CN113889312B - 一种细晶粒高绝缘性能复合软磁合金粉末及其制备方法 - Google Patents
一种细晶粒高绝缘性能复合软磁合金粉末及其制备方法 Download PDFInfo
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Abstract
一种细晶粒高绝缘性能复合软磁合金粉末及其制备方法,该软磁合金粉末的化学式为Fe1‑x‑ySixCry/M,式中x为0.045‑0.06,y为0.045~0.06,M为纳米Al2O3或ZrO2。其制备方法包括以下步骤:(1)配料;(2)熔炼:将步骤(1)所得的混合料置于中频感应熔炼炉中进行高温熔炼,直至形成高温熔液;(3)喷雾制粉:将步骤(2)所得的高温熔液倾倒至中间包坩埚,通过限流导液管流入喷雾室,在高压高速雾化介质氮气作用下将高温熔液冲击破碎成细小金属熔滴,继而在下落冷却过程中表面张力作用下,凝固成复合软磁合金球形或亚球形粉末;(4)钝化;(5)造粒,即成。本发明能细化晶粒粒度,提高FeSiCr软磁合金粉末的绝缘耐压性。
Description
技术领域
本发明涉及一种软磁合金粉末及其制备方法,尤其涉及一种细晶粒高绝缘性能复合软磁合金粉末及其制备方法。
背景技术
随着5G/6G、物联网和NFC等新兴网络及电子行业的发展,软磁材料电子元器件的需求日益增加,对电子元器件的小型化、超薄型一体成型电感的性能要求越来越高。一体成型电感需要高磁导率、高饱和和低损耗的软磁合金粉末,FeSiCr软磁合金粉末因具有高磁导率和中高频磁损耗低的特点广泛应用于一体成型电感。但是,FeSiCr软磁合金粉末制备的一体成型电感具有强度低和容易开裂等缺点。
CN110004382A公开了一种适用于环形电感件用FeSiCr软磁合金粉末的制备方法,步骤如下:1)中频感应熔炼:按以下合金成分质量百分比进行配料:4.0-8.0%Cr,2.0-8.0%Si,1.2-2.0%Ni,0.5-0.8%Mo,85-92.3%Fe;之后将所配的原材料按纯铁、铬铁、纯镍、纯钼、高纯硅的顺序,依次投料于刚玉坩埚中冶炼,待钢液温度达到1580-1620℃,进行造渣脱氧处理;2)水气联合雾化:采用氮气作为过程保护气氛,雾化过程采用40°/30°主副喷双V型喷嘴,钢液中间包底部漏眼尺寸为3.0-4.0mm,雾化压力为100-120MPa,雾化水流量为100-140L/min;3)干燥及筛分处理:采用真空干燥合金粉末,之后进行粉体分级及筛分处理。但该FeSiCr软磁合金粉末的损耗仍然较高。
CN110148509 A公开了一种高可靠性FeSiCr一体成型电感颗粒料及其制备方法,该颗粒料是由FeSiCr绝缘合金粉、纳米BN和纳米SiO2组合改性的E20环氧树脂、高温(≥80℃)低温(50℃附近))两种加热固化型潜伏固化剂有机组合,50℃~70℃的条件下烘烤60分钟~80分钟制得。但该方法中陶瓷氧化物通常是在一体成型电感的配料工艺中掺入到软磁合金粉末里,容易存在掺入不均匀、降低粉末绝缘性的问题,如何使陶瓷氧化物均匀地修饰FeSiCr软磁合金是提高绝缘耐压性的关键。
发明内容
本发明要解决的技术问题是,克服现有技术存在的上述缺陷,提供一种细化晶粒粒度,提高FeSiCr软磁合金粉末绝缘耐压性的细晶粒高绝缘性能复合软磁合金粉末。
本发明进一步要解决的技术问题是,提供一种操作简便的细晶粒高绝缘性能复合软磁合金粉末的制备方法。
