CN113878124A - 一种铁硅铬镓铟氮合金软磁粉末的水气联合雾化制备方法 - Google Patents
一种铁硅铬镓铟氮合金软磁粉末的水气联合雾化制备方法 Download PDFInfo
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Abstract
本发明涉及一种铁硅铬镓铟氮合金软磁粉末的水气联合雾化制备方法，包括如下步骤：1）将含有铁、硅、铬、镓、铟的软磁合金粉末原料加入中频感应炉内，采用吹氩保护冶炼得到合金液；2）在氮气保护条件下，将合金液浇注入负压环境的雾化塔内，通过负压超速气体和高压氨水溶液两种介质先后作用于合金液柱流，合金液柱流先在负压超音速气体作用下，被分散撕裂成金属液滴，然后再通过高压氨水溶液的冲击和冷却，将金属液滴进一步破碎冷却呈近球形的合金软磁粉末，同时使得合金软磁粉末表面形成致密的氧化膜和氮化膜。此方法可以制备高振实密度，高表面电阻率，高损耗特性的合金软磁粉末，作为电感器件的粉末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技术领域，更具体地说是指一种铁硅铬镓铟氮合金软磁粉末的水气联合雾化制备方法。
背景技术
目前，金属软磁粉末通常是以铁硅铬为主，采用化学反应法、熔体雾化法、机械破碎法和点解沉积法等制备方法制成，其中，熔体雾化法制备合金粉末拥有与既定熔融合金完全相同的化学成分，还具有典型的快速凝固组织，合金成分范围宽，粉末形貌球形度好，粒度分布宽的特点，被广泛的应用当下金属软磁粉末制作。
但是，随着科技的发展，电子元器件的应用越来越广，且随着产品性能的提高，对电子元器件所用的磁性材料要求越来越高，特别是针对不同电子产品其功能不同，对金属软磁粉末的材料性质要求也不同，如部分电感器件对软磁材料需要较强电阻率、耐电性、防锈性和耐损耗，而通过上述熔体雾化法制取的铁硅铬软磁粉末，其存在粉末振实密度低、电阻率低、耐电性差、防锈性和耐损耗低等缺陷，无法满足客户实际需求。
发明内容
本发明提供一种铁硅铬镓铟氮合金软磁粉末的水气联合雾化制备方法，以解决现有金属软磁粉末存在的振实密度低、电阻率低、耐电性差、防锈性和耐损耗低等缺陷。
本发明采用如下技术方案：
一种铁硅铬镓铟氮合金软磁粉末的水气联合雾化制备方法，包括如下步骤：
1）将含有铁、硅、铬、镓、铟的软磁合金粉末原料加入中频感应炉内，采用吹氩保护冶炼得到合金液。
2）在氮气保护条件下，将合金液浇注入负压环境的雾化塔内，浇注过程中，通过负压超速气体和高压氨水溶液两种介质先后作用于合金液柱流，合金液柱流先在负压超音速气体作用下，被分散撕裂成金属液滴，并在负压超音速气体下得到初步冷凝，初步冷凝中镓铟两种元素在金属液滴表面富集，然后再通过高压氨水溶液的冲击和冷却，将金属液滴进一步破碎冷却呈近球形的合金软磁粉末，同时使得合金软磁粉末表面形成致密的氧化膜和氮化膜。
上述，最终制成的合金软磁粉末质量比为：铬0.1-10%，硅2-8%，镓0.1-2%，铟0.1-2%，氮0.01-0.5%，铁余量。
进一步地，所述1）冶炼过程中，在预制坩埚中，底部预埋气砖，中频感应炉炉口用炉盖封闭，用氩气作为炉口保护气体。冶炼合金液时，先将铁、铬、硅按顺序先后加入中频感应炉完全熔化，在温度达到1580-1600度时，开始炉底吹氩；在温度达到1640-1660度时，开启炉口吹氩，随后加入镓、铟；镇静除渣后，得到合金液。
