CN106810233A - 高频低损耗锰锌铁氧体及其制造方法 - Google Patents

高频低损耗锰锌铁氧体及其制造方法 Download PDF

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CN106810233A
CN106810233A CN201710037330.1A CN201710037330A CN106810233A CN 106810233 A CN106810233 A CN 106810233A CN 201710037330 A CN201710037330 A CN 201710037330A CN 106810233 A CN106810233 A CN 106810233A
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ferrite
high frequency
sintering
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尧巍华
宋秀鹏
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Dongguan E-Leo Electronics Co Ltd
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Abstract

本发明公开了一种高频低损耗锰锌铁氧体及其制造方法,其按摩尔比例称取主料,于球磨机中混合处理后,在850~980℃的烧结炉内烧结,并保温1~3小时,制得预烧料;进行二次球磨,向得到预烧料中加入辅料进行球磨处理形成粉料;添加第一添加剂及第二添加剂,采用机械进行造粒;在压机上将造粒后的粉料压制成型,将成型后的坯件放入到气氛烧结炉内进行二次烧结,制得高频低功耗锰锌铁氧体材料。本发明通过调整主料、辅料及添加剂的成分比例,利用微波烧结工艺获得一种在高频条件下也能够进行大功率传输的锰锌铁氧体材料,这种材料晶粒结构细小均匀,气孔少,具有高的晶界电阻率,从而使高频损耗大大降低,使变压器的高温稳定性大大提高。

