具体地,五氧化二钒、五氧化二铌、氧化铋、氧化钴、氧化钼、五氧化二磷和碳酸钙的含量分别为100~300PPM、100~300PPM、100~200PPM、200~400PPM、300~500PPM、50~150PPM、150~250PPM。
一种如上述所述的钽掺杂锰锌铁氧体材料的制备方法,具体包括以下步骤:
S1:将氧化铁、氧化锰和氧化锌加入球磨机进行球磨,球磨机的转速为200~250r/min,球磨时间为2~7h,得到混合料A;
S2:将混合料A在空气气氛下进行预烧,预烧温度为850~900℃,预烧时间为50~90min,然后冷却至室温得到预烧料B;
S3:将预烧料B和掺杂料加入球磨机进行二次球磨,球磨机的转速为200~250r/min,球磨时间为6~8h,之后烘干,烘干的温度为70~80℃,烘干的时间为20~24h,得到混合料C;
S4:向混合料C中加入适量聚乙烯醇溶液混合进行喷雾造粒,然后过100~120目筛得到粉末颗粒;
S5:将粉末颗粒放入模具,利用恒载荷压力机进行压制成型,恒载荷压力机施加的载荷为400~500MPa,保压340~380s,得到坯件;
S6:将坯件在平衡气氛下进行烧结,烧结过程具体为:先在真空条件下以2℃/min的速度升温至400℃,再以5℃/min的速度升温至600℃,随后在高纯氮气氛下以3℃/min的速度升温至1200℃,之后充入空气调整至5%氧分压,以1℃/min的速度升温至1250~1315℃,保温4~6h,最后在平衡条件下以5℃/min的速度降温至室温,冷却过程中通高纯氮,即得到所述钽掺杂锰锌铁氧体材料。
实施例1
一种高频低损耗的钽掺杂锰锌铁氧体材料,包括主料和掺杂料,主料包括氧化铁、氧化锰和氧化锌,氧化铁、氧化锰和氧化锌的质量比为70:22:8,掺杂料包括第一副成分和第二副成分,第二副成分为五氧化二钒、五氧化二铌、氧化铋、氧化钴、氧化钼、五氧化二磷和碳酸钙的混合,第一副成分为单质钽。该材料采用以下步骤制备得到:
S1:按照配比称取140g氧化铁、44g氧化锰和16g氧化锌,并加入球磨机进行球磨,球磨机的转速为200r/min,球磨时间为2h,得到混合料A;
S2:将混合料A在850℃和空气气氛下进行预烧60min,然后冷却至室温得到预烧料B;
S3:按照配比,将预烧料B和掺杂料(包括五氧化二钒、五氧化二铌、氧化铋、氧化钴、氧化钼、五氧化二磷、碳酸钙和钽,加入的量依次为100PPM、100PPM、100PPM、200PPM、300PPM、50PPM、150PPM、100PPM)加入球磨机进行二次球磨,球磨机的转速为200r/min,球磨时间为6h,在70℃下烘干24h,得到混合料C;
S4:向混合料C中加入聚乙烯醇溶液混合进行喷雾造粒,然后过100目筛,得到粉末颗粒;
S5:将粉末颗粒放入环形模具,利用恒载荷压力机进行压制成型,恒载荷压力机施加的载荷为400MPa,保压360s,得到坯件;
S6:将坯件在1270℃的温度下进行平衡气氛烧结,烧结过程具体为:先在真空条件下以2℃/min的速度升温至400℃,再以5℃/min的速度升温至600℃,随后在高纯氮气氛下以3℃/min的速度升温至1200℃,之后充入空气调整至5%氧分压,以1℃/min的速度升温至1270℃,保温5h,最后在平衡条件下以5℃/min的速度降温至室温,冷却过程中通高纯氮,得到钽掺杂锰锌铁氧体材料,即磁环,具有约为10~18μm大小的晶粒和4.84g/cm3的密度,利用直流软磁测量仪测得该磁环的磁环起始磁导率为1600,饱和磁感应强度为0.51T;利用交流软磁测量仪在100℃、3MHz和10mT条件下测得损耗为380kW/m3;利用居里点测试仪测得居里温度为220℃,汇总于表1。
实施例2
一种高频低损耗的钽掺杂锰锌铁氧体材料,包括主料和掺杂料,主料包括氧化铁、氧化锰和氧化锌,氧化铁、氧化锰和氧化锌的质量比为71:22:7,掺杂料包括第一副成分和第二副成分,第二副成分为五氧化二钒、五氧化二铌、氧化铋、氧化钴、氧化钼、五氧化二磷和碳酸钙的混合,第一副成分为单质钽。该材料采用以下步骤制备得到:
