CN111370196A - 适用于MIM绕线电感用FeSiCr软磁粉末、制备方法及绕线电感 - Google Patents
适用于MIM绕线电感用FeSiCr软磁粉末、制备方法及绕线电感 Download PDFInfo
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- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
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Abstract
本发明公开的是一种适用于MIM绕线电感用FeSiCr软磁粉末、制备方法及绕线电感,所述FeSiCr软磁粉末的合金成分以质量百分比计为:3.0‑6.0%Cr,3.0‑8.0%Si,0.5‑2.0%Ti,3.0‑5.0%Co,82‑90.5%Fe。与现有技术相比,本发明所制备FeSiCr软磁合金粉末,具有合金成分、组织结构均匀,粉末粒度细且分布合理,球形度好,杂质含量低等优点,可作为MIM绕线电感的原材料得到广泛应用。
Description
技术领域
本发明涉及软磁合金粉末的制备方法领域,具体是指一种适用于MIM绕线电感用FeSiCr软磁粉末、制备方法及绕线电感。
背景技术
铁硅铬(FeSiCr)软磁合金粉末广泛应用于绕线电感类器件,具有体积小、损耗低、耐大电流、屏蔽性能优良、抗腐蚀、可靠性高的特点,在移动通信、服务器、转换器、汽车电子等行业领域获得广泛应用。
常规软磁制品制备方式为传统的粉末干压成型法。具体是将线圈绕组埋入金属磁性粉末内部压制而成,原料粉末的粒度及粒度分布、形貌和压制方式等对其成型坯的密度及其分布有重要影响,压制过程容易造成磁芯密度不均、尺寸精度较低.此外,复杂形状磁芯设计也受到很大的限制等。
金属注射成型技术(Metal Injecting Molding,简称MIM)可以很好地解决这些问题,其结合了粉末冶金和注射成型特性的新型零件生产方法。不仅具有粉末冶金制品的材料利用率高的特点,同时还具有注射成型的生产效率高、制品密度均一、强度、尺寸精度高的优势;可以一次性生产如方柱型、圆柱形等多种类型磁芯产品,而不需要借助切削设备,特别是可以生产形状复杂且精度要求较高的产品。此外,注塑成型自动化程度较高,人工较少,适合大批量工业化生产。
MIM工艺中,最关键也是最基础的是粉体的特性。而粉体性能直接关系到绕线电感工艺的稳定性和磁性能的优劣。原料粉末的粒度及其分布、形貌和粉体性能对其制品的磁性能和产品一致性有着重要的影响。因此,选用粒度细小分布集中、粉末形貌规则呈近球形、氧含量低、无团聚的原料粉末,所制备的绕线电感具有损耗低、感值高、磁导率稳定、直流叠加特性好等诸多优势。
目前,MIM常用FeSiCr软磁粉末的制备方法可分为气雾化法和水气联合雾化法。其中,气雾化法在制备超细粉末方面存在一定困难,且气雾化制备粉末基本呈球形,致使MIM脱脂过程中,生胚保型性差,产品易变形。水气联合雾化制粉方法综合了气雾化和水雾化的优势,所制备合金粉末具有粉末氧含量低,类球形的优点。但水气联合雾化过程中,因主副喷双V型喷嘴喷射形成的负压液墙内,气流较紊乱使得熔融金属液滴之间存在相互碰撞的现象,致使部分粉体颗粒之间存在粘连、团聚的现象,从而导致MIM所制备喂料粘度大流动性降低,填充性较差,生胚注射密度低。
发明内容