本发明解决其技术问题采用的技术方案是,一种细晶粒高绝缘性能复合软磁合金粉末,其化学式为Fe1-x-ySixCry/M,式中x为0.045~0.06,y为0.045~0.06,M为纳米Al2O3或ZrO2。
本发明进一步解决其技术问题采用的技术方案是,一种细晶粒高绝缘性能复合软磁合金粉末的制备方法,包括以下步骤:
(1)配料:称取原料工业纯铁Fe、纯硅Si、纯金属铬Cr、纳米Al2O3或纳米ZrO2,混合均匀,得混合料;
(2)熔炼:将步骤(1)所得的混合料置于中频感应熔炼炉中进行高温熔炼,得高温熔液;
(3)喷雾制粉:将步骤(2)所得的高温熔液倾倒至中间包坩埚,通过限流导液管流入喷雾室,在高压高速的氮气作用下进行雾化,将高温熔液冲击破碎成细小金属熔滴,细小金属熔滴在下落冷却过程中表面张力作用下,凝固成复合软磁合金球形或亚球形粉末;
(4)钝化:使用磷酸二氢铝为钝化剂主剂,蒸馏水与丙酮的混合液为稀释剂,对步骤(3)所得的复合软磁合金球形或亚球形粉末进行钝化处理,然后过滤,收集含水粉末,用高压空气吹至半干,得半干粉末;
(5)造粒:将步骤(4)所得的半干粉末烘干,加入改性环氧树脂与酚醛树脂的混合溶液进行造粒,分筛,烘干,冷却至室温,再加入纳米硬脂酸镁为润滑剂,混合均匀,即得细晶粒高绝缘性能复合软磁合金粉末。
进一步,步骤(1)中,所述原料按以下重量百分比配料:工业纯铁Fe 88-91wt%、纯硅Si 4.5-6.0wt%、纯金属铬Cr 4.5-6.0wt%、纳米Al2O3或纳米ZrO2 0.3-0.5wt%。
进一步,步骤(2)中,所述高温熔炼的功率为80-240KW;所述高温熔炼的温度为1620-1750℃;所述高温熔炼的时间为12-18min(优选15min);所述高温熔炼的真空度为0.001Mpa。
进一步,步骤(3)中,所述高压为0.4-0.85Mpa;所述雾化的粉末粒度D50为8-15μm。
进一步,步骤(4)中,所述钝化剂的加入量为步骤(3)所得复合软磁合金质量的0.3-0.5wt%。
进一步,步骤(4)中,所述钝化的温度为15-75℃,优选50-70℃;所述钝化的时间为20-60min,优选30-40min。
进一步,步骤(4)中,所述稀释剂中蒸馏水与丙酮的体积比为1~3:1。
进一步,步骤(5)中,所述改性环氧树脂与酚醛树脂的混合溶液的加入量为步骤(4)所得半干粉末的质量的2.0~4.0%。
进一步,步骤(5)中,所述分筛后的粉末粒径为50-350目;所述烘干的温度为60~80℃;所述烘干的时间为80~100min。
进一步,步骤(5)中,所述纳米硬脂酸镁的加入量为烘干后的粉末的质量的0.1~0.3wt%。
与现有技术相比,本发明的有益效果为:
(1)本发明复合软磁合金粉末,在FeSiCr软磁合金粉末中加入陶瓷颗粒纳米Al2O3或纳米ZrO2粉末形成复合材料,大幅提高了软磁合金的绝缘耐压性,并且由于不导电的陶瓷颗粒附着在软磁合金晶粒的表面,能够在细化FeSiCr软磁合金粉末晶粒粒度的同时,提高其绝缘耐压性;
(2)本发明复合软磁合金粉末的制备方法,将陶瓷颗粒纳米Al2O3或纳米ZrO2作为原材料在熔炼雾化时加入,简化了生产流程、降低了生产成本,适于工业化大规模生产。
具体实施方式
下面结合具体实施例对本发明作进一步说明。
实施例1
本实施例细晶粒高绝缘性能复合软磁合金粉末的化学式为Fe0.9Si0.055Cr0.045/Al2O3。
本实施例细晶粒高绝缘性能复合软磁合金粉末的制备方法,包括以下步骤:
(1)配料:称取原料工业纯铁Fe 9kg、纯硅Si 0.55kg、纯金属铬Cr 0.45kg和纳米Al2O3 40g,混合均匀,得混合料;
(2)熔炼:将步骤(1)所得的混合料装入中频感应熔炼炉中进行高温熔炼,熔炼的功率为200KW,熔炼的温度为1700℃,熔炼的时间为15min,熔炼的真空度0.001Mpa,得高温熔液;
(3)喷雾制粉:将步骤(2)所得的高温熔液倾倒至中间包坩埚,通过限流导液管流入喷雾室,在高压高速雾化介质氮气作用下将高温熔液冲击破碎成细小金属熔滴,氮气压力为0.75Mpa,细小金属熔滴在下落冷却过程中表面张力作用下凝固成复合软磁合金球形或亚球形粉末;
(4)钝化:使用0.04kg磷酸二氢铝为钝化剂主剂,蒸馏水与丙酮的混合液(体积比为1:1)为稀释剂,将步骤(3)所得的复合软磁合金球形或亚球形粉末在50℃下钝化处理30min,然后过滤,收集含水粉末,高压空气吹至半干,得半干粉末;
(5)造粒:将步骤(4)所得的半干粉末120℃烘干30min,加入0.3kg改性环氧树脂与酚醛树脂的混合溶液进行造粒,分筛,70℃烘干90min,冷却至室温,再加入0.02kg纳米硬脂酸镁为润滑剂,混合均匀,即得细晶粒高绝缘性能复合软磁合金粉末。
性能测试方法:称取本实施例所得细晶粒高绝缘性能复合软磁合金粉末2g在400-600MPa压力条件下,压制外径为14mm、内径为8mm的生坯样品;然后,将样品进行160℃×180min烘烤后随炉冷却至室温;绕制线径为0.5mm的铜线17.5匝,采用Agilent4285A精密LCR测试仪测试磁环电感值,计算粉材磁导率,测试条件为电压0.5V,频率100kHz,电源功率为50W。用方块样品Φ4X1.5mm测试样品的绝缘阻抗性能。
以下实施例2~3和对比例1~4分别所得的复合软磁合金粉末的测试方法与本实施例相同。
实施例2
本实施例细晶粒高绝缘性能复合软磁合金粉末的化学式为Fe0.91Si0.05Cr0.04/Al2O3。
本实施例细晶粒高绝缘性能复合软磁合金粉末的制备方法,包括以下步骤:
(1)配料:称取原料工业纯铁Fe 9.1kg、纯硅Si 0.5kg、纯金属铬Cr 0.4kg和纳米Al2O3 40g,混合均匀,得混合料;
(2)熔炼:将步骤(1)所得的混合料装入中频感应熔炼炉中进行高温熔炼,熔炼的功率为200KW,熔炼的温度为1700℃,熔炼的时间为15min,熔炼的真空度0.001Mpa,得高温熔液;
(3)喷雾制粉:将步骤(2)所得的高温熔液倾倒至中间包坩埚,通过限流导液管流入喷雾室,在高压高速雾化介质氮气作用下将高温熔液冲击破碎成细小金属熔滴,氮气压力为0.75Mpa,细小金属熔滴在下落冷却过程中表面张力作用下凝固成复合软磁合金球形或亚球形粉末;
(4)钝化:使用0.04kg磷酸二氢铝为钝化剂主剂,蒸馏水与丙酮的混合液(体积比为1:1)为稀释剂,将步骤(3)所得的复合软磁合金球形或亚球形粉末在50℃下钝化处理30min,然后过滤,收集含水粉末,高压空气吹至半干,得半干粉末;
(5)造粒:将步骤(4)所得的半干粉末120℃烘干30min,加入0.3kg改性环氧树脂与酚醛树脂的混合溶液进行造粒,分筛,70℃烘干90min,冷却至室温,再加入0.02kg纳米硬脂酸镁为润滑剂,混合均匀,即得细晶粒高绝缘性能复合软磁合金粉末。
实施例3
本实施例细晶粒高绝缘性能复合软磁合金粉末的化学式为Fe0.9Si0.055Cr0.045/ZrO2。