S1:按照配比称取142g氧化铁、44g氧化锰和14g氧化锌,并加入球磨机进行球磨,球磨机的转速为205r/min,球磨时间为2.5h,得到混合料A;
S2:将混合料A在880℃和空气气氛下进行预烧60min,然后冷却至室温得到预烧料B;
S3:按照配比,将预烧料B和掺杂料(包括五氧化二钒、五氧化二铌、氧化铋、氧化钴、氧化钼、五氧化二磷、碳酸钙和钽,加入的量依次为150PPM、100PPM、120PPM、200PPM、300PPM、50PPM、150PPM、150PPM)加入球磨机进行二次球磨,球磨机的转速为205r/min,球磨时间为6.5h,在70℃下烘干24h,得到混合料C;
S4:向混合料C中加入适量聚乙烯醇溶液混合进行喷雾造粒,然后过100目筛,得到粉末颗粒;
S5:将粉末颗粒放入环形模具,利用恒载荷压力机进行压制成型,恒载荷压力机施加的载荷为450MPa,保压360s,得到坯件;
S6:将坯件在1290℃的温度下进行平衡气氛烧结,烧结过程具体为:先在真空条件下以2℃/min的速度升温至400℃,再以5℃/min的速度升温至600℃,随后在高纯氮气氛下以3℃/min的速度升温至1200℃,之后充入空气调整至5%氧分压,以1℃/min的速度升温至1290℃,保温5h,最后在平衡条件下以5℃/min的速度降温至室温,冷却过程中通高纯氮,得到钽掺杂锰锌铁氧体材料,即磁环,具有约为12~18μm大小的晶粒和4.90g/cm3的密度,利用直流软磁测量仪测得该磁环的磁环起始磁导率为2000,饱和磁感应强度为0.52T;利用交流软磁测量仪在100℃、3MHz和10mT条件下测得损耗为360kW/m3;利用居里点测试仪测得居里温度为240℃,汇总于表1。
实施例3
一种高频低损耗的钽掺杂锰锌铁氧体材料,包括主料和掺杂料,主料包括氧化铁、氧化锰和氧化锌,氧化铁、氧化锰和氧化锌的质量比为72:21:8,掺杂料包括第一副成分和第二副成分,第二副成分为五氧化二钒、五氧化二铌、氧化铋、氧化钴、氧化钼、五氧化二磷和碳酸钙的混合,第一副成分为单质钽。该材料采用以下步骤制备得到:
S1:按照配比称取144g氧化铁、42g氧化锰和16g氧化锌,并加入球磨机进行球磨,球磨机的转速为210r/min,球磨时间为4h,得到混合料A;
S2:将混合料A在900℃和空气气氛下进行预烧65min,然后冷却至室温得到预烧料B;
S3:按照配比,将预烧料B和掺杂料(包括五氧化二钒、五氧化二铌、氧化铋、氧化钴、氧化钼、五氧化二磷、碳酸钙和钽,加入的量依次为150PPM、150PPM、150PPM、200PPM、300PPM、70PPM、150PPM、150PPM)加入球磨机进行二次球磨,球磨机的转速为210r/min,球磨时间为7h,在80℃下烘干24h,得到混合料C;
S4:向混合料C中加入聚乙烯醇溶液混合进行喷雾造粒,然后过100目筛,得到粉末颗粒;
S5:将粉末颗粒放入环形模具,利用恒载荷压力机进行压制成型,恒载荷压力机施加的载荷为450MPa,保压360s,得到坯件;
S6:将坯件在1300℃的温度下进行平衡气氛烧结,烧结过程具体为:先在真空条件下以2℃/min的速度升温至400℃,再以5℃/min的速度升温至600℃,随后在高纯氮气氛下以3℃/min的速度升温至1200℃,之后充入空气调整至5%氧分压,以1℃/min的速度升温至1300℃,保温5h,最后在平衡条件下以5℃/min的速度降温至室温,冷却过程中通高纯氮,得到钽掺杂锰锌铁氧体材料,即磁环,具有约为15~18μm大小的晶粒和4.91g/cm3的密度,利用直流软磁测量仪测得该磁环的磁环起始磁导率为2500,饱和磁感应强度为0.52T;利用交流软磁测量仪在100℃、3MHz和10mT条件下测得损耗为338kW/m3;利用居里点测试仪测得居里温度为260℃,汇总于表1。
实施例4
