CN109680210B - 一种μ=150～250铁硅铝软磁磁粉芯的制备方法 - Google Patents
一种μ=150～250铁硅铝软磁磁粉芯的制备方法 Download PDFInfo
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Abstract
本发明利用FeSiAl磁粉，通过粉末的粒度配比、粉末、磁芯退火处理及绝缘包覆等工艺，来实现高磁导率铁硅铝软磁磁粉芯的制备。使用本方法制备得到的铁硅铝软磁磁粉芯的磁导率μe＝150‑250(10kHz‑1MHz)，25℃时该磁粉芯的功率损耗在500‑800kW/m3以下(测试条件：100kHz/100mT)，达到国际领先水平。
Description
技术领域
本发明涉及软磁材料技术领域，是在滤波电感中应用的一种高磁导率μ＝150-250铁硅铝合金磁粉芯的制备方法。
背景技术
金属软磁磁粉芯具有高饱和磁感应强度、高居里温度和高DC-bias等优点，被广泛应用于10kHz-200kHz频率的开关电源中，用于滤波电感。铁硅铝磁粉芯具有高频低损耗、低磁致伸缩系数(噪音小)等优点，破碎式的铁硅铝成本低，具有很大的市场容量。但目前可量产的铁硅铝磁粉芯最高磁导率仅有125，有部分文献专利报到磁导率也只有150以下。目前可以做高磁导率金属磁粉芯(≥160)只有铁镍、铁镍钼材料，但这两种材料价格昂贵，市场需求小；开发出高磁导率铁硅铝磁粉芯，拥有很大市场前景。
专利号CN104361968A的发明专利公开了一种高磁导率FeSiAl软磁合金粉芯的制造方法，采用非真空中频感应炉，将铁硅铝合金铸锭经机械破碎成粉末，退火处理，筛分，按不同粒度配比组成铁硅铝合金粉末，将所述铁硅铝合金粉末进行绝缘处理，添加脱模剂后模压成型制成磁粉芯；再将产品进行热处理，表面绝缘喷涂，得到铁硅铝磁粉芯。本发明所述方法成本低、操作方便，所述磁粉芯性能良好，磁导率高，高频损耗低。但其磁粉芯磁导率仅是147左右，相比于传统FeSiAl磁粉芯是属于高磁导率。
专利号CN107424708A的发明专利公开了利用气雾化铁硅铝磁粉，开发出磁导率40-80，损耗250-350mW/cm3(100kHz，100mT)的FeSiAl磁粉芯，气雾化FeSiAl磁粉芯虽然损耗较好，但磁导率也比较低，不能满足一些需求高磁导率磁芯的滤波电感。
专利号CN104575911B的发明专利公开了高磁导率铁镍钼磁粉芯的制备方法；选取水雾化铁镍钼粉；成膜处理；绝缘处理；添加耐高温粘结剂，制备出磁导率达到190的铁镍钼磁粉芯。由于铁镍钼价格昂贵，是铁硅铝的7倍左右，因此开发出高磁导率的FeSiAl磁粉芯具有更大的市场价值。
发明内容
本发明的目的是为了解决现有磁粉芯磁导率偏低不能满足一些需求高磁导率磁芯的缺陷而提供一种高磁导率及直流叠加性能，很低的功率损耗的μ＝150～250铁硅铝软磁磁粉芯的制备方法。
为了实现上述目的，本发明采用以下技术方案：
一种μ＝150～250铁硅铝软磁磁粉芯的制备方法，所述制备方法包括以下步骤：
(1)采用机械破碎式FeSiAl粉末；
(2)粉末退火：磁粉放入退火炉中，通入保护气体，温度控制在700℃～900℃，热处理0.5～6h；
(3)绝缘包覆：把退火后的FeSiAl磁粉加入到磷酸溶液中进行钝化，烘至干燥后，再加入辅料，辅料用量是磁粉的0.01-0.5％，继续烘至干燥，后续加入有机硅胶水溶于有机溶剂中，烘至干燥；
(4)压制成型：成型压力为16～22吨/cm2；
(5)磁芯热处理：在保护气体下退火，温度为600℃～850℃，保温20～120min；
(6)表面涂层：磁粉芯表面用环氧树脂喷涂。
作为优选，步骤(1)中粉末0.001％＜C＜0.03％，0.001＜O＜0.2％，0.001＜N＜0.2％， 7.5％＜Si＜12.5％，3.5＜Al＜8.5％，余量为铁。
作为优选，粉末粒度：D99＜160um，20um＜D50＜80um。
作为优选，步骤(3)磷酸溶液中，磷酸用量占粉末重量是0.01-0.5％，溶剂选择水、丙酮、酒精中一种或多种溶剂。
作为优选，步骤(3)中，辅料为高岭土、云母粉、氢氧化镁、氢氧化铝、氧化钙、硅酸钠、硅酸钾、氧化钙中一种或多种混合。