本实施例细晶粒高绝缘性能复合软磁合金粉末的制备方法,包括以下步骤:
(1)配料:称取原料工业纯铁Fe 9kg、纯硅Si 0.55kg、纯金属铬Cr 0.45kg和纳米ZrO2 40g,混合均匀,得混合料;
(2)熔炼:将步骤(1)所得的混合料装入中频感应熔炼炉中进行高温熔炼,熔炼的功率为200KW,熔炼的温度为1700℃,熔炼的时间为15min,熔炼的真空度0.001Mpa,得高温熔液;
(3)喷雾制粉:将步骤(2)所得的高温熔液倾倒至中间包坩埚,通过限流导液管流入喷雾室,在高压高速雾化介质氮气作用下将高温熔液冲击破碎成细小金属熔滴,氮气压力为0.75Mpa,细小金属熔滴在下落冷却过程中表面张力作用下凝固成复合软磁合金球形或亚球形粉末;
(4)钝化:使用0.04kg磷酸二氢铝为钝化剂主剂,蒸馏水与丙酮的混合液(体积比为1:1)为稀释剂,将步骤(3)所得的复合软磁合金球形或亚球形粉末在50℃下钝化处理30min,然后过滤,收集含水粉末,高压空气吹至半干,得半干粉末;
(5)造粒:将步骤(4)所得的半干粉末120℃烘干30min,加入0.3kg改性环氧树脂与酚醛树脂的混合溶液进行造粒,分筛,70℃烘干90min,冷却至室温,再加入0.02kg纳米硬脂酸镁为润滑剂,混合均匀,即得细晶粒高绝缘性能复合软磁合金粉末。
对比例1
本对比例软磁合金粉末的化学式为Fe0.9Si0.055Cr0.045。
本对比例软磁合金粉末的制备方法,包括以下步骤:
(1)配料:称取原料工业纯铁Fe 9kg、纯硅Si 0.55kg和纯金属铬Cr 0.45kg,混合均匀,得混合料;
(2)熔炼:将步骤(1)所得的混合料装入中频感应熔炼炉中进行高温熔炼,熔炼的功率为200KW,熔炼的温度为1700℃,熔炼的时间为15min,熔炼的真空度0.001Mpa,得高温熔液;
(3)喷雾制粉:将步骤(2)所得的高温熔液倾倒至中间包坩埚,通过限流导液管流入喷雾室,在高压高速雾化介质氮气作用下将高温熔液冲击破碎成细小金属熔滴,氮气压力为0.75Mpa,细小金属熔滴在下落冷却过程中表面张力作用下凝固成复合软磁合金球形或亚球形粉末;
(4)钝化:使用0.04kg磷酸二氢铝为钝化剂主剂,蒸馏水与丙酮的混合液(体积比为1:1)为稀释剂,将步骤(3)所得的复合软磁合金球形或亚球形粉末在50℃下钝化处理30min,然后过滤,收集含水粉末,高压空气吹至半干,得半干粉末;
(5)造粒:将步骤(4)所得的半干粉末120℃烘干30min,加入0.3kg改性环氧树脂与酚醛树脂的混合溶液进行造粒,分筛,70℃烘干90min,冷却至室温,再加入0.02kg纳米硬脂酸镁为润滑剂,混合均匀,即得细晶粒高绝缘性能复合软磁合金粉末。
对比例2
本对比例复合软磁合金粉末的化学式为Fe0.9Si0.055Cr0.045。
对比例2与实施例1的区别在于,对比例2中纳米Al2O3 40g不是在熔炼雾化时加入,而是在钝化过程中加入。
对比例3
本对比例复合软磁合金粉末的化学式为Fe0.85Si0.065Cr0.085/Al2O3,配料时各原料的重量为Fe 8.5kg、纯硅Si 0.65kg、纯金属铬Cr 0.85kg和纳米Al2O3 40g,混合均匀,得混合料,其它制备条件与实施例1相同。
对比例4
本对比例复合软磁合金粉末的化学式为Fe0.85Si0.065Cr0.085/ZrO2,配料时各原料的重量为Fe 8.5kg、纯硅Si 0.65kg、纯金属铬Cr 0.85kg和纳米ZrO240g,混合均匀,得混合料,其它制备条件与实施例3相同。
