CN112635145B - 一种复合磁粉的制备方法 - Google Patents

一种复合磁粉的制备方法 Download PDF

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CN112635145B
CN112635145B CN202110043995.XA CN202110043995A CN112635145B CN 112635145 B CN112635145 B CN 112635145B CN 202110043995 A CN202110043995 A CN 202110043995A CN 112635145 B CN112635145 B CN 112635145B
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泮敏翔
俞能君
杨杭福
葛洪良
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China Jiliang University
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Abstract

本发明公开了一种复合磁粉的制备方法，属于磁性材料技术领域。该制备方法包括：按照MnBi合金成分称量配料、熔炼和高能球磨，在高能球磨过程中通过氩气高速气流将稀土氮化物喷射到MnBi磁粉中，使MnBi磁粉表面得到稀土氮化物的有效包覆；通过感应熔炼制备Fe30Co70合金溅射靶材；利用磁控溅射技术将Fe30Co70合金靶材溅射在稀土氮化物包覆的MnBi磁粉上，为了避免溅射过程中磁粉的团聚和分散，溅射过程中对基底混合粉体施加振动，振动频率为5~20 Hz，随后将复合磁粉在氩气保护下，进行一级和二级回火热处理，最终获得复合磁粉。本发明工艺过程简单，易操作，有利于复合磁粉在更多永磁器件中的应用，以满足市场需求。

