CN110078488B - 一种高Bs宽温低损耗软磁铁氧体材料及其制备方法 - Google Patents

一种高Bs宽温低损耗软磁铁氧体材料及其制备方法 Download PDF

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CN110078488B
CN110078488B CN201910393242.4A CN201910393242A CN110078488B CN 110078488 B CN110078488 B CN 110078488B CN 201910393242 A CN201910393242 A CN 201910393242A CN 110078488 B CN110078488 B CN 110078488B
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temperature
ferrite material
wide
soft magnetic
powder
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CN110078488A (zh
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李永劬
王微达
郭凤鸣
严建强
李明治
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Haining Lianfeng Magnet Industry Co ltd
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Abstract

本发明公开了一种高Bs宽温低损耗软磁铁氧体材料及其制备方法，铁氧体材料，包括主成分、第一辅助成分、第二辅助成本，其中，主成分包括含量为53.4～54.5mol％的Fe2O3、含量为7.5～9.4mol％为ZnO、含量为0.3～0.8mol％的NiO，其余为MnO；第一辅助成份包括CaCO3、SiO2、Co2O3，第二辅助成份包括Nb2O5、ZrO2、Ta2O5、V2O5、CeO2、HfO2中的一种以上，或者采用TiO2和SnO2中的一种或者两种。本发明的主成份中氧化锌的含量相对较高点，NiO含量相对较低点，容易实现宽温低损耗，并结合制造方法特别是烧结工艺来提高铁氧体材料的密度从而进一步提高高温100度的饱和磁通密度。

Description

一种高Bs宽温低损耗软磁铁氧体材料及其制备方法
技术领域
本发明属于氧化物法制备磁性材料领域，具体涉及软磁铁氧体材料及其制备方法。
背景技术
随着个人用小轿车的快速发展，人类对汽车的性能和环保提出了更高的要求。传统的机械装置已经无法满足人们对汽车功能不断提高的要求，现代电子控制技术正被极大地应用于汽车的各个方面，从而带来对软磁铁氧体的新应用和新要求，因为汽车行驶时会有较大的温度变化，并不是工作在一个较小的温度区间，这就迫切需要一种在宽广温度范围内都保持低损耗的软磁铁氧体材料。
为了满足这种需求，TDK在2003年率先推出了宽温低损耗材料—PC95，揭开了宽温应用领域节能时代的序幕，紧跟其后，FDK公司也于2004年12月推出了宽温低损耗材料—6H60。国内外都掀起了研究宽温低损耗材料的热潮。
80PLUS计划是由美国能源署出台，Ecos Consulting负责执行的一项全国性节能现金奖励方案，起初在美国，现已推广到多数国家，为降低能耗，鼓励系统商在生产台式机或服务器时选配使用100％负载、50％负载、20％负载效率均在80％以上,为了满足20％、50％、100％负载的效率都很高，其中的电源部份需使用宽温低损耗软磁铁氧体材料。并且还推广到家电、照明领域。
发明内容
本发明所要解决的技术问题就是提供一种具有更高Bs以及更低损耗的高Bs宽温低损耗软磁铁氧体材料及制备方法。