作为优选，步骤(2)与步骤(5)中，保护气体所用的气体为氮气、氢气、氩气中一种或多种混合气体。
作为优选，步骤(4)压制成型时加入磁粉重量0.1％～0.8％的脱模剂。
作为优选，所述脱模剂为硬脂酸盐、滑石粉、二硫化钼中的一种或几种。
本发明具有以下优点：1)设备及工艺简单，成本低；2)产品具有高磁导率及直流叠加性能，很低的功率损耗；3)使用有机粘结剂，提高磁粉芯热处理温度，提升磁性能。
附图说明
图1是170u/200u铁硅铝磁粉芯直流叠加性能图。
图2是170u/200u铁硅铝磁粉芯损耗性能。
图中，a.DS200u；b.DS170u；c.DS170u-50kHz；d.DS170u-100kHz；e.DS200u-50kHz；f.DS200u-100kHz。
具体实施方式
下面结合实施例对本发明作进一步详细的描述，但本发明的实施方式不限于此。
实施例1
一种μ＝150～250铁硅铝软磁磁粉芯的制备方法，取铁硅铝磁粉，C：0.008％，N：0.01％，O：0.08％，Si：9.5％，Al：5.5％，余量为铁，粉末粒度D99＝158um，D50＝68um，原粉在纯氮气气氛800℃退火6h；再加入0.012％磷酸水溶液，炒至完全干燥；再加入0.1％氢氧化镁、0.1％硅酸钠混合水溶液，炒至完全干燥；加入0.3％高温有机硅胶水丙酮溶液，烘干至完全干燥，最后加入磁粉重量的0.3％的硬脂酸锌作为脱模剂，混合均匀后，压制成20.3mm*12.7mm*6.35mm的磁环，成型压力位18.5t/cm2；将成型后的磁芯在氮气气氛下，700℃保温50min进行热处理；冷却后在磁芯表面喷涂环氧树脂，固化后得到μ＝246铁硅铝磁粉芯。经检测，得到的铁硅铝磁粉芯的磁性能如表1所示。
实施例2
一种μ＝150～250铁硅铝软磁磁粉芯的制备方法，取铁硅铝磁粉，C：0.012％，N：0.05％， O：0.2％，Si：9.0％，Al：5.1％，余量为铁，粉末粒度D99＝147um，D50＝60um，原粉在纯氢气气氛700℃退火0.5h；再加入0.1％磷酸酒精溶液，炒至完全干燥；再加入质量分数为0.3％高岭土、0.2％云母粉混合水溶液，炒至完全干燥；加入质量分数为0.5％高温有机硅胶水甲苯溶液，烘干至完全干燥，最后加入磁粉重量的0.5％的硬脂酸铝作为脱模剂，混合均匀后，压制成20.3mm*12.7mm*6.35mm的磁环，成型压力位20.5t/cm2；将成型后的磁芯在氮气气氛下， 850℃保温30min进行热处理；冷却后在磁芯表面喷涂环氧树脂，固化后得到μ＝203铁硅铝磁粉芯。经检测，得到的铁硅铝磁粉芯的磁性能如表1所示。
实施例3
一种μ＝150～250铁硅铝软磁磁粉芯的制备方法，取铁硅铝磁粉，C：0.03％，N：0.2％，O：0.05％， Si：7.5％，A1：8.5％，余量为铁，粉末粒度D99＝145um，D50＝63um，原粉在纯氩气气氛900℃退火0.5h；再加入0.5％磷酸丙酮溶液，炒至完全干燥；再加入质量分数为0.2％氢氧化铝、 0.2％硅酸钾混合水溶液，炒至完全干燥；加入质量分数为0.8％高温有机硅胶水丙酮溶液，烘干至完全干燥，最后加入磁粉重量的0.1％的二硫化钼作为脱模剂，混合均匀后，压制成 20.3mm*12.7mm*6.35mm的磁环，成型压力位16t/cm2；将成型后的磁芯在氩气气氛下，600℃保温120min进行热处理；冷却后在磁芯表面喷涂环氧树脂，固化后得到μ＝183铁硅铝磁粉芯。经检测，得到的铁硅铝磁粉芯的磁性能如表1所示。
实施例4
一种μ＝150～250铁硅铝软磁磁粉芯的制备方法，取铁硅铝磁粉，C：0.006％，N：0.02％， O：0.15％，Si：12.5％，Al：3.5％，余量为铁，粉末粒度D99＝138um，D50＝59um，原粉在氮氢混合气氛850℃退火1h；再加入0.2％磷酸丙酮溶液，炒至完全干燥；再加入质量分数为0.1％氧化钙水、0.3％硅酸钾溶液，炒至完全干燥；加入质量分数为0.1％高温有机硅胶水二甲苯溶液，烘干至完全干燥，最后加入磁粉重量的0.4％的硬脂酸铝作为脱模剂，混合均匀后，压制成20.3mm*12.7mm*6.35mm的磁环，成型压力位18t/cm2；将成型后的磁芯在氮气气氛下， 680℃保温60min进行热处理；冷却后在磁芯表面喷涂环氧树脂，固化后得到μ＝176铁硅铝磁粉芯。经检测，得到的铁硅铝磁粉芯的磁性能如表1所示。