Description

高频低损耗锰锌铁氧体及其制造方法
技术领域
本发明涉及一种软磁低功耗材料技术领域,尤其是涉及一种高频低损耗锰锌铁氧体及其制造方法。
背景技术
现代电子技术的发展趋势是为用户提供体积更小、更加节约能源的电子设备,为此,就需要体积更小、效率更高的开关电源。显著增加切换频率,是实现以上要求的一种可行方式,通过使用氮化镓GaN的电路,可获得所需高频。
2016年为GaN的爆发年,国际上众多大公司如EPC、TI、Navitas等都于近期推出基于GaN的功率驱动及控制芯片,随着新一代的电子开关管技术上的成熟,开关电源系统的频率也由几百kHz跃升至1MHz以上。在开关电源中,变压器占有很大一部分体积,同时也消耗了很大一部分能量。因此,降低变压器中使用的锰锌铁氧体材料的功率损耗就显得尤为重要。
为了制造高频低损耗材料,就必须对锰锌铁氧体的损耗机理进行分析和研究,并采取相应的掺杂和工艺。由文献可知,锰锌铁氧体的磁芯损耗可以分为三个主要部分:磁滞损耗Ph、涡流损耗Pe和剩余损耗Pr。这三种损耗在总损耗中各自所占的比例随着工作频率和磁通密度及温度的不同而差别很大,它们可以在一个很宽的范围内变化。在低频下,Ph占优势,因此,形成无点阵缺陷和无气孔的均匀晶粒结构以减小畴壁运动的阻力对减小Ph非常重要,同时也可以降低总损耗。在中频下,Pe所占的比例增大,要降低总损耗,可以通过增大材料电阻率的方法来抑制Pe的增大,此时可以使用CaO-SiO2复合掺杂在晶界形成高电阻层来抑制Pe的增大,但是,晶界层会增大畴壁运动的阻力,从而使Ph增大,因此必须综合考量工艺条件对Ph和Pe的不同影响。而对磁通密度比较低或高频(>1MHz)条件下剩余损耗Pr就会变得很重要,因此,此时只有设法降低Pr才能降低总损耗。
发明内容
基于此,有必要针对现有技术的不足,提供一种高频低损耗锰锌铁氧体及其制造方法,制造过程更加节能,同时所制得的铁氧体材料晶粒结构更加细小均匀,没有异常晶粒的长大,晶界电阻率高,降低了高频涡流损耗,晶粒内部无杂相,对磁畴转动及畴壁位移的阻滞小,减小了的磁滞损耗。
为解决上述技术问题,本发明所采用的技术方案是:一种高频低损耗锰锌铁氧体,包括主料、辅料、第一添加剂及第二添加剂,其中,主料包括53~59mol%的Fe2O3、5~10mol%的ZnO、31~42mol%的MnO,辅料包括0.1~1.5wt%的分散剂、0.5~3wt%的消泡剂、1~3wt%的粘合剂,第一添加剂包括30~80ppm的SiO2、500~3000ppm的CaCO3、200~2000ppm的TiO2及50~600ppm的V2O5,第二添加剂为50~300ppm Nb2O5、80~300ppm HfO2、50~300ppm ZrO2及50~300ppm Ta2O5中的一种或几种。
一种高频低损耗锰锌铁氧体的制造方法,其特征在于,包括如下步骤:
按摩尔比例称取主料,于球磨机中混合处理后,在850~980℃的烧结炉内烧结,并保温1~3小时,制得预烧料;
进行二次球磨,向得到预烧料中加入辅料进行球磨处理形成粉料;
添加第一添加剂及第二添加剂,采用机械进行造粒;
在压机上将造粒后的粉料压制成型,将成型后的坯件放入到气氛烧结炉内进行二次烧结,制得高频低功耗锰锌铁氧体材料。
在其中一个实施例中,所述气氛烧结炉为微波气氛烧结炉。
综上所述,本发明高频低损耗锰锌铁氧体及其制造方法通过调整主料、辅料及添加剂的成分比例,利用微波烧结工艺获得一种在高频条件下也能够进行大功率传输的锰锌铁氧体材料,这种材料晶粒结构细小均匀,气孔少,具有高的晶界电阻率,从而使高频损耗大大降低,使变压器的高温稳定性大大提高。
具体实施方式
为能进一步了解本发明的特征、技术手段以及所达到的具体目的、功能,下面结合具体实施方式对本发明作进一步详细描述。
本发明高频低损耗锰锌铁氧体包括主料、辅料、第一添加剂及第二添加剂,其中,主料包括53~59mol%的Fe2O3、5~10mol%的ZnO、31~42mol%的MnO,辅料包括0.1~1.5wt%的分散剂、0.5~3wt%的消泡剂、1~3wt%的粘合剂,第一添加剂包括30~80ppm的SiO2、500~3000ppm的CaCO3、200~2000ppm的TiO2及50~600ppm的V2O5,第二添加剂为50~300ppm Nb2O5、80~300ppm HfO2、50~300ppm ZrO2及50~300ppm Ta2O5中的一种或几种。
在其中一个实施例中,所述粘合剂为聚乙烯醇。
根据上述本发明高频低损耗锰锌铁氧体,本发明提供一种高频低损耗锰锌铁氧体的制造方法,该方法中涉及的高频低损耗锰锌铁氧体可以与上述高频低损耗锰锌铁氧体实施例阐述的技术特征相同,并能产生相同的技术效果。本发明高频低损耗锰锌铁氧体的制造方法通过调整主料、辅料及添加剂的成分比例,利用微波烧结工艺获得一种在高频条件下也能够进行大功率传输的锰锌铁氧体材料,这种材料晶粒结构细小均匀,气孔少,具有高的晶界电阻率,从而使高频损耗大大降低,使变压器的高温稳定性大大提高。
本发明高频低损耗锰锌铁氧体的制造方法,包括如下步骤:
按摩尔比例称取主料,于球磨机中混合处理后,在850~980℃的烧结炉内烧结,并保温1~3小时,制得预烧料;
进行二次球磨,向得到预烧料中加入辅料进行球磨处理形成粉料;
添加第一添加剂及第二添加剂,采用机械进行造粒;
在压机上将造粒后的粉料压制成型,将成型后的坯件放入到气氛烧结炉内进行二次烧结,制得高频低功耗锰锌铁氧体材料。
在其中一个实施例中,主料包括53~59mol%的Fe2O3、5~10mol%的ZnO、31~42mol%的MnO,辅料包括0.1~1.5wt%的分散剂、0.5~3wt%的消泡剂、1~3wt%的粘合剂,第一添加剂包括30~80ppm的SiO2、500~3000ppm的CaCO3、200~2000ppm的TiO2及50~600ppm的V2O5,第二添加剂为50~300ppm Nb2O5、80~300ppm HfO2、50~300ppm ZrO2及50~300ppm Ta2O5中的一种或几种。