进一步地，所述步骤2）雾化塔的雾化桶加装变频低压引风机、压力传感器、单向阀、定向管道、冷凝器和导流板，通过压力传感器和变频低压引风机将雾化桶内压力维持在98-99KPa压力条件下，将合金液浇注入负压环境的雾化塔内，雾化桶内用氮气作为保护气氛，氮气流量在10-20M3/H，氮气通过变频低压引风机、定向管道、冷凝器和导流板在雾化桶内高速定向流动，形成负压超音速气体，将合金液柱流分散撕裂成金属液滴。
进一步地，浇注过程中漏包采用氩气保护，漏眼直径4-6毫米。
进一步地，上述负压超音速气体的压力为0.1-10KPa，速度为1—5马赫。
进一步地，所述高压氨水溶液的喷射压力120-200MPa，流量为150-350L/min。
进一步地，所述高压氨水溶液的氨水溶液浓度为0.5-2%。
进一步地，所述步骤2）雾化过程中产生的气体和雾化桶内的氮气一起被变频低压引风机排出雾化桶，并导入低浓度磷酸溶液中做无害化处理。
由上述对本发明结构的描述可知，和现有技术相比，本发明具有如下优点：
1、 本发明合金软磁粉末原料中含有镓铟，这两种元素本身熔点低，可以明显降低铁硅铬合金的熔点，提高合金液的流动性，降低合金液的粘度，利于粉末的球化，提高合金软磁粉末的振实密度。其次，由于粉末快冷过程的温度梯度变化，能够使得镓铟会偏析并在金属液滴表面富集，再在高压氨水溶液的冲击和冷却时，富集在金属液滴表面的镓铟会与氨水中氨反应，生产部分氮化铟和氮化镓，而粉体表面大量富集了的氮化铟和氮化镓，会与粉末表面的氧化硅、氧化铬、氧化铁共同形成了较为致密的氧化膜和氮化膜。该致密的氧化膜和氮化膜能够明显提高合金软磁粉末表面的电阻率，明显提升改善了合金软磁粉末在软磁电感器件应用中的耐电压特性和防锈性，改善了粉体表面电阻的非线性伏安特性，同时由于镓、铟、氮化镓、氮化铟对合金的改性，明显改善了高频大功率使用条件下的损耗特性。
2、本发明不同传统雾化法的气体吹散合金液柱流，而是采用负压环境下通过负压超音速气体作用将合金液柱流分散撕裂成金属液滴，避免了传统正压气体吹击金属液滴表面，影响镓铟在金属液滴表面分布，有利于镓铟在金属液滴表面富集。
具体实施方式
下面说明本发明实施例的具体实施方式。
一种铁硅铬镓铟氮合金软磁粉末的水气联合雾化制备方法，包括如下步骤:
1) 将含有铁、硅、铬、镓、铟的软磁合金粉末原料加入中频感应炉内，采用吹氩保护冶炼得到合金液。
进一步，在冶炼过程中，在预制坩埚中，底部预埋气砖，中频感应炉的炉口用炉盖封闭，用氩气作为炉口保护气体。冶炼时，先将铁、铬、硅按顺序先后加入中频感应炉完全熔化，在温度达到1580-1600度时，开始炉底吹氩；在温度达到1640-1660度时，开启炉口吹氩，随后加入镓、铟；镇静除渣后，得到合金液。
上述冶炼中，镓、铟两种元素因容易氧化，在熔炼过程中，要往相对靠后的顺序加入，并且在加入的过程中通过氩气和炉盖保护，以降低冶炼过程中镓、铟的氧化，降低合金液中的氧化物杂质。
2）在氮气保护条件下，将合金液浇注入负压环境的雾化塔内，浇注过程中，通过负压超速气体和高压氨水溶液两种介质先后作用于合金液柱流，合金液柱流先在负压超音速气体作用下，被分散撕裂成金属液滴，并在负压超音速气体下得到初步冷凝，初步冷凝中镓铟两种元素在金属液滴表面富集，然后再通过高压氨水溶液的冲击和冷却，将金属液滴进一步破碎冷却呈近球形的合金软磁粉末，同时使得合金软磁粉末表面形成致密的氧化膜和氮化膜。制成的软磁合金粉末原料质量比为：铬0.1-10%，硅2-8%，镓0.1-2%，铟0.1-2%，氮0.01-0.5%，铁余量。