表1本发明实施例1~3与对比例1~4分别所得的复合软磁合金粉末的性能参数测试结果
Claims (23)
1.一种细晶粒高绝缘性能复合软磁合金粉末,其特征在于,其化学式为Fe1-x-ySixCry/M,式中x为0.045~0.06,y为0.045~0.06,M为纳米Al2O3或ZrO2;
所述细晶粒高绝缘性能复合软磁合金粉末的制备方法,包括以下步骤:
(1)配料:称取原料工业纯铁Fe、纯硅Si、纯金属铬Cr、纳米Al2O3或纳米ZrO2,混合均匀,得混合料;所述原料按以下重量百分比配料:工业纯铁Fe 88-91wt%、纯硅Si 4.5-6.0wt%、纯金属铬Cr 4.5-6.0wt%、纳米Al2O3或纳米ZrO2 0.3-0.5wt%;
(2)熔炼:将步骤(1)所得的混合料置于中频感应熔炼炉中进行高温熔炼,得高温熔液;所述高温熔炼的温度为1620-1750℃;
(3)喷雾制粉:将步骤(2)所得的高温熔液倾倒至中间包坩埚,通过限流导液管流入喷雾室,在高压高速的氮气作用下进行雾化,将高温熔液冲击破碎成细小金属熔滴,细小金属熔滴在下落冷却过程中表面张力作用下,凝固成复合软磁合金球形或亚球形粉末;
(4)钝化:使用磷酸二氢铝为钝化剂主剂,蒸馏水与丙酮的混合液为稀释剂,对步骤(3)所得的复合软磁合金球形或亚球形粉末进行钝化处理,然后过滤,收集含水粉末,用高压空气吹至半干,得半干粉末;
(5)造粒:将步骤(4)所得的半干粉末烘干,加入改性环氧树脂与酚醛树脂的混合溶液进行造粒,分筛,烘干,冷却至室温,再加入纳米硬脂酸镁为润滑剂,混合均匀,即得细晶粒高绝缘性能复合软磁合金粉末。
2.根据权利要求1所述的细晶粒高绝缘性能复合软磁合金粉末,其特征在于,所述制备方法的步骤(2)中,所述高温熔炼的功率为80-240KW;所述高温熔炼的时间为12-18min;所述高温熔炼的真空度为0.001MPa。
3.根据权利要求1或2所述的细晶粒高绝缘性能复合软磁合金粉末,其特征在于,所述制备方法的步骤(3)中,所述高压为0.4-0.85Mpa;所述雾化的粉末粒度D50为8-15μm。
4.根据权利要求1或2所述的细晶粒高绝缘性能复合软磁合金粉末,其特征在于,所述制备方法的步骤(4)中,钝化剂的加入量为步骤(3)所得复合软磁合金球形或亚球形粉末质量的0.3-0.5wt%。
5.根据权利要求3所述的细晶粒高绝缘性能复合软磁合金粉末,其特征在于,所述制备方法的步骤(4)中,钝化剂的加入量为步骤(3)所得复合软磁合金球形或亚球形粉末质量的0.3-0.5wt%。
6.根据权利要求1或2所述的细晶粒高绝缘性能复合软磁合金粉末,其特征在于,所述制备方法的步骤(4)中,钝化的温度为15-75℃;钝化的时间为20-60min。
7.根据权利要求3所述的细晶粒高绝缘性能复合软磁合金粉末,其特征在于,所述制备方法的步骤(4)中,钝化的温度为15-75℃;钝化的时间为20-60min。
8.根据权利要求4所述的细晶粒高绝缘性能复合软磁合金粉末,其特征在于,所述制备方法的步骤(4)中,钝化的温度为15-75℃;钝化的时间为20-60min。
9.根据权利要求1或2所述的细晶粒高绝缘性能复合软磁合金粉末,其特征在于,所述制备方法的步骤(5)中,所述改性环氧树脂与酚醛树脂的混合溶液的加入量为步骤(4)所得半干粉末的质量的2.0~4.0%。
