CN105839005A - 一种具有涂层的铁铝基磁性材料的制备方法 - Google Patents

一种具有涂层的铁铝基磁性材料的制备方法 Download PDF

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CN105839005A
CN105839005A CN201610199630.5A CN201610199630A CN105839005A CN 105839005 A CN105839005 A CN 105839005A CN 201610199630 A CN201610199630 A CN 201610199630A CN 105839005 A CN105839005 A CN 105839005A
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Abstract

本发明公开了一种具有涂层的铁铝基磁性材料的制备方法，该铁铝基磁性材料由以下原子配比的合金制成：（Fe1‑xAlx）1‑a‑b‑cSiaPrbZrc，其中x=0.15‑0.25，a=0.13‑0.15，b=0.04‑0.06，c=0.02‑0.03。本发明制备的铁铝基磁性材料，采用Pr替代部分Fe，采用的Zr可提高材料的非晶形成能力。本发明通过采用涂层方式，调节涂层中的纳米锰锌铁氧体粉和内部铁铝基磁性材料的偶合作用，能够大幅提高软磁合金的饱和磁化强度，同时能够保持较低的矫顽力。

Description

一种具有涂层的铁铝基磁性材料的制备方法
技术领域
本发明涉及磁性材料制造领域，具体涉及一种具有涂层的铁铝基磁性材料的制备方法。
背景技术
铁基纳米晶软磁合金材料自问世以来，因具有高饱和磁感应强度、高磁导率、低损耗、低矫顽力等特点而得到极大的重视和深入的研究，并广泛应用于开关电源和电磁传感器等领域。
铁硅铝磁粉芯具有优秀的性价比，但是其抗磁饱和能力和铁硅磁粉芯相比有较大的差距，而这又随着器件小型化的迫切要求更显得矛盾突出。此外，目前铁硅铝磁粉芯的发展趋势是追求制备出同时拥有高导磁率和低损耗的金属软磁粉芯，要想达到这个目标，其中原材料粉末至关重要，粉末的元素成份配置、粒度分布等物理化学性能对软磁制品的磁性能影响很大。
发明内容
本发明提供一种具有涂层的铁铝基磁性材料的制备方法，该铁铝基磁性材料，具有优异的软磁性能及高磁感应强度。
为了实现上述目的，实现上述目的，本发明提供了一种具有涂层的铁铝基磁性材料的制备方法，该铁铝基磁性材料由以下原子配比的合金制成：（Fe1-xAlx）1-a-b-cSiaPrbZrc，其中x=0.15-0.25，a=0.13-0.15，b=0.04-0.06，c=0.02-0.03
该方法包括如下步骤：
（1）制备合金
首先按照上述重量百分含量进行配料，所有原料的纯度均大于99.9％，其中，Pr以铁镨合金的方式加入，铁镨合金中Pr的重量百分比为25%；
将原料分别放入高频感应熔炼炉中，抽真空至5×10-3Pa，充入适量氩气作为保护气体，调节电流至5-8安培，待原料完全熔化后，再熔炼10-20分钟，熔炼温度为1510-1530℃，浇注冷却后得到母合金；
将所述母合金放入重熔管式坩埚中进行重熔，重熔温度为1500-1510℃；所述重熔管式坩埚放入真空感应成型炉内，其顶部置于真空感应成型炉转轮轮缘之下2-4mm处，所述重熔管式坩埚内放置一个可上下移动的耐火柱塞，该耐火柱塞和管式坩埚内壁的间隙为1-2mm，所述母合金置于重熔管式坩埚内的耐火柱塞顶面熔化，熔化后被转轮轮缘拖拽形成合金丝，其中真空成型炉转轮轮缘的旋转线速度为25-27m/s，所得合金丝的直径为100-200微米；
（2）热处理
将合金丝在热处理炉中并在高真空条件下，在420℃-550℃下热处理30-60min，再淬火至室温，得到热处理后的铁铝基磁性材料；
（3）制备具有涂层的软磁合金材料
在装有搅拌器的三口烧瓶中按比例加入正硅酸乙酯、γ-甲基丙烯酰氧基丙基三甲氧基硅烷和乙醇，其摩尔比为3:2:2；在搅拌下滴入醋酸，加入量为5g/100mL，室温反应3h后，加入甲基丙烯酸甲酯和引发剂偶氮二异丁腈，加入量分别为10g/100mL和5g/100mL，然后室温下搅拌20min得到溶胶待用；然后将市售的粒度为50-100nm的锰锌铁氧体粉和溶胶混合得到涂料，锰锌铁氧体粉和溶胶的重量比为6:0.4-0.6；
然后将上述涂料涂抹到上述热处理后的铁铝基磁性材料上，涂层厚度为3-5微米；经15min烘烤固化，烘烤温度为130℃，得到具有涂层的铁铝基磁性材料材料。