更具体的，雾化塔的雾化桶加装变频低压引风机、压力传感器、单向阀、定向管道、冷凝器和导流板，通过压力传感器和变频低压引风机将雾化桶内压力维持在98-99KPa压力条件下。将合金液浇注入负压环境的雾化塔内，雾化桶内用氮气作为保护气氛，氮气流量控制在在10-20M3/H。浇注过程中漏包采用氩气保护，漏眼直径4-6毫米，氮气作为破碎气体，通过变频低压引风机、定向管道、冷凝器和导流板在雾化桶内高速定向流动，没有涡旋，降低了涡旋产生的能量损耗，形成负压超音速气体，作为优选负压超音速气体的压力控制在0.1-10KPa，速度控制在1—5马赫。合金液柱流在负压超音速气体作用下，通过改变气体速度和压力，利用气体压力从高到低、再从低到高，气体体积压缩膨胀的快速变化，将合金液柱流分散撕裂成金属液滴。然后再通过高压氨水溶液的冲击和冷却，将金属液滴进一步破碎冷却成近球形的合金软磁粉末，由此，得到本发明金属软磁粉末颗粒。作为优选，高压氨水溶液的喷射压力控制在120-200MPa；流量控制在150-350L/min，氨水溶液浓度为0.5-2%。
本发明制得的合金软磁粉末相较于传统的铁硅铬软磁粉末，由于镓铟两种元素本身熔点低，可以明显降低铁硅铬合金的熔点，提高合金液的流动性，降低合金液的粘度，利于粉末的球化，提高合金软磁粉末的振实密度。并且，由于雾化制粉破碎凝固的快冷过程中粉末从核心到表面，它是有一个温度梯度变化的，不同元素冷却的速度是不一样的，就会造成熔点低的金属元素形成表面富集，因此在合金液柱流被分散撕裂成金属液滴时，镓铟会偏析并在金属液滴表面富集。此外，本发明不同传统雾化法的气体吹散合金液柱流，而是采用负压环境下通过负压超音速气体作用将合金液柱流分散撕裂成金属液滴，避免了传统正压气体吹击金属液滴表面，影响镓铟在金属液滴表面分布，有利于镓铟在金属液滴表面富集。
然后，在高压氨水溶液的冲击和冷却过程中，富集在金属液滴表面的镓铟会和氨水中的氨反应，生产部分氮化铟和氮化镓，同时由于粉末表面和核心冷却速度差异，粉体表面大量富集了氮化铟和氮化镓，氮化铟和氮化镓与粉末表面的氧化硅、氧化铬、氧化铁共同形成了较为致密的氧化膜和氮化膜。雾化过程中产生的氢气和氨气，会与雾化桶内的氮气保护气一起，被变频低压引风机排出雾化桶，导入到低浓度磷酸溶液中做无害化处理。
综上，本发明所制备的合金软磁粉末相较于传统的铁硅铬软磁粉末，由于粉体表面形成了上述致密的氧化膜和氮化膜，从而明显提高了合金软磁粉末表面的电阻率，明显提升改善了合金软磁粉末在软磁电感器件应用中的耐电压特性和防锈性，改善了粉体表面电阻的非线性伏安特性，同时由于镓、铟、氮化镓、氮化铟对合金的改性，明显改善了高频大功率使用条件下的损耗特性。
经检测，下面为本发明所制制成的产品B与现有雾化法制成的铁硅铬产品A的材料性能对比表。
| 品名 | 电压V | 压强Mpa | 电阻Ω | 电导率S/mm | 电阻率Ω.mm | 高度mm | 压实密度g/cm3 |
| A | 0.054081 | 25.01 | 54.0805 | 6.28E-04 | 1591.2 | 2.66 | 3.829292 |
| B | 1.08943 | 25.05 | 10894.3 | 3.76E-07 | 266169 | 3.20 | 3.97887 |