在其中一个实施例中,所述粘合剂为聚乙烯醇。
在其中一个实施例中,所述二次烧结的烧结温度为1100~1280℃,烧结时间为0.5~2小时。
在其中一个实施例中,所述二次烧结采用二次还原烧结法,具体地,在还原气氛中升温至750~950℃,气氛烧结炉内氧含量为0.1%,以促进放氧,使得锰锌铁氧体材料提前生成并致密化;继续升温至1100~1280℃进行煅烧0.5~2小时,制得高频低功耗锰锌铁氧体材料。
在其中一个实施例中,所述气氛烧结炉为微波气氛烧结炉,相对于传统电加热气氛烧结炉具有更加节能的优点,同时所制得的铁氧体材料晶粒结构更加细小均匀,没有异常晶粒的长大,晶界电阻率高,降低了高频涡流损耗,晶粒内部无杂相,对磁畴转动及畴壁位移的阻滞小,减小了的磁滞损耗。
本发明采用本领域的常规的干法生产工艺制备高频低功耗锰锌铁氧体材料,同时使用微波气氛烧结炉进行烧结,制备方法过程简单,相比传统电加热气氛烧结方法能耗更低;这种高频低功耗锰锌铁氧体材料具有在1~3MHz的开关电源系统内传输功率高、功率损失小、温度稳定性及可靠性高等优点,可以应用于使用频率在1MHz以上的开关电源系统中的变压器和电感器等领域
实施例一
主料中使用Fe2O3(宝钢铁红)54mol%、ZnO(京华锌)6mol%、MnO(湖南金瑞锰,折算为Mn3O4)40mol%,于球磨机中混合时间30分钟,在900℃的烧结炉内保温时间2小时;添加辅料分散剂0.5wt%、消泡剂1wt%及聚乙烯醇粘合剂2wt%后二次球磨时间1小时制得粉料;添加微量添加剂50ppm SiO2、3000ppm CaCO3、150ppm Nb2O5、1000ppm TiO2、350ppm V2O5、150ppm ZrO2、80ppm HfO2,喷雾造粒,利用压机将造粒后的粉料压制成坯件放到微波气氛烧结炉进行二次烧结,制得高频低功耗锰锌铁氧体材料,其中,二次烧结的烧结温度为1150℃,在3%的氧分压下保温烧结1小时,降温时,微波气氛烧结炉内降温温度与氧分压按照Blank公式计算来调节气氛。
所得的高频低功耗锰锌铁氧体材料的性能参数如下:
实施例二
主料使用Fe2O3(宝钢铁红)56mol%、ZnO(京华锌)5mol%、MnO(湖南金瑞锰,折算为Mn3O4)39mol%,于球磨机中混合时间30分钟,在910℃的烧结炉内保温时间2小时;添加辅料分散剂0.5wt%、消泡剂1wt%及聚乙烯醇粘合剂2wt%后二次球磨时间1小时制得粉料;添加微量添加剂50ppm SiO2、2500ppm CaCO3、150ppm Nb2O5、500ppm TiO2、300ppm V2O5、150ppm ZrO2、100ppm Ta2O5,喷雾造粒,利用压机将造粒后的粉料压制成坯件放到微波气氛烧结炉进行二次烧结,制得高频低功耗锰锌铁氧体材料,其中,二次烧结的烧结温度为1160℃,在3%的氧分压下保温烧结1小时,降温时,微波气氛烧结炉内降温温度与氧分压按照Blank公式计算来调节气氛。
所得的锰锌功率铁氧体材料的性能参数如下:
实施例三
主料使用Fe2O3(宝钢铁红)57mol%、ZnO(京华锌)6mol%、MnO(湖南金瑞锰,折算为Mn3O4)37mol%,于球磨机中混合时间30分钟,在920℃的烧结炉内保温时间2小时;添加辅料分散剂0.5wt%、消泡剂1wt%及聚乙烯醇粘合剂2wt%后二次球磨时间1小时制得粉料;添加微量添加剂50ppm SiO2、2000ppm CaCO3、250ppm Nb2O5、500ppm TiO2、300ppm V2O5、200ppm ZrO2、120ppm Ta2O5,喷雾造粒,利用压机将造粒后的粉料压制成坯件放到微波气氛烧结炉进行二次烧结,制得高频低功耗锰锌铁氧体材料,其中,二次烧结的烧结温度为1170℃,在3%的氧分压下保温烧结1小时,降温时,微波气氛烧结炉内降温温度与氧分压按照Blank公式计算来调节气氛。
所得的锰锌功率铁氧体材料的性能参数如下:
实施例四
主料使用Fe2O3(宝钢铁红)58mol%、ZnO(京华锌)6mol%、MnO(湖南金瑞锰,折算为Mn3O4)36mol%,于球磨机中混合时间30分钟,在950℃的烧结炉内保温时间2小时;添加辅料分散剂0.5wt%、消泡剂1wt%及聚乙烯醇粘合剂2wt%后二次球磨时间1小时制得粉料;添加的微量添加剂为50ppm SiO2、2000ppm CaCO3、200ppm Nb2O5、500ppm TiO2、300ppm V2O5、150ppm ZrO2、200ppm Ta2O5,喷雾造粒,利用压机将造粒后的粉料压制成坯件放到微波气氛烧结炉进行二次烧结,制得高频低功耗锰锌铁氧体材料,其中,二次烧结的烧结温度为1170℃,在3%的氧分压下保温烧结1小时,降温时,微波气氛烧结炉内降温温度与氧分压按照Blank公式计算来调节气氛。
所得的锰锌功率铁氧体材料的性能参数如下:
综上所述,本发明高频低损耗锰锌铁氧体及其制造方法通过调整主料、辅料及添加剂的成分比例,利用微波烧结工艺获得一种在高频条件下也能够进行大功率传输的锰锌铁氧体材料,这种材料晶粒结构细小均匀,气孔少,具有高的晶界电阻率,从而使高频损耗大大降低,使变压器的高温稳定性大大提高。
以上所述实施例仅表达了本发明的几种实施方式,其描述较为具体和详细,但并不能因此而理解为对本发明范围的限制。应当指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。因此,本发明的保护范围应以所附权利要求为准。