为解决上述技术问题，本发明采用如下技术方案：一种高Bs宽温低损耗软磁铁氧体材料，包括主成分、第一辅助成分、第二辅助成本，其中，主成分包括含量为53.4～54.5mol％的Fe2O3、含量为7.5～9.4mol％为ZnO、含量为0.3～0.8mol％的NiO，其余为MnO；第一辅助成份包括CaCO3、SiO2、Co2O3，第二辅助成份包括Nb2O5、ZrO2、Ta2O5、V2O5、CeO2、HfO2中的一种以上，或者采用TiO2和SnO2中的一种或者两种，辅助成份的添加量如下：
CaCO3：100～1000ppm，
SiO2：10～100ppm，
Co2O3：2500～4500ppm，
Nb2O5：20～500ppm，
ZrO2：20～500ppm，
Ta2O5：50～500ppm，
V2O5：50～800ppm，
CeO2：50～400ppm，
HfO2：50～400ppm，
TiO2：0～2000ppm，
SnO2：0～3000ppm。
本发明还提供了一种高Bs宽温低损耗软磁铁氧体材料制备方法，采用上述的铁氧体材料作为原料进行制备，包括如下步骤：
(1)原料混合：根据四种主成分原料的配比进行配料后，放入球磨机或砂磨机中，并加入纯水，使四种原料进行充分的混合；
(2)烘干：将混合均匀的料浆泵入烘干设备中烘干；
(3)预烧：将烘干的粉料放入预烧设备中预烧，预烧温度为800～1000℃，预烧保温时间为30～180分钟；
(4)粉碎：将预烧后的粉料在振磨机中先初步粉碎成平均粒度≤5μm的小颗粒粉末，再加入辅助成份的组合，再加入纯水进行细粉碎，细粉碎后的粉料平均粒度控制在0.7～1.3μm之间；
(5)喷雾造粒：将细粉碎后的浆料在喷雾塔中进行喷雾造粒，喷雾造粒出的粉料松装比重控制在1.25～1.50g/cm3；
(6)成型：将喷雾造粒的粉料使用成型机压制成毛坯；
(7)烧结：将成型好的毛坯放在真空气氛炉中烧结，，开始升温阶段炉内压力为常压状态，在升温到700℃～(保温温度-X)℃的全程或部分温度内进行抽真空，X＝0～160，真空度控制在小于3×103Pa，当升温到(保温温度-X)℃时，停止抽真空，并充入适当比例的氮氧混合气，使炉压上升并保持在正压，范围为(1大气压+500Pa)～(1大气压+3000Pa)。
可选的，步骤(1)中原料与纯水的重量比为1.0：0.7～1.5，纯水的电导率小于20μs/cm。
可选的，步骤(6)中成型后毛坯密度控制为2.9～3.1g/cm3。
可选的，步骤(7)中保温温度为1220～1290℃，保温时间为180～360分钟。
本发明采用上述技术方案，具有如下有益效果：
1、现有技术中高Bs宽温低损耗软磁铁氧体材料,提高高温Bs的一种方法是依靠在组分中采用较高氧化铁含量、较低氧化锌含量的方法，例如组分中氧化铁含量为53.5-54.5mol％,氧化锌含量为小于7.5mol％；另一种方法是添加NiO,NiO添加量大于1mol％，一般在1mol％-5mol％。本发明的主成份中氧化锌的含量相对较高点，NiO含量相对较低点，容易实现宽温低损耗，并结合制造方法特别是烧结工艺来提高铁氧体材料的密度从而进一步提高高温100度的饱和磁通密度。
饱和磁通密度可由下列经验公式(1)给出：
Figure GDA0002108035210000041
式中，Bs(T)为测定温度下材料的饱和磁通密度；Bs(0)为绝对零度下材料的饱和磁通密度；ρ为材料的实际烧结密度；ρ1为材料的理论密度；T为测定温度；Tc材料的居里温度；r为常数。从式(1)可知：饱和磁通密度是温度的函数关系，要提高高温下的饱和磁通密度，选择适合的组分是必要的，而提高材料的最终密度也是一个重要方法。
在锰锌铁氧体烧结工艺上提高材料最终密度的方法常用的有两种，一种是提高烧结的最高温度来提高锰锌铁氧体材料最终密度；另一种是在升温过程中通入氮气或低氧含量的氮氧混合气。本发明是在升温过程中进行抽真空来尽快抽走锰锌铁氧体反应中的一些废气(主要是Fe2O3原料中含有微量的S、Cl)和空气，从而减少锰锌铁氧体中的气孔、提高锰锌铁氧体材料最终密度。
