CN106086776B - 一种氮化铁磁粉的低温等离子氮化制备方法 - Google Patents

一种氮化铁磁粉的低温等离子氮化制备方法 Download PDF

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CN106086776B
CN106086776B CN201610469967.3A CN201610469967A CN106086776B CN 106086776 B CN106086776 B CN 106086776B CN 201610469967 A CN201610469967 A CN 201610469967A CN 106086776 B CN106086776 B CN 106086776B
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李静
袁玮
彭晓领
杨艳婷
徐靖才
王攀峰
金红晓
金顶峰
洪波
王新庆
葛洪良
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Dongyang Dingfeng Magnetism Material Co ltd
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    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/36—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases using ionised gases, e.g. ionitriding
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    • B22F1/14—Treatment of metallic powder
    • B22F1/145—Chemical treatment, e.g. passivation or decarburisation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
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    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
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Abstract

本发明涉及一种氮化铁磁粉的低温等离子氮化制备方法。该发明以平均粒径为2~80μm的雾化铁粉、羟基铁粉或还原铁粉为原材料；通入O2，在300~400℃氧化1‑10h，以获得氧化铁粉；通入氢气，在300~400℃还原4‑20h，以重新获得铁粉；低温等离子氮化，控制温度在120~200℃，氮化1~30h；降温，随炉冷却至室温，取出样品。该方法采用低温氮等离子进行渗氮，解决了氨气渗氮法中氨气分解效率低下的瓶颈问题，有效地提高了渗氮效率。

Description

一种氮化铁磁粉的低温等离子氮化制备方法
技术领域
本发明涉及一种氮化铁磁粉的低温等离子氮化制备方法，属于材料制备领域。
背景技术
Fe-N化合物优良的软磁性、抗氧化性和耐磨性，使之成为理想的磁记录介质和磁感元件材料，受到人们的关注。Fe-N化合物主要有Fe3N，Fe4N和α"-Fe16N2等几种。根据国内外文献报道，α"-Fe16N2的磁性是铁氮化合物中最好的一类，它的饱和磁化强度达到280emu/g，比纯铁高，是目前发现的具有最高饱和磁化强度的物质。
由于α"-Fe16N2相在常温下是一个亚稳相，它的生成区很窄，所以要制备出α"-Fe16N2是一件很困难的事情，而且制备α"-Fe16N2的实验基本上都不具有重复性，每次的实验结果都不可能一模一样。多年来，众多科学家尝试从物理机制和应用角度重现具有高饱和磁化强度的α"-Fe16N2，也使用了很多的方法，比如氮化退火法、共析法、离子注入法、化学气相沉积法，物理气相沉积法等。
目前制备α"-Fe16N2的团队中最成功的是日木东北大学研宄生院高桥研教授、小川智之和户田工业助教等组成的研究小组。他们成功的以克为单位生成了α"-Fe16N2粉末。这是全球首次以高达91%的纯度，可再现地生成以g为单位的α"-Fe16N2。他们生产的α"-Fe16N2粉末粒径从几十到几百纳米，在50K下饱和磁化强度为230emu/g，在室温下为221emu/g，高于纯铁。
针对以上，本发明采用氧化、还原、低温等离子法氮化的方法制备了含α"-Fe16N2相的铁磁性材料。
发明内容
本发明的目的在于提供一种氮化铁磁粉的低温等离子氮化制备方法。
采用气相渗氮制备α"-Fe16N2时，通常采用的是氨气气氛，通过氨气在α-Fe表面的吸附、分解、扩散进行的。而最关键的一步是氨气在α-Fe表面的分解，也是决定氮化效率的关键。本发明采用低温等离子体技术，直接采用高能离子化的氮对α-Fe进行氮化，有效地增大了氮化效率。
本发明的具体步骤为：
1）材料准备
选择平均粒径为2~80μm的铁粉为原材料，铁粉可以为雾化铁粉、羟基铁粉或还原铁粉；
2）氧化
将铁粉置于热处理炉中，以恒定的速率通入O2，在300~400℃氧化1-10h，以获得氧化铁粉；
3）还原
通入氢气，在300~400℃还原4-20h，以重新获得铁粉；
4）低温等离子氮化
低温等离子氮化，控制温度在120~200℃，氮化1~30h；降温，随炉冷却至室温，取出样品。
本发明的优点是：采用低温氮等离子进行渗氮，解决了氨气渗氮法中氨气分解效率低下的瓶颈问题，有效地提高了渗氮效率。
具体实施方式
下面结合实施例对本发明进行详细描述，以便更好地理解本发明的目的、特点和优点。虽然本发明是结合该具体的实施例进行描述，但并不意味着本发明局限于所描述的具体实施例。相反，对可以包括在本发明权利要求中所限定的保护范围内的实施方式进行的替代、改进和等同的实施方式，都属于本发明的保护范围。对于未特别标注的工艺参数，可按常规技术进行。
本发明的具体步骤为：
1）材料准备
选择平均粒径为2~80μm的铁粉为原材料，铁粉可以为雾化铁粉、羟基铁粉或还原铁粉；
2）氧化
将铁粉置于热处理炉中，以恒定的速率通入O2，在300~400℃氧化1-10h，以获得氧化铁粉；
3）还原
通入氢气，在300~400℃还原4-20h，以重新获得铁粉；
4）低温等离子氮化
低温等离子氮化，控制温度在120~200℃，氮化1~30h；降温，随炉冷却至室温，取出样品。
通过本发明可以更加有效地制备含α"-Fe16N2相的氮化铁磁粉。
实施例1：
步骤为：
1）材料准备
选择平均粒径为2μm的雾化铁粉为原材料；
2）氧化
将铁粉置于热处理炉中，以恒定的速率通入O2，在300℃氧化10h，以获得氧化铁粉；
3）还原
通入氢气，在300℃还原20h，以重新获得铁粉；
4）低温等离子氮化
低温等离子氮化，控制温度在120℃，氮化30h；降温，随炉冷却至室温，取出样品。
对实施例1所制备的样品进行XRD表征，检测到了α"-Fe16N2相。
实施例2：
步骤为：
1）材料准备
选择平均粒径为4μm的羟基铁粉为原材料；
2）氧化
将铁粉置于热处理炉中，以恒定的速率通入O2，在320℃氧化8h，以获得氧化铁粉；
3）还原
通入氢气，在320℃还原15h，以重新获得铁粉；
4）低温等离子氮化
低温等离子氮化，控制温度在140℃，氮化20h；降温，随炉冷却至室温，取出样品。
对实施例2所制备的样品进行XRD表征，检测到了α"-Fe16N2相。
实施例3：
步骤为：
1）材料准备
选择平均粒径为10μm的羟基铁粉为原材料；
2）氧化
将铁粉置于热处理炉中，以恒定的速率通入O2，在340℃氧化6h，以获得氧化铁粉；
3）还原
通入氢气，在340℃还原10h，以重新获得铁粉；
4）低温等离子氮化
低温等离子氮化，控制温度在160℃，氮化15h；降温，随炉冷却至室温，取出样品。
对实施例3所制备的样品进行XRD表征，检测到了α"-Fe16N2相。
实施例4：
步骤为：
1）材料准备
选择平均粒径为20μm的雾化铁粉为原材料；
2）氧化
将铁粉置于热处理炉中，以恒定的速率通入O2，在360℃氧化4h，以获得氧化铁粉；
3）还原
通入氢气，在360℃还原8h，以重新获得铁粉；
4）低温等离子氮化
低温等离子氮化，控制温度在170℃，氮化10h；降温，随炉冷却至室温，取出样品。
对实施例4所制备的样品进行XRD表征，检测到了α"-Fe16N2相。
实施例5：
步骤为：
1）材料准备
选择平均粒径为40μm的还原铁粉为原材料；
2）氧化
将铁粉置于热处理炉中，以恒定的速率通入O2，在380℃氧化2h，以获得氧化铁粉；
3）还原
通入氢气，在380℃还原6h，以重新获得铁粉；
4）低温等离子氮化
低温等离子氮化，控制温度在180℃，氮化4h；降温，随炉冷却至室温，取出样品。
对实施例5所制备的样品进行XRD表征，检测到了α"-Fe16N2相。
实施例6：
步骤为：
1）材料准备
选择平均粒径为80μm的羟基铁粉为原材料；
2）氧化
将铁粉置于热处理炉中，以恒定的速率通入O2，在400℃氧化1h，以获得氧化铁粉；
3）还原
通入氢气，在400℃还原4h，以重新获得铁粉；
4）低温等离子氮化
低温等离子氮化，控制温度在200℃，氮化1h；降温，随炉冷却至室温，取出样品。
对实施例6所制备的样品进行XRD表征，检测到了α"-Fe16N2相。