实施例5
一种μ＝150～250铁硅铝软磁磁粉芯的制备方法，取铁硅铝磁粉，C：0.011％，N：0.08％， O：0.18％，Si：8.5％，Al：6.5％，余量为铁，粉末粒度D99＝116um，D50＝46um，原粉在氮气混合气氛750℃退火1.5h；再加入0.15％磷酸酒精溶液，炒至完全干燥；再加入质量分数为0.2％高岭土干粉充分混合均匀；加入质量分数为0.4％高温有机硅胶水丙酮溶液，烘干至完全干燥，最后加入磁粉重量的0.1％的滑石粉和0.2％硬脂酸铝作为脱模剂，混合均匀后，压制成 20.3mm*12.7mm*6.35mm的磁环，成型压力位19.5t/cm2；将成型后的磁芯在氩氢混合气保护下，760℃保温40min进行热处理；冷却后在磁芯表面喷涂环氧树脂，固化后得到μ＝152铁硅铝磁粉芯。经检测，得到的铁硅铝磁粉芯的磁性能如表1所示。
表1实施例磁粉芯性能
磁导率170、200铁硅铝磁粉芯的性能见图1与图2。
Claims (7)
1.一种μ＝150～250铁硅铝软磁磁粉芯的制备方法，其特征在于，所述制备方法包括以下步骤：
（1）采用机械破碎式FeSiAl粉末；
（2）粉末退火：磁粉放入退火炉中，通入保护气体，温度控制在700℃～900℃，热处理0.5～6h；
（3）绝缘包覆：把退火后的FeSiAl磁粉加入到磷酸溶液中进行钝化，烘至干燥后，再加入辅料，辅料用量是磁粉的0.01-0.5％，继续烘至干燥，后续加入有机硅胶水溶于有机溶剂中，烘至干燥；辅料为高岭土、云母粉、氢氧化镁、氢氧化铝、氧化钙、硅酸钠、硅酸钾、氧化钙中一种或多种混合；
（4）压制成型：成型压力为16～22吨/cm2；
（5）磁芯热处理：在保护气体下退火，温度为600℃～850℃，保温20～120min；
（6）表面涂层：磁粉芯表面用环氧树脂喷涂。
2.根据权利要求1所述的一种μ＝150～250铁硅铝软磁磁粉芯的制备方法，其特征在于，步骤（1）中粉末0.001％＜C＜0.03％，0.001＜O＜0.2％，0.001＜N＜0.2％，7.5％＜Si＜12.5％，3.5＜Al＜8.5％，余量为铁。
3.根据权利要求1所述的一种μ＝150～250铁硅铝软磁磁粉芯的制备方法，其特征在于，粉末粒度：D99＜160um，20um＜D50＜80um。
4.根据权利要求1所述的一种μ＝150～250铁硅铝软磁磁粉芯的制备方法，其特征在于，步骤（3）磷酸溶液中，磷酸用量占粉末重量是0.01-0.5％，溶剂选择水、丙酮、酒精中一种或多种溶剂。
5.根据权利要求1所述的一种μ＝150～250铁硅铝软磁磁粉芯的制备方法，其特征在于，步骤（2）与步骤（5）中，保护气体所用的气体为氮气、氢气、氩气中一种或多种混合气体。
6.根据权利要求1所述的一种μ＝150～250铁硅铝软磁磁粉芯的制备方法，其特征在于，步骤（4）压制成型时加入磁粉重量0.1％～0.8％的脱模剂。
7.根据权利要求6所述的一种μ＝150～250铁硅铝软磁磁粉芯的制备方法，其特征在于，所述脱模剂为硬脂酸盐、滑石粉、二硫化钼中的一种或几种。
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| CN106409461A (zh) * | 2016-08-31 | 2017-02-15 | 北京康普锡威科技有限公司 | 一种低损耗FeSi6.5软磁复合粉芯的制备方法 |
| CN107256753A (zh) * | 2017-07-28 | 2017-10-17 | 青岛云路先进材料技术有限公司 | 高效能铁硅铝粉末的制备和筛选方法 |
| CN107578873A (zh) * | 2017-09-12 | 2018-01-12 | 横店集团东磁股份有限公司 | 一种磁导率μ=400的铁镍钼金属磁粉芯的制备方法 |
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