2、两种辅助成分的添加主要是降低宽温范围内损耗的，Co2O3主要作用是补偿磁晶各向异性常数K1的温度曲线，从而实现在较宽的温度范围内损耗较低。第二辅助成分中各成分效果近似，都可达到类似的低损耗效果。
本发明的具体技术方案及其有益效果将会在下面的具体实施方式中进行详细的说明。
具体实施方式
本发明提供一种高Bs宽温低损耗软磁铁氧体材料，包括主成分、第一辅助成分、第二辅助成本，其中，主成分包括含量为53.4～54.5mol％的Fe2O3、含量为7.5～9.4mol％为ZnO、含量为0.3～0.8mol％的NiO，其余为MnO；第一辅助成份包括CaCO3、SiO2、Co2O3，第二辅助成份包括Nb2O5、ZrO2、Ta2O5、V2O5、CeO2、HfO2中的一种以上，或者采用TiO2和SnO2中的一种或者两种，辅助成份的添加量如下(以粉料总重量为参照)：
CaCO3：100～1000ppm，
SiO2：10～100ppm，
Co2O3：2500～4500ppm
Nb2O5：20～500ppm，
ZrO2：20～500ppm，
Ta2O5：50～500ppm，
V2O5：50～800ppm，
CeO2：50～400ppm，
HfO2：50～400ppm，
TiO2：0～2000ppm。
SnO2：0～3000ppm。
另外，一种高Bs宽温低损耗软磁铁氧体材料制备方法，包括如下步骤：
(1)原料混合：根据四种主成分原料的配比进行配料后，放入球磨机或砂磨机中，并加入纯水，使四种原料进行充分的混合；
(2)烘干：将混合均匀的料浆泵入烘干设备中烘干；
(3)预烧：将烘干的粉料放入预烧设备中预烧，预烧温度为800～1000℃，预烧保温时间为30～180分钟；
(4)粉碎：将预烧后的粉料在振磨机中先初步粉碎成平均粒度≤5μm的小颗粒粉末，再加入辅助成份的组合，再加入纯水进行细粉碎，细粉碎后的粉料平均粒度控制在0.7～1.3μm之间；
(5)喷雾造粒：将细粉碎后的浆料在喷雾塔中进行喷雾造粒，喷雾造粒出的粉料松装比重控制在1.25～1.50g/cm3；
(6)成型：将喷雾造粒的粉料使用成型机压制成毛坯；
(7)烧结：将成型好的毛坯放在真空气氛炉中烧结，开始升温阶段炉内压力为常压状态，在升温到700℃～(保温温度-X)℃的全程或部分温度内进行抽真空，X＝0～160，真空度控制在小于3×103Pa，当升温到(保温温度-X)℃时，停止抽真空，并充入适当比例的氮氧混合气，使炉压上升并保持在正压，范围为(1大气压+500Pa)～(1大气压+3000Pa)。
为了更好地说明本发明中在高温下超低损耗并具有更高Bs的软磁铁氧体材料及其制备方法，下面将提供具体实施例，但本发明并不限于这些实施例。
实施例1～5：
一种高Bs宽温低损耗软磁铁氧体材料的制备方法，其具体步骤如下：
(1)原料混合：按照主配方中的配比，精确称量Fe2O3的含量为53.4～54.5mol％，ZnO的含量为7.5～9.4mol％，NiO的含量为0.3～0.8mol％，其余为MnO，并加入纯水，纯水的电导率小于2us/cm，纯水的电导率过大会引入有害杂质导致损耗上升；原料与纯水的重量比为1.0：1.0，使用砂磨机进行砂磨40±2分钟，使四种原材料进行充分的混合。
(2)烘干：将混合均匀的料浆泵入喷雾干燥机中烘干并造粒。
(3)预烧：将烘干的粉料放入预烧设备中预烧，预烧温度为880℃，预烧保温时间为90分钟。
(4)粉碎：将预烧后的粉料在振磨机中先粗步粉碎成平均粒度≤5μm的小颗粒粉末，再加入辅助成份和纯水，放入砂磨机中进行细粉碎，细粉碎后的粉料平均粒度为0.85～1.1μm。
(5)喷雾造粒：将细粉碎后的料浆泵入喷雾干燥机中进行喷雾造粒。
(6)成型：将喷雾造粒的粉料使用成型机压制成外径约为30mm、内径为18mm、高7.2mm的环形毛坯。
(7)烧结：将成型好的环形毛坯放在真空气氛炉中烧结。开始升温阶段(室温～700℃)炉内压力为常压状态并充入空气，在升温到700℃～1220℃的全程温度内进行抽真空，真空度控制在20～100Pa，当升温到1220℃时，停止抽真空，并充入氧含量为1％的氮氧混合气，并使炉压上升和控制到(1大气压+800Pa)～(1大气压+2500Pa)。保温温度为1270℃，保温时间为240分钟，保温和降温过程中的气氛按平衡氧分压控制。