有鉴于此,本发明的目的在于克服现有MIM用气雾化FeSiCr软磁合金粉末细粉率低,MIM生胚保型性差致使产品易变形的缺陷,以及采用水气联合雾化FeSiCr软磁合金粉末颗粒之间存在粘连团聚,导致喂料流动性差,注射生胚密度低的问题。
为了解决上述问题,本发明的核心创新点是:通过优化合金成分、采用水气联合雾化制粉并结合流化床气流磨粉体改性的方式制备了一种适用于MIM绕线电感用FeSiCr软磁合金粉末。
铁硅铬(FeSiCr)软磁合金粉末广泛应用于绕线电感类器件,具有良好的直流叠加特性、可塑性好、高频功率损耗低、抗老化能力强、磁导率高等特点,该电感类器件广泛应用于手机、电脑等电子通信行业领域。
Si增大了合金的电阻率,进而降低涡流损耗;并且随着Si含量的增加,磁晶各向异性常数和磁致伸缩系数逐渐减小,这对提高合金磁导率是有利的。Cr可以提高材料的塑性、机械强度、以及在恶劣环境中的抗腐蚀能力。适量掺杂合金元素,优化合金化学成分对于改善绕线电感类器件的直流叠加特性、磁芯损耗、电阻率等磁特性参数具有十分显著的效果。Co位于周期表中第VIII族第四周期,具有较高的饱和磁感应强度,Co-Fe之间的强交换偶尔作用可以有效提高软磁材料居里温度和软磁性能,适当添加Co可以增大FeSiCr磁芯饱和磁感应强度,进而改善其直流偏置特性。而少量Ti的添加减少了粉末内部如析出相、内应力、空洞和夹杂等阻碍磁化的组织缺陷,降低FeSiCr系列产品矫顽力、磁芯损耗;而Ti原子尺寸较Fe大,同时Ti的添加细化了合金晶粒尺寸,电子散射概率增加,这对于提升合金电阻率具有显著效果,从而降低磁芯损耗、提高其耐击穿性能。
水气联合雾化制粉方法雾化机理是在氮气保护的条件下,合金液在经过中间包底部的漏眼流入雾化区域,被高速循环负压气流进行初次击碎,形成粗大金属液滴,再通过紧耦合双V型主副喷喷嘴喷射出的超高压水进行二次破碎,继而冷却凝固为类球形粉末颗粒。
流化床气流磨工艺是利用高速气流(300-500m/s)带动粉体颗粒,使其相互碰撞、冲击,利用碰撞时产生的冲击力使团聚粒子分散,团聚体解开的一种物理破碎的粉体加工技术。粉末中团聚体经颗粒之间冲击而分散,且由于粉体之间的表面摩擦运动而磨削掉颗粒表面的棱角,颗粒表面变得更加圆滑和规整,从而得到呈类球形且分散的粉末颗粒。而后,经气流磨破碎后物料被负压上升气流输送至分级区,由内分级轮筛选出达到粒度要求的粉末,未满足粒度要求的粗粉返回粉碎区继续破碎。该工艺具有生产效率高,粉体粒度均匀、类球形以及粉体之间无粘连、分散性好等特点,适用于采用MIM制备绕线电感产品。
MIM绕线电感用FeSiCr软磁合金粉末,其所使用粉末的化学成分、粒径、粉末形貌及氧含量等参数至关重要。粉末化学成分决定了绕线电感件软磁性能及防锈性。粉末粒度细小,呈类球形、分散少无团聚,则MIM喂料装载量大流动性好,且后续产品脱脂烧结过程维形性好,所制备绕线电感件烧结密度、尺寸一致性和稳定性更高。确保了所制备绕线电感类器件具有优良的直流叠加特性、高频低损耗、耐击穿能力强、磁导率高等优异综合软磁性能。
为了达成上述目的,本发明的解决方案是:
一种适用于MIM绕线电感用FeSiCr软磁粉末,其中:其成分以质量百分比计分别为:3.0-6.0%Cr,3.0-8.0%Si,0.5-2.0%Ti,3.0-5.0%Co,82-90.5%Fe。
进一步,所述FeSiCr软磁粉末的激光粒度D90:22-24μm,粉末氧含量≤0.2wt%,粉末振实密度≥4.4g/cm3。