Description

一种复合磁粉的制备方法
技术领域
本发明涉及磁性材料技术领域，尤其涉及一种复合磁粉的制备方法。
背景技术
近年来，随着世界稀土资源的日益减少、价格快速增长，及时开发一类新型高磁性稀土永磁体，是磁性产品发展的要求，更是我国稀土产业可持续发展的重大课题。MnBi永磁体具有价格低廉、不易腐蚀、力学性能好等优点，特别是它在一定温度范围内矫顽力呈正的温度系数，可以弥补NdFeB永磁体的不足之处。但是，由于MnBi低温相是由包晶反应形成，极难制备单相合金，从而导致其磁性能偏低，极大地限制该类材料的应用。因此，如何获得高性能纯单相锰铋合金，成为锰铋永磁材料拓宽应用范围的关键问题。
双相纳米晶结构永磁体中的软磁相为合金提供高的矫顽力，而硬磁相为合金提供高的矫顽力，两相之间的交换耦合作用直接体现在了合金的磁性能。目前，国内外研究较多的是NdFeB/α-Fe、SmCo/(α-Fe,Fe-Co)等复合磁体上。而在MnBi基复合磁体中，对其研究的较少，因此，本专利通过选取高各向异性常数的MnBi作为硬磁相，而具有高饱和磁化强度的FeCo作为软磁相，同时通过氩气高速气流将粒径范围为200~500 nm的稀土氮化物喷射到高能球磨过程中的MnBi磁粉中，使MnBi磁粉表面得到稀土氮化物的有效包覆，实现了稀土元素在软/硬磁相之间的扩散，有效实现了软/硬磁相的复合及稀土元素的扩散，最终获得了高性能的复合磁粉。
发明内容
针对现有技术中存在的问题，本发明目的在于提供一种复合磁粉的制备方法。
本发明的复合磁粉的制备方法，包括如下步骤：
（1）按照原子百分比MnxBi100-x进行称重配料并通过真空感应熔炼获得合金铸锭，其中35≤x≤65，随后MnBi合金铸锭通过高能球磨机制得MnBi磁粉，并且MnBi合金铸锭在高能球磨的运行过程中，通过氩气高速气流将粒径范围为200~500 nm的稀土氮化物喷射到MnBi磁粉中，使MnBi磁粉表面得到稀土氮化物的有效包覆；
（2）按照Fe30Co70合金成分称量配料，并通过感应熔炼制备Fe30Co70合金溅射靶材；
（3）利用磁控溅射技术将步骤（2）制得的Fe30Co70合金靶材溅射在步骤（1）制得的混合粉体上，为了避免溅射过程中磁粉的团聚和分散，溅射过程中对基底混合粉体施加振动，振动频率为5~20 Hz；
（4）将步骤（3）制得的复合磁粉在氩气保护下，进行一级和二级回火热处理，最终获得复合磁粉。
进一步的，步骤（1）中所述的高能球磨的时间为1~8 h，氩气高速气流的流速为100~200 m/s；所述的稀土氮化物为氮化铽、氮化镥、氮化钇或氮化镝中的一种或者几种。
进一步的，步骤（3）中所述的溅射过程中磁控溅射电流为20~40 A，磁控溅射时间为0.5~5 h。
进一步的，步骤（4）中所述的一级回火热处理的温度为600~900 ℃，热处理时间为1~10 h，随后水冷至室温；所述的二级回火热处理的温度为200~500 ℃，热处理时间为1~3 h，最后水冷至室温。
与现有的技术相比，本发明具有如下优点和有益效果：本发明将高各向异性常数的MnBi作为硬磁相，而具有高饱和磁化强度的FeCo作为软磁相，同时通过氩气高速气流稀土氮化物喷射到高能球磨过程中的MnBi磁粉上，使MnBi磁粉表面得到稀土氮化物的有效包覆，实现了稀土元素在软/硬磁相之间的扩散，在提升复合磁体的磁性能的同时可以在一定程度降低原料成本；同时，本发明通过磁控溅射及溅射过程中对基底混合粉体施加振动，有效避免了溅射过程中磁粉的团聚和分散，并通过一级和二级回火热处理，最终获得了高性能的复合磁粉。
具体实施方式
下面将结合实施例对本发明做进一步的详细说明，但本发明并不仅仅局限于以下实施例。
实施例1
（1）按照原子百分比Mn35Bi65进行称重配料并通过真空感应熔炼获得合金铸锭，随后Mn35Bi65合金铸锭在高能球磨的运行过程中（高能球磨时间为8 h），通过氩气高速气流（流速为200 m/s）将粒径范围为200 nm的稀土氮化铽喷射到Mn35Bi65磁粉中，使Mn35Bi65磁粉表面得到稀土氮化铽的有效包覆；
（2）按照Fe30Co70合金成分称量配料，并通过感应熔炼制备Fe30Co70合金溅射靶材；
（3）利用磁控溅射技术将步骤（2）制得的Fe30Co70合金靶材溅射在步骤（1）制得的混合粉体上，为了避免溅射过程中磁粉的团聚和分散，溅射过程中对基底混合粉体施加振动，振动频率为20 Hz；所述的溅射过程中磁控溅射电流为40 A，磁控溅射时间为5 h；
（4）将步骤（3）制得的复合磁粉在氩气保护下，进行一级和二级回火热处理，所述的一级回火热处理的温度为900 ℃，热处理时间为9 h，随后水冷至室温；所述的二级回火热处理的温度为200 ℃，热处理时间为2 h，最后水冷至室温，最终获得复合磁粉。
采用本发明制备的复合磁粉经磁性能测试，矫顽力为18.79 kOe，饱和磁化强度为60.2 emu/g。
实施例2
（1）按照原子百分比Mn50Bi50进行称重配料并通过真空感应熔炼获得合金铸锭，随后Mn50Bi50合金铸锭在高能球磨的运行过程中（高能球磨时间为5 h），通过氩气高速气流（流速为180 m/s）将粒径范围为300 nm的稀土氮化镥喷射到Mn50Bi50磁粉中，使Mn50Bi50磁粉表面得到稀土氮化镥的有效包覆；
（2）按照Fe30Co70合金成分称量配料，并通过感应熔炼制备Fe30Co70合金溅射靶材；
（3）利用磁控溅射技术将步骤（2）制得的Fe30Co70合金靶材溅射在步骤（1）制得的混合粉体上，为了避免溅射过程中磁粉的团聚和分散，溅射过程中对基底混合粉体施加振动，振动频率为15 Hz；所述的溅射过程中磁控溅射电流为35 A，磁控溅射时间为3 h；
（4）将步骤（3）制得的复合磁粉在氩气保护下，进行一级和二级回火热处理，所述的一级回火热处理的温度为800 ℃，热处理时间为8 h，随后水冷至室温；所述的二级回火热处理的温度为300 ℃，热处理时间为2 h，最后水冷至室温，最终获得复合磁粉。
采用本发明制备的复合磁粉经磁性能测试，矫顽力为17.56 kOe，饱和磁化强度为57.5 emu/g。
实施例3
（1）按照原子百分比Mn60Bi40进行称重配料并通过真空感应熔炼获得合金铸锭，随后Mn60Bi40合金铸锭在高能球磨的运行过程中（高能球磨时间为3 h），通过氩气高速气流（流速为130 m/s）将粒径范围为400 nm的稀土氮化钇喷射到Mn60Bi40磁粉中，使Mn60Bi40磁粉表面得到稀土氮化钇的有效包覆；
（2）按照Fe30Co70合金成分称量配料，并通过感应熔炼制备Fe30Co70合金溅射靶材；
（3）利用磁控溅射技术将步骤（2）制得的Fe30Co70合金靶材溅射在步骤（1）制得的混合粉体上，为了避免溅射过程中磁粉的团聚和分散，溅射过程中对基底混合粉体施加振动，振动频率为10 Hz；所述的溅射过程中磁控溅射电流为25 A，磁控溅射时间为2 h；
（4）将步骤（3）制得的复合磁粉在氩气保护下，进行一级和二级回火热处理，所述的一级回火热处理的温度为700 ℃，热处理时间为7 h，随后水冷至室温；所述的二级回火热处理的温度为400 ℃，热处理时间为3 h，最后水冷至室温，最终获得复合磁粉。
采用本发明制备的复合磁粉经磁性能测试，矫顽力为15.28 kOe，饱和磁化强度为52.7 emu/g。
实施例4
（1）按照原子百分比Mn65Bi35进行称重配料并通过真空感应熔炼获得合金铸锭，随后Mn65Bi35合金铸锭在高能球磨的运行过程中（高能球磨时间为1 h），通过氩气高速气流（流速为100 m/s）将粒径范围为500 nm的稀土氮化镝喷射到Mn65Bi35磁粉中，使Mn65Bi35磁粉表面得到稀土氮化镝的有效包覆；
（2）按照Fe30Co70合金成分称量配料，并通过感应熔炼制备Fe30Co70合金溅射靶材；
（3）利用磁控溅射技术将步骤（2）制得的Fe30Co70合金靶材溅射在步骤（1）制得的混合粉体上，为了避免溅射过程中磁粉的团聚和分散，溅射过程中对基底混合粉体施加振动，振动频率为5 Hz；所述的溅射过程中磁控溅射电流为20 A，磁控溅射时间为0.5 h；
（4）将步骤（3）制得的复合磁粉在氩气保护下，进行一级和二级回火热处理，所述的一级回火热处理的温度为600 ℃，热处理时间为6 h，随后水冷至室温；所述的二级回火热处理的温度为500 ℃，热处理时间为3 h，最后水冷至室温，最终获得复合磁粉。
采用本发明制备的复合磁粉经磁性能测试，矫顽力为9.87 kOe，饱和磁化强度为51.9 emu/g。