实施例1～5的具体配方如表1中编号1～5所示。
实施例1～5的主要技术指标测试结果见表2编号1～5所示。
比较例6、7、8的制备方法与实施例1～5主要差别在烧结工序，烧结工序为：开始升温阶段(室温～700℃)炉内压力为常压状态并充入空气，在升温到700℃时充入0.1％的氮氧混合气并使炉压上升到(1大气压+800Pa)～(1大气压+2500Pa)，一直到升温至1220℃，当升温到1220℃时，转变成充入氧含量为1％的氮氧混合气，保温温度为1290℃，保温时间为240分钟，保温和降温过程中的气氛按平衡氧分压控制。
比较例6、7和8的具体配方如表1中6、7和8所示。
比较例6、7和8的主要技术指标测试结果见表2所示。
表1
Figure GDA0002108035210000071
Figure GDA0002108035210000081
表2
Figure GDA0002108035210000082
结合表1、表2可见：实施例1～5在测试频率为100kHz、工作磁通密度为200mT，温度25～120℃时的功率损耗都小于340kW/m3，其中100℃时的功率损耗小于290kW/m3；在测试频率为300kHz、工作磁通密度为100mT，温度25～120℃时的功率损耗都小于300kW/m3，其中在100℃时的功率损耗小于280kW/m3。实施例1～5由于采用抽真空的烧结工艺，可以实现烧结温度比比较例6～8低20度，从而降低了300kHz的高频损耗，有利于实现100～300kHz宽频范围内低损耗。实施例1～5具有更高Bs，在25℃下Bs为550～559mT；在100℃下的Bs为450～458mT。
表3
Figure GDA0002108035210000083
Figure GDA0002108035210000091
结合表1、表2可见：比较例6和7在300kHz、100mT的功率损耗要明显高于实施例1～5，并且Bs也要低些，在25℃下Bs分别为535、540mT，100℃的Bs分别为432、440mT。比较例8为常规宽温低损耗配方，在300kHz、100mT的功率损耗也要明显高于实施例1～5，并且100℃的Bs典型值为420mT，明显低于实施例1～5。
表3为实施例1～5与比较例6～8的密度比较，实施例1～5的密度高于比较例6～8。
实施例9～12：
(1)原料混合：精确称量Fe2O3的含量为53.8mol％，ZnO含量为8.4mol％，NiO含量为0.55mol％，其余为MnO。见表4所示。并加入纯水，纯水的电导率小于2μs/cm；原料与纯水的重量比为1.0：1.0，使用砂磨机进行砂磨40±2分钟，使四种原材料进行充分的混合；
表4
Figure GDA0002108035210000092
(2)烘干：将混合均匀的料浆泵入喷雾干燥机中烘干并造粒。
(3)预烧：将烘干的粉料放入预烧设备中预烧，预烧温度为900℃，预烧保温时间为80分钟。
(4)粉碎：将预烧后的粉料在振磨机中先粗步粉碎成平均粒度≤5μm的小颗粒粉末，再加入辅助成份和纯水，放入砂磨机中进行细粉碎。实施例9～12的辅助成份的添加量见表5。
表5
Figure GDA0002108035210000101
(5)喷雾造粒：将细粉碎后的料浆泵入喷雾干燥机中进行喷雾造粒。
(6)成型：将喷雾造粒的粉料使用成型机压制成外径约为30mm、内径为18mm、高7.2mm的环形毛坯。
(7)烧结：将成型好的环形毛坯放在真空气氛炉中烧结。开始升温阶段(室温～700℃)炉内压力为常压状态，在升温到800℃时开始抽真空，真空度控制在50～150Pa，当升温到1050℃时，停止抽真空，并充入纯氮气，使炉压上升并保持在(1大气压+800Pa)～(1大气压+1500Pa),并以每小时80℃的速度缓慢升温到1150℃；当升温到1150℃时，又开始抽真空并停止充入氮气；当升温到1220℃时，停止抽真空，并充入氧含量为1％的氮氧混合气，使炉压上升并保持在(1大气压+800Pa)～(1大气压+1500Pa)。保温温度为1270℃，保温时间为240分钟，保温和降温过程中的气氛按平衡氧分压控制。
