CN108395233A - 大功率低功耗高频变压器用锰锌铁氧体材料及制备方法 - Google Patents

大功率低功耗高频变压器用锰锌铁氧体材料及制备方法 Download PDF

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CN108395233A
CN108395233A CN201810250372.8A CN201810250372A CN108395233A CN 108395233 A CN108395233 A CN 108395233A CN 201810250372 A CN201810250372 A CN 201810250372A CN 108395233 A CN108395233 A CN 108395233A
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ferrite material
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刘运
戴加兵
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NANTONG GUANYOUDA MAGNET Co Ltd
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Abstract

本发明属软磁铁氧体材料技术领域，所述锰锌铁氧体材料由主成分和添加剂组成，所述主成分按物质的质量百分比，以氧化物计算：Fe203为70～72.5%，Zn0为4.5～5.5%，NiO为1.5～3.5%，Sm2O3为1～2%，余量为Mn304；有益效果：3500±25%的起始磁导率，且在25～140℃温度区域内谷点功率损耗达270kw/m­ 3，TC大于270℃，在500KHZ、50mT、100℃测试条件下功耗损耗小于280kw/m3，在1MHZ，30mT，100℃测试条件功耗损耗小于480kw/m3。

Description

大功率低功耗高频变压器用锰锌铁氧体材料及制备方法
技术领域
本发明属于铁氧体电子材料技术领域，具体涉及一种大功率低功耗高频变压器用锰锌铁氧体材料。
背景技术
随着电子信息产业的不断迅速发展，作为目前产量最大，应用最广泛的软磁铁氧体材料，已广泛应用于各种电子元器件中。世界各大铁氧体公司竞相提高锰锌铁氧体材料技术性能，以适应不用的应用领域，在变频空调、无极灯照明电子、电力电子、IT产业、通讯、家用电子等用户的要求下，一种要求材料具有更高的BS，更好的直流叠加特性，更低的功率损耗，更宽的使用频率和更宽的温度适应范围、更高的居里温度，因此，锰锌铁氧体材料的研究已进入到了宽温、高直流叠加、高BS、更低的功率损耗领域、更高居里温度领域。分析市场上各材料制造厂家所推出的材料，不难看出各材料厂家都在寻求一种宽温、低损耗材料、高居里温度以取代众多的高频低功耗铁氧体材料。
大型的高频变压器的广泛使用及性能提高，促进了该材料的不断开发与投产，在低频200～300KHZ中低频率状态下广泛使用。但是存在如何兼顾内置和外置两种结构下使用变压器效率达到最佳，同时要求在-40℃下具有足够的磁导率，同时要求发热要小，损耗低；另一方面电子产品在工作中总有电流成分，为防止电子产品不因有电流的存在而影响正常使用，因此还需要材料有足够的BS、直流叠加特性；同时在特定的环境下如环境温度达到280℃或更高时电子器件还能正常工作的。
作为使用最广泛的电源变压器、办公自动化、家用电子、通信等要求具有宽温、低损耗、高磁导率、高直流叠加是不可缺少的组件，
如中国专利申请（CN101183582A）公开的一种高饱和BS低损耗的锰锌功率铁氧体材料，它通过优化配方和掺杂，特别是加入2～4mol%Ni0得到BS（100度下大于460T）高频功耗500KHZ、50mT、100度下小于150KW/m3、但没有提及宽温宽频和居里点高低，因而其应用范围有限。
另外在中国专利申请（CN1749209A）公开了一种高饱和磁通密度、低损耗锰锌铁氧体材料及其制备方法，它通过掺杂和工艺控制，得到了100KHZ、200mT、45℃时低于245kw/m3的功耗和1194A/m、50mT、25℃时饱和磁通密度高于535mT的结果，但同样没有提及宽温和宽频、居里温度，因而其使用范围相当有限。
发明内容
本发明要达到的目的是要提供一种具有高的起始磁导率、且在25～140℃功耗相当，在25～180℃温度范围内功耗曲线平坦，剩磁小，叠加特性好、同时在高频500KHZ、50mT、100℃测试条件下功耗损耗小于250kw/m3， 在1MHZ，30mT，100℃测试条件功耗损耗小于400kw/m3，居里温度达到270℃以上的高频宽温高叠加低损耗高居里温度的软磁铁氧体材料。