本发明制备的铁铝基磁性材料，采用Pr替代部分Fe，采用的Zr可提高材料的非晶形成能力。本发明通过采用涂层方式，调节涂层中的纳米锰锌铁氧体粉和内部铁铝基磁性材料的偶合作用，能够大幅提高软磁合金的饱和磁化强度，同时能够保持较低的矫顽力。
具体实施方式
实施例一
本实施例的铁铝基磁性材料由以下原子配比的合金制成：（Fe0.85Al0.15）0.81Si0.13Pr0.04Zr0.02。
首先按照上述重量百分含量进行配料，所有原料的纯度均大于99.9％，其中，Pr以铁镨合金的方式加入，铁镨合金中Pr的重量百分比为25%。
将原料分别放入高频感应熔炼炉中，抽真空至5×10-3Pa，充入适量氩气作为保护气体，调节电流至5安培，待原料完全熔化后，再熔炼10分钟，熔炼温度为1510℃，浇注冷却后得到母合金。
将所述母合金放入重熔管式坩埚中进行重熔，重熔温度为1500℃；所述重熔管式坩埚放入真空感应成型炉内，其顶部置于真空感应成型炉转轮轮缘之下2-4mm处，所述重熔管式坩埚内放置一个可上下移动的耐火柱塞，该耐火柱塞和管式坩埚内壁的间隙为1-2mm，所述母合金置于重熔管式坩埚内的耐火柱塞顶面熔化，熔化后被转轮轮缘拖拽形成合金丝，其中真空成型炉转轮轮缘的旋转线速度为25m/s，所得合金丝的直径为100微米。
将合金丝在热处理炉中并在高真空条件下，在420℃下热处理30min，再淬火至室温，得到热处理后的铁铝基磁性材料。
在装有搅拌器的三口烧瓶中按比例加入正硅酸乙酯、γ-甲基丙烯酰氧基丙基三甲氧基硅烷和乙醇，其摩尔比为3:2:2；在搅拌下滴入醋酸，加入量为5g/100mL，室温反应3h后，加入甲基丙烯酸甲酯和引发剂偶氮二异丁腈，加入量分别为10g/100mL和5g/100mL，然后室温下搅拌20min得到溶胶待用；然后将市售的粒度为50-100nm的锰锌铁氧体粉和溶胶混合得到涂料，锰锌铁氧体粉和溶胶的重量比为6:0.4。
然后将上述涂料涂抹到上述热处理后的铁铝基磁性材料上，涂层厚度为3微米；经15min烘烤固化，烘烤温度为130℃，得到具有涂层的铁铝基磁性材料材料。
实施例二
本实施例的铁铝基磁性材料由以下原子配比的合金制成：（Fe0.75Al0.25）0.76Si0.15Pr0.06Zr0.03。
首先按照上述重量百分含量进行配料，所有原料的纯度均大于99.9％，其中，Pr以铁镨合金的方式加入，铁镨合金中Pr的重量百分比为25%。
将原料分别放入高频感应熔炼炉中，抽真空至5×10-3Pa，充入适量氩气作为保护气体，调节电流至8安培，待原料完全熔化后，再熔炼20分钟，熔炼温度为1530℃，浇注冷却后得到母合金。
将所述母合金放入重熔管式坩埚中进行重熔，重熔温度为1510℃；所述重熔管式坩埚放入真空感应成型炉内，其顶部置于真空感应成型炉转轮轮缘之下2-4mm处，所述重熔管式坩埚内放置一个可上下移动的耐火柱塞，该耐火柱塞和管式坩埚内壁的间隙为1-2mm，所述母合金置于重熔管式坩埚内的耐火柱塞顶面熔化，熔化后被转轮轮缘拖拽形成合金丝，其中真空成型炉转轮轮缘的旋转线速度为27m/s，所得合金丝的直径为200微米。
将合金丝在热处理炉中并在高真空条件下，在550℃下热处理60min，再淬火至室温，得到热处理后的铁铝基磁性材料。
在装有搅拌器的三口烧瓶中按比例加入正硅酸乙酯、γ-甲基丙烯酰氧基丙基三甲氧基硅烷和乙醇，其摩尔比为3:2:2；在搅拌下滴入醋酸，加入量为5g/100mL，室温反应3h后，加入甲基丙烯酸甲酯和引发剂偶氮二异丁腈，加入量分别为10g/100mL和5g/100mL，然后室温下搅拌20min得到溶胶待用；然后将市售的粒度为50-100nm的锰锌铁氧体粉和溶胶混合得到涂料，锰锌铁氧体粉和溶胶的重量比为6: 0.6。
然后将上述涂料涂抹到上述热处理后的铁铝基磁性材料上，涂层厚度为3-5微米；经15min烘烤固化，烘烤温度为130℃，得到具有涂层的铁铝基磁性材料材料。
比较例
将铁和铝丝以及单晶硅熔配为合金，将熔配好的合金放入真空室的底部有孔的石英试管中，循环三次抽真空和反充入高纯Ar气；采用高频电磁方法加热熔配合金，再将Ar气充入石英试管将熔融态样品吹至旋转的转轮上成合金薄带；将所得合金薄带在Ar气保护下在400℃条件下保温1小时，然后随炉冷却至室温下出炉。将纯度99.8％的铁和99.98％的镍丝在有高纯Ar气保护下熔配为Fe-Al合金，样品质量2.5克，控制其中Fe的含量在77-79wt％。
对相同形状和尺寸的实施例1-2及比较例的铁芯进行磁性能测试，在25℃进行测试，（1）合金的矫顽力采用KM-Ot ype List-Koerzimeter矫顽力仪测量；（2）合金的饱和磁感应强度Bs采用静态磁性能测量仪，以磁场为800A/m下的磁感应强度作为合金的饱和磁感应强度Bs。测试结果显示：实施例1-2的矫顽力相对比较例降低42%以上，饱和磁感应强度相对比较例提高29%以上。

