CN105861978B - 一种氮化铁磁粉的机械球磨制备方法 - Google Patents

一种氮化铁磁粉的机械球磨制备方法 Download PDF

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CN105861978B
CN105861978B CN201610469969.2A CN201610469969A CN105861978B CN 105861978 B CN105861978 B CN 105861978B CN 201610469969 A CN201610469969 A CN 201610469969A CN 105861978 B CN105861978 B CN 105861978B
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彭晓领
李静
杨艳婷
徐靖才
王攀峰
洪波
金红晓
金顶峰
王新庆
葛洪良
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China Jiliang University
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • 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
    • C23C8/08—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 only one element being applied
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    • C23C8/26—Nitriding of ferrous surfaces
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    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/16—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on nitrides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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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    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
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    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling

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Abstract

本发明涉及一种氮化铁磁粉的机械球磨制备方法。该发明采用球磨氮化的方法：选择平均粒径为2~80μm的铁粉为原材料，将铁粉放入球磨罐中，选择球料比为10:1~50：1，充入0.1~0.5MPa的氨气，或选择氨水为球磨介质，控制球磨机转速为300~1000r/min，控制球磨时间为5~100h，获得球磨铁粉；将球磨后的铁粉取出，置于热处理炉中，通入保护气氛氩气或氮气，在120~200℃退火0.5~5h；降温，随炉冷却至室温，取出样品。该方法通过球磨过程中对铁粉内部造成缺陷和温度升高，加速渗氮过程。

Description

一种氮化铁磁粉的机械球磨制备方法
技术领域
本发明涉及一种氮化铁磁粉的机械球磨制备方法，属于材料制备领域。
背景技术
磁性材料，是古老而用途十分广泛的功能材料。通常所说的磁性材料是指强磁性物质。而物质的磁性早在3000年以前就被人们所认识和应用，例如中国古代用天然磁铁作为指南针。现代磁性材料已经广泛的用在我们的生活之中，例如将永磁材料用作马达，应用于变压器中的铁心材料，作为存储器使用的磁光盘，计算机用磁记录软盘等。磁性材料与信息化、自动化、机电一体化、国防、国民经济的方方面面紧密相关。
具有宽磁滞回线、高矫顽力、高剩磁，一经磁化即能保持恒定磁性的材料，称为永磁材料。常用的永磁材料分为铝镍钴系永磁合金、铁铬钴系永磁合金、永磁铁氧体、稀土永磁材料。现在高性能的永磁材料主要是稀土永磁材料。但是随着稀土价格上涨，稀土资源的管控，人们慢慢地将目光转移到不含稀土的永磁材料的开发上。而其中氮化铁系材料因其具有高饱和磁化强度，并具有耐磨、耐腐蚀等优点，有很高的应用价值而受到人们的关注。
随氮含量的变化，氮化铁具有不同的结构和性能，这其中α"-Fe16N2的饱和磁化强度值为2.83 T，远高于其他材料，引起人们浓厚的兴趣。多年来，众多科学家使用了多种方法，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。然而令人遗憾的是单相的α"-Fe16N2长期以来制备困难。
针对以上，本发明的目的是采用高能球磨的方式，为氮化提供有利条件，进而获得α"-Fe16N2相，提高氮化铁材料的磁性。
发明内容
本发明的目的在于提供一种含α"-Fe16N2相的氮化铁磁粉的机械球磨制备方法。
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）球磨氮化
将铁粉放入球磨罐中，选择球料比为10:1~50：1，充入0.1~0.5MPa的氨气，或选择氨水为球磨介质，控制球磨机转速为300~1000r/min，控制球磨时间为5~100h，获得球磨铁粉；
3）退火热处理
将球磨后的铁粉取出，置于热处理炉中，通入保护气氛氩气或氮气，在120~200℃退火0.5~5h；降温，随炉冷却至室温，取出样品。
本发明的优点是：通过球磨过程中对铁粉内部造成缺陷和温度升高，加速渗氮过程。
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）球磨氮化
将铁粉放入球磨罐中，选择球料比为10:1~50：1，充入0.1~0.5MPa的氨气，或选择氨水为球磨介质，控制球磨机转速为300~1000r/min，控制球磨时间为5~100h，获得球磨铁粉；
3）退火热处理
将球磨后的铁粉取出，置于热处理炉中，通入保护气氛氩气或氮气，在120~200℃退火0.5~5h；降温，随炉冷却至室温，取出样品。
通过本发明可以方便地制备含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）球磨氮化
将铁粉放入球磨罐中，选择球料比为10:1，充入0.5MPa的氨气，控制球磨机转速为300r/min，控制球磨时间为100h，获得球磨铁粉；
3）退火热处理
将球磨后的铁粉取出，置于热处理炉中，通入保护气氛氩气，在120℃退火5h；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6μm的羟基铁粉为原材料；
2）球磨氮化
将铁粉放入球磨罐中，选择球料比为20：1，选择氨水为球磨介质，控制球磨机转速为450r/min，控制球磨时间为70h，获得球磨铁粉；
3）退火热处理
将球磨后的铁粉取出，置于热处理炉中，通入保护气氛氮气，在140℃退火4h；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15μm的还原铁粉为原材料；
2）球磨氮化
将铁粉放入球磨罐中，选择球料比为30：1，充入0.3MPa的氨气，控制球磨机转速为600r/min，控制球磨时间为40h，获得球磨铁粉；
3）退火热处理
将球磨后的铁粉取出，置于热处理炉中，通入保护气氛氩气，在160℃退火2h；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40μm的羟基铁粉为原材料；
2）球磨氮化
将铁粉放入球磨罐中，选择球料比为40：1，选择氨水为球磨介质，控制球磨机转速为800r/min，控制球磨时间为15h，获得球磨铁粉；
3）退火热处理
将球磨后的铁粉取出，置于热处理炉中，通入保护气氛氮气，在180℃退火1h；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80μm的还原铁粉为原材料，铁粉可以为雾化铁粉、羟基铁粉或；
2）球磨氮化
将铁粉放入球磨罐中，选择球料比为50：1，充入0.1MPa的氨气，控制球磨机转速为1000r/min，控制球磨时间为5h，获得球磨铁粉；
3）退火热处理
将球磨后的铁粉取出，置于热处理炉中，通入保护气氛氩气或氮气，在200℃退火0.5h；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。

Claims (1)

1.一种α"-Fe16N2氮化铁磁粉的机械球磨制备方法，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）球磨氮化
将铁粉放入球磨罐中，选择球料比为10:1~50：1，充入0.1~0.5MPa的氨气，或选择氨水为球磨介质，控制球磨机转速为300~1000r/min，控制球磨时间为5~100h，获得球磨铁粉；
3）退火热处理
将球磨后的铁粉取出，置于热处理炉中，通入保护气氛氩气或氮气，在120~200℃退火0.5~5h；降温，随炉冷却至室温，取出样品。
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US5330554A (en) * 1991-08-30 1994-07-19 Aisin Seiki Kabushiki Kaisha Method for producing iron-nitride powders

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5330554A (en) * 1991-08-30 1994-07-19 Aisin Seiki Kabushiki Kaisha Method for producing iron-nitride powders

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Title
α＇＇-Fe16N2的制备及性能研究;诸葛兰剑等;《磁性材料及器件》;20000430;第31卷(第2期);第5页-第9页、附图4 *

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