本发明所采用的技术方案是。
大功率低功耗高频变压器用锰锌铁氧体材料，所述锰锌铁氧体材料由主成分和添加剂组成，所述主成分按物质的质量百分比，以氧化物计算：Fe203为70～72.5%，Zn0为4.5～5.5%，NiO为1.5～3.5%，Sm2O3为1～2%，余量为Mn304。
所述添加剂按质量百分比以氧化物计算：Ca0：0.025～0.075%、Nb205：0.02～0.08%、V205：0.015～0.08%、Ti02：0.05～0.3%、C0203：0.09～0.65%、Zr02：0.003～0.15%、Ni0：0.04～0.45% 、Mg0：0.02～0.15%、Li2O:0.04～0.068%。
大功率低功耗高频变压器用锰锌铁氧体材料的制备方法如下。
步骤一、将所述主成分按物质的质量百分比Fe203为73.5～75%，Zn0为5～8.5%，Sm2O3为9～11.5%，余量为Mn304用星形球磨机混合均匀。
步骤二、将所述步骤1）所得的粉料在950～1325℃下进行预烧；保温时间为4～5.5小时。
步骤三、将所述步骤2）所得的粉料按质量比加入含有Ca0：0.025～0.075%、Nb205：0.02～0.08%、V205：0.015～0.08%、Ti02：0.05～0.3%、C0203：0.09～0.65%、Zr02：0.003～0.15%、Ni0：0.04～0.45% 、Mg0：0.02～0.15%、Li2O:0.04～0.068%的添加剂，并进行第二次星形球磨，球磨后的粉料平均匀粒径达到0.8～0.9微米。
步骤四、将所述步骤三所得的二次星形球磨料烘干后造粒、成型，制成标准生坯样品。
步骤五、将所述步骤四所得的生坏样品铜水炉中进行高温烧结处理。
步骤六、将所述步骤五所得的坯料在高温烧结炉中二次煅烧去铜。
所述步骤四为：将所述步骤三所得的粉料按质量比加入8～10%的PVA有机粘合剂，并混合均匀，造粒后，在试验室16吨压机上将粉料压制成样品坯件，所述步骤五为：将所述步骤四所得的生坏样品铜水炉中进行高温烧结处理，在升温段1100～1250℃进行致密化，在1330～1355℃保温4～6个小时。
利用本发明制得的磁芯具有如下有益效果。
利用铜水的保护烧结；添加了含有Sm2O3的主料和含有Li2O的添加剂。使得磁芯产品拥有3500±25%的起始磁导率；在25～140℃温度区域内谷点功率损耗达270kw/m3，TC大于270℃，在500KHZ、50mT、100℃测试条件下功耗损耗小于280kw/m3， 在1MHZ，30mT，100℃测试条件功耗损耗小于480kw/m3。
具体实施方式
以下结合实施例对本发明作进一步说明。
例一、大功率低功耗高频变压器用锰锌铁氧体材料，所述锰锌铁氧体材料由主成分和添加剂组成，所述主成分按物质的质量百分比，以氧化物计算：Fe203为70%，Zn0为4.5%，NiO为3.5%，Sm2O3为1%，余量为Mn304。
所述添加剂按质量百分比以氧化物计算：Ca0：0.025～0.075%、Nb205：0.02～0.08%、V205：0.015～0.08%、Ti02：0.05～0.3%、C0203：0.09～0.65%、Zr02：0.003～0.15%、Ni0：0.04～0.45% 、Mg0：0.02～0.15%、Li2O:0.04～0.068%。
大功率低功耗高频变压器用锰锌铁氧体材料的制备方法，包括以下步骤。
步骤一、将所述主成分按物质的质量百分比Fe203为73.5%，Zn0为5%，Sm2O3为11.5%，余量为Mn30用星形球磨机混合均匀。
步骤二、将所述步骤1）所得的粉料在950～1325℃下进行预烧；保温时间为4小时。
步骤三、将所述步骤2）所得的粉料按质量比加入含有Ca0：0.025～0.075%、Nb205：0.02～0.08%、V205：0.015～0.08%、Ti02：0.05～0.3%、C0203：0.09～0.65%、Zr02：0.003～0.15%、Ni0：0.04～0.45% 、Mg0：0.02～0.15%、Li2O:0.04～0.068%的添加剂，并进行第二次星形球磨，球磨后的粉料平均匀粒径达到0.8～0.9微米。
步骤四、将所述步骤三所得的二次星形球磨料烘干后造粒、成型，制成标准生坯样品。
步骤五、将所述步骤四所得的生坏样品铜水炉中进行高温烧结处理。
步骤六、将所述步骤五所得的坯料在高温烧结炉中二次煅烧去铜。
在大功率低功耗高频变压器用锰锌铁氧体材料的制备方法中，所述步骤四为：将所述步骤三所得的粉料按质量比加入8～10%的PVA有机粘合剂，并混合均匀，造粒后，在试验室16吨压机上将粉料压制成样品坯件，所述步骤五为：将所述步骤四所得的生坏样品铜水炉中进行高温烧结处理，在升温段1100～1250℃进行致密化，在1330～1355℃保温4个小时。
