CN110078489B - 一种低损耗软磁铁氧体材料及其制备方法 - Google Patents

一种低损耗软磁铁氧体材料及其制备方法 Download PDF

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CN110078489B
CN110078489B CN201910393594.XA CN201910393594A CN110078489B CN 110078489 B CN110078489 B CN 110078489B CN 201910393594 A CN201910393594 A CN 201910393594A CN 110078489 B CN110078489 B CN 110078489B
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temperature
ferrite material
soft magnetic
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heat preservation
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李永劬
王微达
严建强
李明治
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Haining Lianfeng Magnet Industry Co ltd
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Abstract

本发明公开了一种低损耗软磁铁氧体材料及其制备方法，其中铁氧体材料包括主成分和辅助成分，其中，主成分包括含量为52.5～53.5mol％的Fe2O3、含量为7.5～10.2mol％为ZnO、含量为0.2～1mol％的FeTiO3，其余为MnO；辅助成份包括CaCO3、SiO2、Nb2O5、ZrO2、Ta2O5、Cr2O3、V2O5、CoO，包括主成分和辅助成分，其中，主成分包括含量为52.7～53.7mol％的Fe2O3、含量为7.5～10.2mol％为ZnO、含量为0.2～1mol％的FeTiO3，其余为MnO；辅助成份包括CaCO3、SiO2、Nb2O5、ZrO2、Ta2O5、Cr2O3、V2O5、CoO，辅助成份添加其中任意四种以上，添加总量为600～3000ppm。本发明主成份中氧化铁的含量相对较少点，侧重于依靠制造方法特别是烧结工艺来进一步提高高温100度的饱和磁通密度，优点在于可以兼顾高温高Bs和更低的损耗。