一种高频低损耗的钽掺杂锰锌铁氧体材料,包括主料和掺杂料,主料包括氧化铁、氧化锰和氧化锌,氧化铁、氧化锰和氧化锌的质量比为70.5:22:7.5,掺杂料包括第一副成分和第二副成分,第二副成分为五氧化二钒、五氧化二铌、氧化铋、氧化钴、氧化钼、五氧化二磷和碳酸钙的混合,第一副成分为单质钽。该材料采用以下步骤制备得到:
S1:按照配比称取141g氧化铁、44g氧化锰和15g氧化锌,并加入球磨机进行球磨,球磨机的转速为220r/min,球磨时间为4h,得到混合料A;
S2:将混合料A在900℃和空气气氛下进行预烧70min,然后冷却至室温得到预烧料B;
S3:按照配比,将预烧料B和掺杂料(包括五氧化二钒、五氧化二铌、氧化铋、氧化钴、氧化钼、五氧化二磷、碳酸钙和钽,加入的量依次为200PPM、120PPM、120PPM、300PPM、250PPM、70PPM、200PPM、300PPM)加入球磨机进行二次球磨,球磨机的转速为210r/min,球磨时间为7h,在80℃下烘干24h,得到混合料C;
S4:向混合料C中加入聚乙烯醇溶液混合进行喷雾造粒,然后过100目筛,得到粉末颗粒;
S5:将粉末颗粒放入环形模具,利用恒载荷压力机进行压制成型,恒载荷压力机施加的载荷为450MPa,保压360s,得到坯件;
S6:将坯件在1300℃的温度下进行平衡气氛烧结,烧结过程具体为:先在真空条件下以2℃/min的速度升温至400℃,再以5℃/min的速度升温至600℃,随后在高纯氮气氛下以3℃/min的速度升温至1200℃,之后充入空气调整至5%氧分压,以1℃/min的速度升温至1300℃,保温5h,最后在平衡条件下以5℃/min的速度降温至室温,冷却过程中通高纯氮,得到钽掺杂锰锌铁氧体材料,即磁环,具有约为15~20μm大小的晶粒和4.93g/cm3的密度,利用直流软磁测量仪测得该磁环的磁环起始磁导率为2400,饱和磁感应强度为0.50T;利用交流软磁测量仪在100℃、3MHz和10mT条件下测得损耗为352kW/m3;利用居里点测试仪测得居里温度为255℃,汇总于表1。
对比例1
一种锰锌铁氧体材料,包括主料和掺杂料,主料包括氧化铁、氧化锰和氧化锌,氧化铁、氧化锰和氧化锌的质量比为72:21:8,掺杂料包括五氧化二钒、五氧化二铌、氧化铋、氧化钴、氧化钼、五氧化二磷、碳酸钙。该材料采用以下步骤制备得到:
S1:按照配比称取144g氧化铁、42g氧化锰和16g氧化锌,并加入球磨机进行球磨,球磨机的转速为210r/min,球磨时间为4h,得到混合料A;
S2:将混合料A在900℃和空气气氛下进行预烧65min,然后冷却至室温得到预烧料B;
S3:按照配比,将预烧料B和掺杂料(包括五氧化二钒、五氧化二铌、氧化铋、氧化钴、氧化钼、五氧化二磷、碳酸钙,加入的量依次为150PPM、150PPM、150PPM、200PPM、300PPM、70PPM、150PPM)加入球磨机进行二次球磨,球磨机的转速为210r/min,球磨时间为7h,在80℃下烘干24h,得到混合料C;
S4:向混合料C中加入聚乙烯醇溶液混合进行喷雾造粒,然后过100目筛,得到粉末颗粒;
S5:将粉末颗粒放入环形模具,利用恒载荷压力机进行压制成型,恒载荷压力机施加的载荷为450MPa,保压360s,得到坯件;
S6:将坯件在1300℃的温度下进行平衡气氛烧结,烧结过程具体为:先在真空条件下以2℃/min的速度升温至400℃,再以5℃/min的速度升温至600℃,随后在高纯氮气氛下以3℃/min的速度升温至1200℃,之后充入空气调整至5%氧分压,以1℃/min的速度升温至1300℃,保温5h,最后在平衡条件下以5℃/min的速度降温至室温,冷却过程中通高纯氮,得到无钽掺杂对应于实施例3的锰锌铁氧体材料,具有约为15~20μm大小的晶粒和4.90g/cm3的密度。利用直流软磁测量仪测得该磁环的磁环起始磁导率为2550,饱和磁感应强度为0.51T;利用交流软磁测量仪在100℃、3MHz和10mT条件下测得损耗为480kW/m3;利用居里点测试仪测得居里温度为257℃,汇总于表1。
表1