本发明的另一目的在于提供一种适用于MIM绕线电感用FeSiCr软磁粉末的制备方法,其中,包括如下步骤:
1)中频感应熔炼:其采用的合金成分以质量百分比计为:3.0-6.0%Cr,3.0-8.0%Si,0.5-2.0%Ti,3.0-5.0%Co,82-90.5%Fe;
2)将熔炼形成合金材料通过水气联合雾化形成合金粉末;
3)真空干燥合金粉末;
4)粉体气流磨:采用流化床气流磨对干燥后的合金粉体进行破碎分散;
5)合批处理。
进一步,在步骤1)中,按上述合金成分进行配料,将原材料按纯铁、纯铬、钛铁、纯钴、高纯硅的顺序,依次投料、于刚玉坩埚中冶炼,控制冶炼功率为200-500KW,冶炼时长为60.0-80.0分钟,待钢液温度达到1580-1620℃,降低功率为90-120KW,采用适量除渣剂、脱氧剂对钢液进行造渣脱氧处理,过程时长为10.0-15.0分钟,继而扒渣干净,起泵浇钢。
进一步,在步骤2)中,采用氮气作为过程保护气氛,氮气流量为30.0m3/h;雾化过程采用35°/25°主副喷喷盘,钢液中间包底部漏眼尺寸为3.0-4.0mm,雾化压力为90-120MPa,雾化水流量为100-140L/min;
进一步,在步骤3)中,采用双锥真空干燥机干燥合金粉末,干燥温度为130-190℃,真空度≤-0.09MPa;
进一步,在步骤4)中,磨室料量控制在18-20kg,工质压力0.6-0.65MPa,分选轮转速为1000-2500r/min。
本发明的又一目的是提供一种用上述FeSiCr软磁粉末制备形成的绕线电感,其中,在氩气气氛和1000℃烧结条件下,其烧结密度≥5.9g/cm3;电感值Ls≥50μH;电阻率≥80.5×10-5Ω·cm;损耗Ps≤400kW/m3@0.5T,100KHZ。
采用上述方案后,本发明的核心创新点是:通过优化合金成分、采用水气联合雾化制粉并结合流化床气流磨粉体改性的方式制备了一种适用于MIM绕线电感用FeSiCr软磁合金粉末,并在实际研发过程中对各个细节参数进行了限定,如此方能得到达到所需标准的合金粉末以及绕线电感。
与现有技术相比,本发明具有以下有益效果:
1、将原材料按以下合金质量百分比成分配料:3.0-6.0%Cr,3.0-8.0%Si,0.5-2.0%Ti,3.0-5.0%Co,82-90.5%Fe,通过中频感应熔炼,水气联合雾化,配合后期真空干燥,粉体分级及筛分、合批处理等工序,可制备球形度好、氧含量低、粒度分布合理FeSiCr软磁合金粉末;具体粉末激光粒度为D90:22-24μm,氧含量≤0.2wt%,振实密度≥4.4g/cm3。
2、一种绕线电感件:(一)将聚甲醛(POM)、高密度聚乙烯(HDPE)、乙酸-乙酸乙烯共聚物(EVA)、硬脂酸(SA)和聚乙烯蜡(PE-Wax)等材料于190℃密炼机中混炼均匀得到粘结剂;再将FeSiCr粉末和粘结剂于密炼机中180℃密炼120min,其中粉末装载量为62%,得到块状泥料,再经造粒机制备出MIM用粒状喂料。(二)将喂料在注塑机料筒里190℃加热熔化,并注射成Φ27mm×内径Φ14.5mm环形生胚。生胚于110℃脱脂炉内硝酸脱脂2小时。最后对磁环进行真空烧结,烧结温度为1000℃,保温2小时。
采用排水法测量电感件的烧结密度;采用TH2816B/TH2826 LCR测试仪测试电感在f=100kHz,1V条件下电感值Ls;采用SZT-2C四探针测试仪测量电感的电阻率;采用MATS-2010SA软磁合金交流测量装置测试环形电感在Bm=0.5T,f=100kHz条件下损耗值。可知电感件烧结密度≥5.9g/cm3;电感值Ls≥50μH;电阻率≥80.5×10-5Ω·cm;损耗Ps≤400kW/m3。