Description

一种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
随着便携式电子设备的快速发展，尤其是手机、笔记本电脑、数码相机的 巨大需求，也带动了相关配套元件的快速发展，并给这些元件的特性提出了更 高的要求。由于便携式电子设备日趋向小型化和轻量化，从而要求为这些电子 设备提供精准电压的开关电源也要小型化和轻量化，所以在变压器中起核心作 用的磁性材料必须具有更高的性能。主要要求磁性材料工作时具有很低的损耗， 并且具有较高的饱和磁通密度Bs以保证器件工作的稳定性。
发明内容
本发明所要解决的技术问题就是提供一种便携式电子设备开关电源用低损 耗软磁铁氧体材料，降低损耗并提高饱和磁通密度Bs。
为解决上述技术问题，本发明采用如下技术方案：一种低损耗软磁铁氧体 材料，包括主成分和辅助成分，其中，主成分包括含量为52.5～53.5mol％的Fe2O3、 含量为7.5～10.2mol％为ZnO、含量为0.2～1mol％的FeTiO3，其余为MnO；辅助成 份包括CaCO3、SiO2、Nb2O5、ZrO2、Ta2O5、Cr2O3、V2O5、CoO，包括主成分和辅助 成分，其中，主成分包括含量为52.7～53.7mol％的Fe2O3、含量为7.5～10.2mol％ 为ZnO、含量为0.2～1mol％的FeTiO3，其余为MnO；辅助成份包括CaCO3、SiO2、 Nb2O5、ZrO2、Ta2O5、Cr2O3、V2O5、CoO，辅助成份添加其中任意四种以上，添加总 量为600～3000ppm，辅助成份的添加量如下：
CaCO3：100～1000ppm，
SiO2：10～100ppm，
Nb2O5：20～500ppm，
ZrO2：20～500ppm，
Ta2O5：50～500ppm，
Cr2O3：50～500ppm，
V2O5：50～800ppm，
CoO：200～1000ppm。
本发明还提供了一种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780～1000℃，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0.8～1.5μm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)中成型后毛坯为外径29.5mm、内径17.7mm、高度7.1mm 的环形毛坯，毛坯密度控制为2.9～3.1g/cm3。
可选的，步骤(7)中保温温度为1240～1360℃，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：
以前报道的技术提高高温100度的饱和磁通密度Bs一般依靠在组分中大幅 度增加氧化铁含量，但由于氧化铁含量太多导致损耗谷点移向较低温度，从而 导致100℃、100kHz、200mT时的损耗Pcv上升到500kW/m3以上，目前也有专 利技术是通过添加Ni或Li的化合物来将损耗曲线的低谷移动到100度，从而 兼顾100℃Bs≈450mT并使100℃时的Pcv降低到320kW/m3左右，但是以上方 法很难使100℃时的Pcv降低到250kW/m3左右。因为添加Ni或Li的化合物较 多时容易导致损耗上升，添加较少时损耗曲线的低谷移动不到100度。本发明 采用的技术方案，主成份中氧化铁的含量相对较少点，侧重于依靠制造方法特 别是烧结工艺来进一步提高高温100度的饱和磁通密度。优点在于可以兼顾高 温高Bs(100℃Bs≈450mT)和更低的损耗(100℃、100kHz、200mT时的Pcv≈ 250kW/m3)。
饱和磁通密度可由下列经验公式(1)给出：
Figure BDA0002057423990000031
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为材料的居里温度；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。
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
一种低损耗软磁铁氧体材料，包括主成分和辅助成分，其中，主成分包括 含量为52.5～53.5mol％的Fe2O3、含量为7.5～10.2mol％为ZnO、含量为0.2～1mol％ 的FeTiO3，其余为MnO；辅助成份包括CaCO3、SiO2、Nb2O5、ZrO2、Ta2O5、Cr2O3、 V2O5、CoO，辅助成份添加其中任意四种以上，添加总量为600～3000ppm(以原料 总重量为参照)，辅助成份的添加量如下：
CaCO3：100～1000ppm，
SiO2：10～100ppm，
Nb2O5：20～500ppm，
ZrO2：20～500ppm，
Ta2O5：50～500ppm，
Cr2O3：50～500ppm，
V2O5：50～800ppm，
CoO：200～1000ppm。
一种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780～1000℃，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0.8～1.5μm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：
一种在高温下超低损耗并具有更高Bs的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 52.5～53.5mol％，ZnO含量为7.5～10.2mol％，FeTiO3含量为0.2～1mol％，其余为 MnO。并加入纯水，原料与纯水的重量比为1.0：1.0，纯水的电导率小于2μs/cm (纯水的电导率过大会引入有害杂质导致损耗上升)，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900℃，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0.95～1.15μm。
(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29.5mm、内径17.7mm、 高度7.1mm的环形毛坯，毛坯密度控制为2.9～3.1g/cm3；
(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700℃开始抽真空并一直持续 到1250℃，真空度控制在10～100Pa，当升温到1250℃时，停止抽真空，并充 入氧含量为1％～3％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1300℃，保温时间为240分钟，保温时充入氧含量 为3％～5％的氮氧混合气，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1～5所示。
实施例1～5的主要技术指标测试结果见表2所示。
比较例6和7的具体配方如表1中6和7所示,比较例6和7的制备方法与 实施例1～5的主要差别在烧结工序，其余制备方法相同；比较例6和7的烧结工 序为：开始升温阶段(室温～800℃)炉内压力为常压状态并充入空气，在升温 到800℃时充入0.4％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1250℃，当升温到1250℃时，转变成充入氧含量为 1％～3％的氮氧混合气。保温温度为1320℃，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和7的主要技术指标测试结果见表2所示；
表1
Figure BDA0002057423990000071
表2
Figure BDA0002057423990000072
Figure BDA0002057423990000081
结合表1、表2可见：编号1～5的实施例，25℃、100℃时具有更高Bs，在 25℃时Bs为556～558mT，在100℃时Bs为447～458mT；而比较例6和7在25℃的 Bs为523～528mT，100℃的Bs为416～420mT；实施例1～5在100℃时的功率损耗 较低，在244～247kW/m3；比较例6和7在100℃时的功率损耗为262kW/m3、264 kW/m3；
实施例8～10：实施例8～10的主配方见表3所示。
(1)原料混合：精确称量Fe2O3的含量为53.0mol％，ZnO含量为9.2mol％， FeTiO3含量为0.4mol％，其余为MnO。并加入纯水，原料与纯水的重量比为1.0： 1.0，纯水的电导率小于2μs/cm，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3
Figure BDA0002057423990000082
(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。辅助成份的添 加量见表4。
(5)喷雾造粒：将细粉碎后的料浆加入所需比例的PVA溶液并搅拌均匀， 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18 mm、高10mm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700℃时开始抽真空，真空度控制 在50～200Pa，当升温到1050℃时，停止抽真空，并充入氮气，使炉压上升并 保持在(1大气压+800Pa)～(1大气压+1500Pa),并以每小时90℃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1240℃ 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1290℃，保温时间为240分钟， 保温时充入氧含量为3％～5％的氮氧混合气，降温过程中的气氛按平衡氧分压控 制。
实施例8～10的辅助成份如表4中8～10所示。
实施例8～10的主要技术指标测试结果见表4所示。
比较例11和12的主配方同实施例8～10，见表3所示。
比较例11和12的辅助成份如表4中11和12所示。
比较例11和12的制备方法与实施例8～10相同。
比较例11和12的主要技术指标测试结果见表4所示。
从表4、表5可见：实施例8～10的25℃、100℃的Bs分别为556、450mT左 右；并且功耗较低，25℃、100℃的功耗分别约为600、250kW/m3。
比较例11的Bs也较高，但功耗较高，25℃和100℃的功耗明显高于实施例 8～10，主要原因是辅助成份SiO2的含量高出了优选范围。
比较例12的Bs也较高，但功耗较高，25℃和100℃的功耗明显高于实施例 8～10，主要原因是辅助成份Cr2O3的含量高出了优选范围。
表4
Figure BDA0002057423990000101
表5
Figure BDA0002057423990000102
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 (4)

1.一种低损耗软磁铁氧体材料，其特征在于：包括主成分和辅助成分，其中，主成分包括含量为52.7~53.7mol%的Fe2O3、含量为7.5~10.2mol%为ZnO、含量为0.2~1mol%的FeTiO3，其余为MnO；辅助成份包括CaCO3、SiO2、Nb2O5、ZrO2、Ta2O5、Cr2O3、V2O5、CoO，辅助成份添加其中任意四种以上，添加总量为600~3000ppm，辅助成份的添加量如下：
CaCO3：100~1000ppm，
SiO2：10~100ppm，
Nb2O5：20~500ppm，
ZrO2：20~500ppm，
Ta2O5：50~500ppm，
Cr2O3：50~500ppm，
V2O5：50~800ppm，
CoO：200~1000ppm，
上述一种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780~1000℃，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0.8~1.5μm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。
2.根据权利要求1所述的一种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所述的一种低损耗软磁铁氧体材料，其特征在于：步骤（6）中成型后毛坯为外径29.5mm、内径17.7mm、高度7.1mm的环形毛坯，毛坯密度控制为2.9～3.1g/cm3。
4.根据权利要求1所述的一种低损耗软磁铁氧体材料，其特征在于：步骤（7）中保温温度为1240~1360℃，保温时间为180~360分钟。
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