例二、大功率低功耗高频变压器用锰锌铁氧体材料，其特征在于，所述锰锌铁氧体材料由主成分和添加剂组成，所述主成分按物质的质量百分比，以氧化物计算：Fe203为72.5%，Zn0为5.5%，NiO为1.5%，Sm2O3为2%，余量为Mn304。
所述添加剂按质量百分比以氧化物计算：Ca0：0.025～0.075%、Nb205：0.02～0.08%、V205：0.015～0.08%、Ti02：0.05～0.3%、C0203：0.09～0.65%、Zr02：0.003～0.15%、Ni0：0.04～0.45% 、Mg0：0.02～0.15%、Li2O:0.04～0.068%。
大功率低功耗高频变压器用锰锌铁氧体材料的制备方法，包括以下步骤。
步骤一、将所述主成分按物质的质量百分比Fe203为73.5%，Zn0为5%，Sm2O3为11.5%，余量为Mn304用星形球磨机混合均匀。
步骤二、将所述步骤1）所得的粉料在950～1325℃下进行预烧；保温时间为5.5小时。
步骤三、将所述步骤2）所得的粉料按质量比加入含有Ca0：0.025～0.075%、Nb205：0.02～0.08%、V205：0.015～0.08%、Ti02：0.05～0.3%、C0203：0.09～0.65%、Zr02：0.003～0.15%、Ni0：0.04～0.45% 、Mg0：0.02～0.15%、Li2O:0.04～0.068%的添加剂，并进行第二次星形球磨，球磨后的粉料平均匀粒径达到0.8～0.9微米。
步骤四、将所述步骤三所得的二次星形球磨料烘干后造粒、成型，制成标准生坯样品。
步骤五、将所述步骤四所得的生坏样品铜水炉中进行高温烧结处理。
步骤六、将所述步骤五所得的坯料在高温烧结炉中二次煅烧去铜。
在大功率低功耗高频变压器用锰锌铁氧体材料的制备方法中，所述步骤四为：将所述步骤三所得的粉料按质量比加入8～10%的PVA有机粘合剂，并混合均匀，造粒后，在试验室16吨压机上将粉料压制成样品坯件，所述步骤五为：将所述步骤四所得的生坏样品铜水炉中进行高温烧结处理，在升温段1100～1250℃进行致密化，在1330～1355℃保温6个小时。
例三、大功率低功耗高频变压器用锰锌铁氧体材料，其特征在于，所述锰锌铁氧体材料由主成分和添加剂组成，所述主成分按物质的质量百分比，以氧化物计算Fe203为71%，Zn0为5%，NiO为3%，Sm2O3为1.5%，余量为Mn304。
所述添加剂按质量百分比以氧化物计算：Ca0：0.025～0.075%、Nb205：0.02～0.08%、V205：0.015～0.08%、Ti02：0.05～0.3%、C0203：0.09～0.65%、Zr02：0.003～0.15%、Ni0：0.04～0.45% 、Mg0：0.02～0.15%、Li2O:0.04～0.068%。
大功率低功耗高频变压器用锰锌铁氧体材料的制备方法，包括以下步骤。
步骤一、将所述主成分按物质的质量百分比Fe203为74.5%，Zn0为7.5%，Sm2O3为10.5%，余量为Mn304用星形球磨机混合均匀。
步骤二、将所述步骤1）所得的粉料在950～1325℃下进行预烧；保温时间为5小时。
步骤三、将所述步骤2）所得的粉料按质量比加入含有Ca0：0.025～0.075%、Nb205：0.02～0.08%、V205：0.015～0.08%、Ti02：0.05～0.3%、C0203：0.09～0.65%、Zr02：0.003～0.15%、Ni0：0.04～0.45% 、Mg0：0.02～0.15%、Li2O:0.04～0.068%的添加剂，并进行第二次星形球磨，球磨后的粉料平均匀粒径达到0.8～0.9微米。
步骤四、将所述步骤三所得的二次星形球磨料烘干后造粒、成型，制成标准生坯样品。
步骤五、将所述步骤四所得的生坏样品铜水炉中进行高温烧结处理。
步骤六、将所述步骤五所得的坯料在高温烧结炉中二次煅烧去铜。
在大功率低功耗高频变压器用锰锌铁氧体材料的制备方法中，所述步骤四为：将所述步骤三所得的粉料按质量比加入8～10%的PVA有机粘合剂，并混合均匀，造粒后，在试验室16吨压机上将粉料压制成样品坯件，所述步骤五为：将所述步骤四所得的生坏样品铜水炉中进行高温烧结处理，在升温段1100～1250℃进行致密化，在1330～1355℃保温5个小时。
表1 本发明磁芯材料性能。
表2 本发明以EC4445为例的叠加特性
由表1和表2可见，本发明的锰锌系铁氧体材料通过对主成分及副成分进行调整，具体为Sm2O3、Li2O联合补偿作用的加强，宽温特性明显；掺杂体系如Ni0加入使用TC的提高，机械强度得到改善，同时气氛控制及致密化工艺使用该材料具有较高的起始磁导率，在25～180℃温度区域内的功耗比较平坦，100℃功耗小于270 mw/cm3，高频功耗较低，直流叠加优良，居里温度大于270℃ 。