Claims (4)

1.一种复合磁粉的制备方法，其特征在于包括如下步骤：
（1）按照原子百分比MnxBi100-x进行称重配料并通过真空感应熔炼获得合金铸锭，其中35≤x≤65，随后MnBi合金铸锭通过高能球磨机制得MnBi磁粉，并且在高能球磨的运行过程中，通过氩气高速气流将粒径范围为200~500 nm的稀土氮化物喷射到MnBi磁粉中，使MnBi磁粉表面得到稀土氮化物的有效包覆；
（2）按照Fe30Co70合金成分称量配料，并通过感应熔炼制备Fe30Co70合金溅射靶材；
（3）利用磁控溅射技术将步骤（2）制得的Fe30Co70合金靶材溅射在步骤（1）制得的混合粉体上，为了避免溅射过程中磁粉的团聚和分散，溅射过程中对基底混合粉体施加振动，振动频率为5~20 Hz；
（4）将步骤（3）制得的复合磁粉在氩气保护下，进行一级和二级回火热处理，最终获得复合磁粉。
2. 根据权利要求1 所述的一种复合磁粉的制备方法，其特征在于：步骤（1）中所述的高能球磨的时间为1~8 h，氩气高速气流的流速为100~200 m/s；所述的稀土氮化物为氮化铽、氮化镥、氮化钇或氮化镝中的一种或者几种。
3. 根据权利要求1 所述的一种复合磁粉的制备方法，其特征在于：步骤（3）中所述的溅射过程中磁控溅射电流为20~40 A，磁控溅射时间为0.5~5 h。
4. 根据权利要求1 所述的一种复合磁粉的制备方法，其特征在于：步骤（4）中所述的一级回火热处理的温度为600~900 ℃，热处理时间为1~10 h，随后水冷至室温；所述的二级回火热处理的温度为200~500 ℃，热处理时间为1~3 h，最后水冷至室温。
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