Figure BDA0002951186760000101
对比实施例1、实施例2、实施例3、实施例4和对比例1,可得到:添加了单质钽的钽掺杂锰锌铁氧体材料具有高频低损耗的特性,在100℃、3MHz、10mT的条件下,损耗为338~380kW/m3,远低于未添加单质钽的锰锌铁氧体材料(为480kW/m3)。
对比实施例1、实施例2、实施例3和实施例4,可得到:在氧化铁、氧化锰和氧化锌的质量比为(70~71):(21~22):(7~8),掺杂料包括五氧化二钒、五氧化二铌、氧化铋、氧化钴、氧化钼、五氧化二磷、碳酸钙和钽,尤其是包括钽,且钽的含量为100~350PPM时,钽掺杂锰锌铁氧体材料具有高频低损耗的特性。
上述的对实施例的描述是为便于该技术领域的普通技术人员能理解和使用发明。熟悉本领域技术的人员显然可以容易地对这些实施例做出各种修改,并把在此说明的一般原理应用到其他实施例中而不必经过创造性的劳动。因此,本发明不限于上述实施例,本领域技术人员根据本发明的揭示,不脱离本发明范畴所做出的改进和修改都应该在本发明的保护范围之内。

Claims (10)

1.一种高频低损耗的钽掺杂锰锌铁氧体材料,其特征在于,包括主料和掺杂料,所述主料包括氧化铁、氧化锰和氧化锌,所述氧化铁、氧化锰和氧化锌的质量比为(70~71):(21~22):(7~8),所述掺杂料包括第一副成分,所述第一副成分为单质钽。
2.根据权利要求1所述的一种高频低损耗的钽掺杂锰锌铁氧体材料,其特征在于,所述掺杂料中还包括第二副成分,所述第二副成分选自五氧化二钒、五氧化二铌、氧化铋、氧化钴、氧化钼、五氧化二磷或碳酸钙中的一种或多种混合。
3.根据权利要求1所述的一种高频低损耗的钽掺杂锰锌铁氧体材料,其特征在于,所述材料中,以材料原料的总质量为100wt%计,掺杂料的总量为100~2350PPM。
4.一种如权利要求1-3任一项所述的钽掺杂锰锌铁氧体材料的制备方法,其特征在于,所述制备方法具体包括以下步骤:
S1:将氧化铁、氧化锰和氧化锌加入球磨机进行球磨,得到混合料A;
S2:将混合料A进行预烧,然后冷却至室温得到预烧料B;
S3:将预烧料B和掺杂料加入球磨机进行二次球磨,之后烘干,得到混合料C;
S4:向混合料C中加入聚乙烯醇溶液混合进行喷雾造粒,然后过筛得到粉末颗粒;
S5:将粉末颗粒放入模具,进行压制成型,得到坯件;
S6:将坯件在平衡气氛下进行烧结,即得到所述钽掺杂锰锌铁氧体材料。
5.根据权利要求4所述的一种钽掺杂锰锌铁氧体材料的制备方法,其特征在于,步骤S1中,球磨机的转速为200~250r/min,球磨时间为2~7h。
6.根据权利要求4所述的一种钽掺杂锰锌铁氧体材料的制备方法,其特征在于,步骤S2中,在空气气氛下进行预烧,预烧温度为850~900℃,预烧时间为50~90min。
7.根据权利要求4所述的一种钽掺杂锰锌铁氧体材料的制备方法,其特征在于,步骤S3中,球磨机的转速为200~250r/min,球磨时间为6~8h,置于真空烘箱中进行烘干,烘干的温度为70~80℃,烘干的时间为20~24h。
8.根据权利要求4所述的一种钽掺杂锰锌铁氧体材料的制备方法,其特征在于,步骤S4中,造粒后过100~120目筛。
9.根据权利要求4所述的一种钽掺杂锰锌铁氧体材料的制备方法,其特征在于,步骤S5中,利用恒载荷压力机进行压制成型,恒载荷压力机施加的载荷为400~500MPa,保压340~380s。
10.根据权利要求4所述的一种钽掺杂锰锌铁氧体材料的制备方法,其特征在于,步骤S6中,烧结过程具体为:先在真空条件下以2℃/min的速度升温至400℃,再以5℃/min的速度升温至600℃,随后在高纯氮气氛下以3℃/min的速度升温至1200℃,之后充入空气调整至5%氧分压,以1℃/min的速度升温至1250~1315℃,保温4~6h,最后在平衡条件下以5℃/min的速度降温至室温,冷却过程中通高纯氮。
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