实施例9～12的主要技术指标测试结果见表6所示；
表6
Figure GDA0002108035210000102
Figure GDA0002108035210000111
结合表5、表6可见：实施例9～12在测试频率为100kHz、工作磁通密度为200mT，温度25～120℃时的功率损耗都小于340kW/m3，其中100℃时的功率损耗小于290kW/m3；在测试频率为300kHz、工作磁通密度为100mT，温度25～120℃时的功率损耗都小于300kW/m3，其中100℃时的功率损耗小于280kW/m3。实施例9～12还具有高Bs，在25℃下Bs为552～554mT；在100℃下Bs为451～453mT。
以上所述，仅为本发明的具体实施方式，但本发明的保护范围并不局限于此，熟悉该本领域的技术人员应该明白本发明包括但不限于上面具体实施方式中描述的内容。任何不偏离本发明的功能和结构原理的修改都将包括在权利要求书的范围中。

Claims (3)

1.一种高Bs宽温低损耗软磁铁氧体材料，其特征在于：包括主成分、第一辅助成分、第二辅助成分，其中，主成分包括含量为53.4~53.95mol%的Fe2O3、含量为7.5~9.4mol%为ZnO、含量为0.3~0.8mol%的NiO，其余为MnO；第一辅助成分包括CaCO3、SiO2、Co2O3，第二辅助成分包括Nb2O5、ZrO2、Ta2O5、V2O5、CeO2、HfO2中的一种以上，或者采用TiO2和SnO2中的一种或者两种，辅助成分的添加量如下：
CaCO3：100~1000ppm，
SiO2：10~100ppm，
Co2O3：2500~4500ppm，
Nb2O5：20~500ppm，
ZrO2：20~500ppm，
Ta2O5：50~500ppm，
V2O5：50~800ppm，
CeO2：50~400ppm，
HfO2：50~400ppm，
TiO2：0~2000ppm，
SnO2：0~3000ppm；
上述一种高Bs宽温低损耗软磁铁氧体材料的制备方法，包括如下步骤：
（1）原料混合：根据四种主成分原料的配比进行配料后，放入球磨机或砂磨机中，并加入纯水，使四种原料进行充分的混合；
（2）烘干：将混合均匀的料浆泵入烘干设备中烘干；
（3）预烧：将烘干的粉料放入预烧设备中预烧，预烧温度为800~1000℃，预烧保温时间为30~180分钟；
（4）粉碎：将预烧后的粉料在振磨机中先初步粉碎成平均粒度≤5μm的小颗粒粉末，再加入辅助成分的组合，再加入纯水进行细粉碎，细粉碎后的粉料平均粒度控制在0.7~1.3μm之间；
（5）喷雾造粒：将细粉碎后的浆料在喷雾塔中进行喷雾造粒，喷雾造粒出的粉料松装比重控制在1.25～1.50g/cm3；
（6）成型：将喷雾造粒的粉料使用成型机压制成毛坯；
（7）烧结：将成型好的毛坯放在真空气氛炉中烧结，开始升温阶段炉内压力为常压状态，在升温到700℃～保温温度-X℃的全程或部分温度内进行抽真空，X=0～160，真空度控制在小于3×103Pa，当升温到保温温度- X℃时，停止抽真空，并充入适当比例的氮氧混合气，使炉压上升并保持在正压，范围为1大气压+500Pa~ 1大气压+3000Pa，保温温度为1220℃，保温时间为180~360分钟。
2.根据权利要求1所述的一种高Bs宽温低损耗软磁铁氧体材料，其特征在于：步骤（1）中原料与纯水的重量比为1.0：0.7~1.5，纯水的电导率小于20μs/cm。
3.根据权利要求1所述的一种高Bs宽温低损耗软磁铁氧体材料，其特征在于：步骤（6）中成型后毛坯密度控制为2.9～3.1g/cm3。
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