10.根据权利要求3所述的细晶粒高绝缘性能复合软磁合金粉末,其特征在于,所述制备方法的步骤(5)中,所述改性环氧树脂与酚醛树脂的混合溶液的加入量为步骤(4)所得半干粉末的质量的2.0~4.0%。
11.根据权利要求4所述的细晶粒高绝缘性能复合软磁合金粉末,其特征在于,所述制备方法的步骤(5)中,所述改性环氧树脂与酚醛树脂的混合溶液的加入量为步骤(4)所得半干粉末的质量的2.0~4.0%。
12.根据权利要求6所述的细晶粒高绝缘性能复合软磁合金粉末,其特征在于,所述制备方法的步骤(5)中,所述改性环氧树脂与酚醛树脂的混合溶液的加入量为步骤(4)所得半干粉末的质量的2.0~4.0%。
13.根据权利要求1或2所述的细晶粒高绝缘性能复合软磁合金粉末,其特征在于,所述制备方法的步骤(5)中,所述分筛后的粉末粒径为50-350目;所述烘干的温度为60~80℃;所述烘干的时间为80~100min。
14.根据权利要求3所述的细晶粒高绝缘性能复合软磁合金粉末,其特征在于,所述制备方法的步骤(5)中,所述分筛后的粉末粒径为50-350目;所述烘干的温度为60~80℃;所述烘干的时间为80~100min。
15.根据权利要求4所述的细晶粒高绝缘性能复合软磁合金粉末,其特征在于,所述制备方法的步骤(5)中,所述分筛后的粉末粒径为50-350目;所述烘干的温度为60~80℃;所述烘干的时间为80~100min。
16.根据权利要求6所述的细晶粒高绝缘性能复合软磁合金粉末,其特征在于,所述制备方法的步骤(5)中,所述分筛后的粉末粒径为50-350目;所述烘干的温度为60~80℃;所述烘干的时间为80~100min。
17.根据权利要求9所述的细晶粒高绝缘性能复合软磁合金粉末,其特征在于,所述制备方法的步骤(5)中,所述分筛后的粉末粒径为50-350目;所述烘干的温度为60~80℃;所述烘干的时间为80~100min。
18.根据权利要求1或2所述的细晶粒高绝缘性能复合软磁合金粉末,其特征在于,所述制备方法的步骤(5)中,所述纳米硬脂酸镁的加入量为烘干后的粉末的质量的0.1~0.3wt%。
19.根据权利要求3所述的细晶粒高绝缘性能复合软磁合金粉末,其特征在于,所述制备方法的步骤(5)中,所述纳米硬脂酸镁的加入量为烘干后的粉末的质量的0.1~0.3wt%。
20.根据权利要求4所述的细晶粒高绝缘性能复合软磁合金粉末,其特征在于,所述制备方法的步骤(5)中,所述纳米硬脂酸镁的加入量为烘干后的粉末的质量的0.1~0.3wt%。
21.根据权利要求6所述的细晶粒高绝缘性能复合软磁合金粉末,其特征在于,所述制备方法的步骤(5)中,所述纳米硬脂酸镁的加入量为烘干后的粉末的质量的0.1~0.3wt%。
22.根据权利要求9所述的细晶粒高绝缘性能复合软磁合金粉末,其特征在于,所述制备方法的步骤(5)中,所述纳米硬脂酸镁的加入量为烘干后的粉末的质量的0.1~0.3wt%。
23.根据权利要求13所述的细晶粒高绝缘性能复合软磁合金粉末,其特征在于,所述制备方法的步骤(5)中,所述纳米硬脂酸镁的加入量为烘干后的粉末的质量的0.1~0.3wt%。
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CN109216006A (zh) * | 2018-08-29 | 2019-01-15 | 深圳顺络电子股份有限公司 | 软磁合金粉芯及其制备方法 |
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