3、本发明采用水气联合雾化结合气流磨工艺制备此合金粉末,更好地保证制备的软磁合金粉末球形度好振实密度高,粉体分散性好,粉末氧含量低,MIM绕线电感具有烧结密度高、感值、电阻率高以及损耗低的特点。
具体实施方式
下面结合实例,对本发明做进一步详细的说明,但本发明的实施方式不止于此。
实施例1
一种适用于MIM绕线电感用FeSiCr软磁粉末的制备方法,包括:
1)中频感应熔炼:
合金成分以质量百分比计为86.5wt%Fe,3.5wt%Si,4.5wt%Cr,0.5wt%Ti,5.0wt%Co,按上述合金成分进行配料,将原材料按纯铁、铬铁、纯镍、纯钼、高纯硅的顺序,依次投料、于刚玉坩埚中冶炼,控制冶炼功率为200-500KW,冶炼时长为60.0-80.0分钟,待钢液温度达到1580-1620℃,降低功率为90-120KW,采用适量除渣剂、脱氧剂对钢液进行造渣脱氧处理,过程时长为10.0分钟,继而扒渣干净,起泵浇钢;
2)水气联合雾化:采用氮气作为过程保护气氛,氮气流量为30.0m3/h;雾化过程采用35°/25°主副喷喷盘,钢液中间包底部漏眼尺寸为4.0mm,雾化压力为100MPa,雾化水流量为120L/min;
3)真空干燥:采用双锥真空干燥机干燥合金粉末,干燥温度为180℃,真空度≤-0.09MPa;
4)粉体气流磨:采用流化床气流磨对合金粉体进行破碎分散;磨室料量控制在18kg,工质压力0.6MPa,分选轮转速为1500r/min;
5)合批处理。
实施例2
本实施例2与实施例1的区别在于:本实施例2中制备的一种适用于MIM绕线电感件用FeSiCr软磁合金粉末成分进行调整,所制备合金粉末合金成分组成为:83.5wt%Fe-6.5wt%Si-4.5wt%Cr-0.5wt%Ti-5.0wt%Co,上述成分均为质量百分比。
实施例3
本实施例3与实施例1的区别在于:本实施例3中调整制备一种适用于MIM绕线电感用FeSiCr软磁粉末的水气联合雾化工艺。具体雾化工艺为:采用氮气作为过程保护气氛,氮气流量为30.0m3/h;采用35°/25°主副喷喷盘;钢液中间包底部漏眼尺寸为5.0mm,雾化水压力为120MPa,水流量为140L/min。
实施例4
本实施例4与实施例1的区别在于:本实施例4中调整制备一种适用于MIM绕线电感用FeSiCr软磁合金粉末的水气联合雾化工艺。具体雾化工艺为:采用氮气作为过程保护气氛,氮气流量为30.0m3/h;采用35°/25°主副喷喷盘,双V型喷嘴;钢液中间包底部漏眼尺寸为4.5mm,雾化水压力为105MPa,水流量为125L/min。
对比例1
本对比例1与实施例1的区别在于:本对比例1中采用水气雾化制粉工艺制备金属粉末。依次中频感应熔炼、常规水雾化、真空干燥、粉体分级及筛分、合批处理等工艺,制成颗粒状合金粉末,对比流化床气流磨对粉末、电感产品性能的影响。
对比例2
本对比例2与实施例1的区别在于:本对比例2中制备的一种FeSiCr软磁合金粉末,合金成分中不含钛、钴合金元素;本对比例2中合金成分设计为:92wt%Fe-3.5wt%Si-4.5wt%Cr。
本发明实施例1-4,对比例1-2所制备的合金粉末及电感件性能表征,见下表1:
表1