Claims (1)

1.一种氮化铁磁粉的低温等离子氮化制备方法，其特征在于具体步骤为：
1）材料准备
选择平均粒径为2~80μm的铁粉为原材料，铁粉为雾化铁粉、羟基铁粉或还原铁粉；
2）氧化
将铁粉置于热处理炉中，以恒定的速率通入O2，在300~400℃氧化1-10h，以获得氧化铁粉；
3）还原
通入氢气，在300~400℃还原4-20h，以重新获得铁粉；
4）低温等离子氮化
低温等离子氮化，控制温度在120~200℃，氮化1~30h；降温，随炉冷却至室温，取出样品。
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CN107818853A (zh) * 2017-11-23 2018-03-20 龙岩紫荆创新研究院 一种氮化磁性粉体及其制备方法
CN109650405A (zh) * 2019-01-21 2019-04-19 昆明理工大学 一种连续合成氨的方法
CN112038082A (zh) * 2020-08-28 2020-12-04 常州古金磁性材料科技有限公司 使用高压氮化的方法制备铁氮磁性材料的方法
CN112872348B (zh) * 2020-12-31 2021-11-30 广东省科学院稀有金属研究所 一种提高稀土-铁合金氮化效率的方法
CN113199030B (zh) * 2021-04-25 2023-08-15 西安建筑科技大学 一种利用离子渗氮制备3d打印不锈钢粉末的方法
CN115181923A (zh) * 2022-06-16 2022-10-14 浙江兴昌风机有限公司 一种铝材基底离子氮化制备氮化铝薄膜的方法

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