Claims (1)

1.一种具有涂层的铁铝基磁性材料的制备方法，该铁铝基磁性材料由以下原子配比的合金制成：（Fe1-xAlx）1-a-b-cSiaPrbZrc，其中x=0.15-0.25，a=0.13-0.15，b=0.04-0.06，c=0.02-0.03
该方法包括如下步骤：
（1）制备合金
首先按照上述重量百分含量进行配料，所有原料的纯度均大于99.9％，其中，Pr以铁镨合金的方式加入，铁镨合金中Pr的重量百分比为25%；
将原料分别放入高频感应熔炼炉中，抽真空至5×10-3Pa，充入适量氩气作为保护气体，调节电流至5-8安培，待原料完全熔化后，再熔炼10-20分钟，熔炼温度为1510-1530℃，浇注冷却后得到母合金；
将所述母合金放入重熔管式坩埚中进行重熔，重熔温度为1500-1510℃；所述重熔管式坩埚放入真空感应成型炉内，其顶部置于真空感应成型炉转轮轮缘之下2-4mm处，所述重熔管式坩埚内放置一个可上下移动的耐火柱塞，该耐火柱塞和管式坩埚内壁的间隙为1-2mm，所述母合金置于重熔管式坩埚内的耐火柱塞顶面熔化，熔化后被转轮轮缘拖拽形成合金丝，其中真空成型炉转轮轮缘的旋转线速度为25-27m/s，所得合金丝的直径为100-200微米；
（2）热处理
将合金丝在热处理炉中并在高真空条件下，在420℃-550℃下热处理30-60min，再淬火至室温，得到热处理后的铁铝基磁性材料；
（3）制备具有涂层的软磁合金材料
在装有搅拌器的三口烧瓶中按比例加入正硅酸乙酯、γ-甲基丙烯酰氧基丙基三甲氧基硅烷和乙醇，其摩尔比为3:2:2；在搅拌下滴入醋酸，加入量为5g/100mL，室温反应3h后，加入甲基丙烯酸甲酯和引发剂偶氮二异丁腈，加入量分别为10g/100mL和5g/100mL，然后室温下搅拌20min得到溶胶待用；然后将市售的粒度为50-100nm的锰锌铁氧体粉和溶胶混合得到涂料，锰锌铁氧体粉和溶胶的重量比为6:0.4-0.6；
然后将上述涂料涂抹到上述热处理后的铁铝基磁性材料上，涂层厚度为3-5微米；经15min烘烤固化，烘烤温度为130℃，得到具有涂层的铁铝基磁性材料材料。
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