Claims (9)

1.一种高频低损耗锰锌铁氧体,其特征在于:包括主料、辅料、第一添加剂及第二添加剂,其中,主料包括53~59mol%的Fe2O3、5~10mol%的ZnO、31~42mol%的MnO,辅料包括0.1~1.5wt%的分散剂、0.5~3wt%的消泡剂、1~3wt%的粘合剂,第一添加剂包括30~80ppm的SiO2、500~3000ppm的CaCO3、200~2000ppm的TiO2及50~600ppm的V2O5,第二添加剂为50~300ppm Nb2O5、80~300ppm HfO2、50~300ppm ZrO2及50~300ppm Ta2O5中的一种或几种。
2.根据权利要求1所述的高频低损耗锰锌铁氧体,其特征在于:所述粘合剂为聚乙烯醇。
3.一种高频低损耗锰锌铁氧体的制造方法,其特征在于,包括如下步骤:
按摩尔比例称取主料,于球磨机中混合处理后,在850~980℃的烧结炉内烧结,并保温1~3小时,制得预烧料;
进行二次球磨,向得到预烧料中加入辅料进行球磨处理形成粉料;
添加第一添加剂及第二添加剂,采用机械进行造粒;
在压机上将造粒后的粉料压制成型,将成型后的坯件放入到气氛烧结炉内进行二次烧结,制得高频低功耗锰锌铁氧体材料。
4.一种如权利要求3所述的高频低损耗锰锌铁氧体的制造方法,其特征在于:所述二次烧结的烧结温度为1100~1280℃,烧结时间为0.5~2小时。
5.一种如权利要求3所述的高频低损耗锰锌铁氧体的制造方法,其特征在于:所述气氛烧结炉为微波气氛烧结炉。
6.一种如权利要求3所述的高频低损耗锰锌铁氧体的制造方法,其特征在于:所述二次烧结采用二次还原烧结法。
7.一种如权利要求3所述的高频低损耗锰锌铁氧体的制造方法,其特征在于:所述二次还原烧结法为在还原气氛中升温至750~950℃,气氛烧结炉内氧含量为0.1%;继续升温至1100~1280℃进行煅烧0.5~2小时,制得高频低功耗锰锌铁氧体材料。
8.一种如权利要求3所述的高频低损耗锰锌铁氧体的制造方法,其特征在于:所述主料包括53~59mol%的Fe2O3、5~10mol%的ZnO、31~42mol%的MnO,辅料包括0.1~1.5wt%的分散剂、0.5~3wt%的消泡剂、1~3wt%的粘合剂,第一添加剂包括30~80ppm的SiO2、500~3000ppm的CaCO3、200~2000ppm的TiO2及50~600ppm的V2O5,第二添加剂为50~300ppmNb2O5、80~300ppm HfO2、50~300ppm ZrO2及50~300ppm Ta2O5中的一种或几种。
9.一种如权利要求8所述的高频低损耗锰锌铁氧体的制造方法,其特征在于:所述粘合剂为聚乙烯醇。
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CN115385677B (zh) * 2022-09-02 2023-05-30 上海华源磁业股份有限公司 一种宽温低功耗锰锌铁氧体pf-2t材料及其制备工艺
CN115385677A (zh) * 2022-09-02 2022-11-25 上海华源磁业股份有限公司 一种宽温低功耗锰锌铁氧体pf-2t材料及其制备工艺
CN115724656A (zh) * 2022-11-14 2023-03-03 陕西煤业化工技术研究院有限责任公司 一种锰锌功率铁氧体材料及其制备方法、开关电源变压器
CN115724656B (zh) * 2022-11-14 2023-10-20 陕西煤业化工技术研究院有限责任公司 一种锰锌功率铁氧体材料及其制备方法、开关电源变压器

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Application publication date: 20170609