上述仅为本发明的具体实施方式，但本发明的设计构思并不局限于此，凡利用此构思对本发明进行非实质性的改动，均应属于侵犯本发明保护范围的行为。
Claims (10)
1.一种铁硅铬镓铟氮合金软磁粉末的水气联合雾化制备方法，其特征在于，包括如下步骤：
1）将含有铁、硅、铬、镓、铟的软磁合金粉末原料加入中频感应炉内，采用吹氩保护冶炼得到合金液；
2）在氮气保护条件下，将合金液浇注入负压环境的雾化塔内，浇注过程中，通过负压超速气体和高压氨水溶液两种介质先后作用于合金液柱流，合金液柱流先在负压超音速气体作用下，被分散撕裂成金属液滴，并在负压超音速气体下得到初步冷凝，初步冷凝中镓铟两种元素在金属液滴表面富集，然后再通过高压氨水溶液的冲击和冷却，将金属液滴进一步破碎冷却呈近球形的合金软磁粉末，同时使得合金软磁粉末表面形成致密的氧化膜和氮化膜。
2.根据权利要求 1 所述的一种铁硅铬镓铟氮合金软磁粉末的水气联合雾化制备方法，其特征在于：所述步骤2）制成的合金软磁粉末质量比为：铬0.1-10%，硅2-8%，镓0.1-2%，铟0.1-2%，氮0.01-0.5%，铁余量。
3.根据权利要求 1 所述的一种铁硅铬镓铟氮合金软磁粉末的水气联合雾化制备方法，其特征在于：所述1）冶炼过程中，在预制坩埚中，底部预埋气砖，中频感应炉炉口用炉盖封闭，用氩气作为炉口保护气体。
4.根据权利要求 3 所述的一种铁硅铬镓铟氮合金软磁粉末的水气联合雾化制备方法，其特征在于：所述1）冶炼合金液时，先将铁、铬、硅按顺序先后加入中频感应炉完全熔化，在温度达到1580-1600度时，开始炉底吹氩；在温度达到1640-1660度时，开启炉口吹氩，随后加入镓、铟；镇静除渣后，得到合金液。
5.根据权利要求 1 所述的一种铁硅铬镓铟氮合金软磁粉末的水气联合雾化制备方法，其特征在于：所述步骤2）雾化塔的雾化桶加装变频低压引风机、压力传感器、单向阀、定向管道、冷凝器和导流板，通过压力传感器和变频低压引风机将雾化桶内压力维持在98-99KPa压力条件下，将合金液浇注入负压环境的雾化塔内，雾化桶内用氮气作为保护气氛，氮气流量在10-20M3/H，氮气通过变频低压引风机、定向管道、冷凝器和导流板在雾化桶内高速定向流动，形成负压超音速气体，将合金液柱流分散撕裂成金属液滴。
6.根据权利要求 5 所述的一种铁硅铬镓铟氮合金软磁粉末的水气联合雾化制备方法，其特征在于：浇注过程中漏包采用氩气保护，漏眼直径4-6毫米。
7.根据权利要求 6 所述的一种铁硅铬镓铟氮合金软磁粉末的水气联合雾化制备方法，其特征在于：所述负压超音速气体的压力为0.1-10KPa，速度为1—5马赫。
8.根据权利要求 1 所述的一种铁硅铬镓铟氮合金软磁粉末的水气联合雾化制备方法，其特征在于：所述高压氨水溶液的喷射压力120-200MPa，流量为150-350L/min。
9.根据权利要求 1 所述的一种铁硅铬镓铟氮合金软磁粉末的水气联合雾化制备方法，其特征在于：所述高压氨水溶液的氨水溶液浓度为0.5-2%。
10.根据权利要求 1 所述的一种铁硅铬镓铟氮合金软磁粉末的水气联合雾化制备方法，其特征在于：所述步骤2）雾化过程中产生的气体和雾化桶内的氮气一起被变频低压引风机排出雾化桶，并导入低浓度磷酸溶液中做无害化处理。
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