Claims (3)

1.大功率低功耗高频变压器用锰锌铁氧体材料，其特征在于，所述锰锌铁氧体材料由主成分和添加剂组成，所述主成分按物质的质量百分比，以氧化物计算：Fe203为70～72.5%，Zn0为4.5～5.5%，NiO为1.5～3.5%，Sm2O3为1～2%，余量为Mn304；
所述添加剂按质量百分比以氧化物计算：Ca0：0.025～0.075%、Nb205：0.02～0.08%、V205：0.015～0.08%、Ti02：0.05～0.3%、C0203：0.09～0.65%、Zr02：0.003～0.15%、Ni0：0.04～0.45% 、Mg0：0.02～0.15%、Li2O:0.04～0.068%。
2.大功率低功耗高频变压器用锰锌铁氧体材料的制备方法，包括以下步骤：
步骤一、将所述主成分按物质的质量百分比Fe203为73.5～75%，Zn0为5～8.5%，Sm2O3为9～11.5%，余量为Mn304用星形球磨机混合均匀；
步骤二、将所述步骤1）所得的粉料在950～1325℃下进行预烧；保温时间为4～5.5小时；
步骤三、将所述步骤2）所得的粉料按质量比加入含有Ca0：0.025～0.075%、Nb205：0.02～0.08%、V205：0.015～0.08%、Ti02：0.05～0.3%、C0203：0.09～0.65%、Zr02：0.003～0.15%、Ni0：0.04～0.45% 、Mg0：0.02～0.15%、Li2O:0.04～0.068%的添加剂，并进行第二次星形球磨，球磨后的粉料平均匀粒径达到0.8～0.9微米；
步骤四、将所述步骤三所得的二次星形球磨料烘干后造粒、成型，制成标准生坯样品；
步骤五、将所述步骤四所得的生坏样品铜水炉中进行高温烧结处理；
步骤六、将所述步骤五所得的坯料在高温烧结炉中二次煅烧去铜。
3.如权利要求2所述的大功率低功耗高频变压器用锰锌铁氧体材料的制备方法，其特征在于，所述步骤四为：将所述步骤三所得的粉料按质量比加入8～10%的PVA有机粘合剂，并混合均匀，造粒后，在试验室16吨压机上将粉料压制成样品坯件，所述步骤五为：将所述步骤四所得的生坏样品铜水炉中进行高温烧结处理，在升温段1100～1250℃进行致密化，在1330～1355℃保温4～6个小时。
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Application publication date: 20180814