由表1可知,本发明实施例1-4均可制备一种适用于MIM绕线电感件用FeSiCr软磁合金粉末。通过对比例1可说明采用水气联合雾化结合气流磨粉体改性工艺更好的保证了制备的软磁合金粉末粒度分布合理,粉末球形度好振实密度高,氧含量低等特点,所制备MIM绕线电感产品具有烧结密度高,磁芯电感值高直流偏置特性好,电阻率率高耐击穿特性好,磁损耗低等诸多优势。通过对比例2可知,Ti、Co元素的复合添加提高了电感产品电感值和电阻率,同时降低了磁芯损耗,FeSiCr烧结成型产品综合磁性能显著改善。
上述实施例仅为本发明的优选实施例,并非对本发明保护范围的限制,但凡采用本发明的设计原理,以及在此基础上进行非创造性劳动而作出的变化,均应属于本发明的保护范围之内。
Claims (8)
1.一种适用于MIM绕线电感用FeSiCr软磁粉末,其特征在于:其成分以质量百分比计分别为:3.0-6.0%Cr,3.0-8.0%Si,0.5-2.0%Ti,3.0-5.0%Co,82-90.5%Fe。
2.如权利要求1所述的一种适用于MIM绕线电感用FeSiCr软磁粉末,其特征在于:所述FeSiCr软磁粉末的激光粒度D90:22-24μm,粉末氧含量≤0.2wt%,粉末振实密度≥4.4g/cm3。
3.一种适用于MIM绕线电感用FeSiCr软磁粉末的制备方法,其特征在于,包括如下步骤:
1)中频感应熔炼:其采用的合金成分以质量百分比计为:3.0-6.0%Cr,3.0-8.0%Si,0.5-2.0%Ti,3.0-5.0%Co,82-90.5%Fe;
2)将熔炼形成合金材料通过水气联合雾化形成合金粉末;
3)真空干燥合金粉末;
4)粉体气流磨:采用流化床气流磨对干燥后的合金粉体进行破碎分散;
5)合批处理。
4.如权利要求3所述的一种适用于MIM绕线电感用FeSiCr软磁粉末的制备方法,其特征在于,在步骤1)中,按上述合金成分进行配料,将原材料按纯铁、纯铬、钛铁、纯钴、高纯硅的顺序,依次投料、于刚玉坩埚中冶炼,控制冶炼功率为200-500KW,冶炼时长为60.0-80.0分钟,待钢液温度达到1580-1620℃,降低功率为90-120KW,采用适量除渣剂、脱氧剂对钢液进行造渣脱氧处理,过程时长为10.0-15.0分钟,继而扒渣干净,起泵浇钢。
5.如权利要求3所述的一种适用于MIM绕线电感用FeSiCr软磁粉末的制备方法,其特征在于,在步骤2)中,采用氮气作为过程保护气氛,氮气流量为30.0m3/h;雾化过程采用35°/25°主副喷喷盘,钢液中间包底部漏眼尺寸为3.0-4.0mm,雾化压力为90-120MPa,雾化水流量为100-140L/min。
6.如权利要求3所述的一种适用于MIM绕线电感用FeSiCr软磁粉末的制备方法,其特征在于,在步骤3)中,采用双锥真空干燥机干燥合金粉末,干燥温度为130-190℃,真空度≤-0.09MPa。
7.如权利要求3所述的一种适用于MIM绕线电感用FeSiCr软磁粉末的制备方法,其特征在于,在步骤4)中,磨室料量控制在18-20kg,工质压力0.6-0.65MPa,分选轮转速为1000-2500r/min。
8.一种用如权利要求1-2任一项所述FeSiCr软磁粉末制备形成的绕线电感,其中,在氩气气氛和1000℃烧结条件下,其烧结密度≥5.9g/cm3;电感值Ls≥50μH;电阻率≥80.5×10-5Ω·cm;损耗Ps≤400kW/m3@0.5T,100KHZ。
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