CN112635145B - 一种复合磁粉的制备方法 - Google Patents
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- 239000006247 magnetic powder Substances 0.000 title claims abstract description 60
- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000010438 heat treatment Methods 0.000 claims abstract description 36
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 35
- 239000000956 alloy Substances 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 31
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 27
- 238000004544 sputter deposition Methods 0.000 claims abstract description 27
- 238000005496 tempering Methods 0.000 claims abstract description 24
- 229910016629 MnBi Inorganic materials 0.000 claims abstract description 22
- -1 rare earth nitride Chemical class 0.000 claims abstract description 21
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 20
- 229910052786 argon Inorganic materials 0.000 claims abstract description 18
- 238000000713 high-energy ball milling Methods 0.000 claims abstract description 16
- 239000011812 mixed powder Substances 0.000 claims abstract description 14
- 230000006698 induction Effects 0.000 claims abstract description 13
- 238000005303 weighing Methods 0.000 claims abstract description 13
- 238000003723 Smelting Methods 0.000 claims abstract description 12
- 230000002776 aggregation Effects 0.000 claims abstract description 8
- 239000006185 dispersion Substances 0.000 claims abstract description 8
- 239000000758 substrate Substances 0.000 claims abstract description 8
- 238000005516 engineering process Methods 0.000 claims abstract description 7
- 238000005477 sputtering target Methods 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000005054 agglomeration Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- IBIOTXDDKRNYMC-UHFFFAOYSA-N azanylidynedysprosium Chemical compound [Dy]#N IBIOTXDDKRNYMC-UHFFFAOYSA-N 0.000 claims description 2
- DPDGELPGCPPHSN-UHFFFAOYSA-N azanylidynelutetium Chemical compound [Lu]#N DPDGELPGCPPHSN-UHFFFAOYSA-N 0.000 claims description 2
- DOHQPUDBULHKAI-UHFFFAOYSA-N azanylidyneterbium Chemical compound [Tb]#N DOHQPUDBULHKAI-UHFFFAOYSA-N 0.000 claims description 2
- AJXBBNUQVRZRCZ-UHFFFAOYSA-N azanylidyneyttrium Chemical compound [Y]#N AJXBBNUQVRZRCZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 239000000696 magnetic material Substances 0.000 abstract description 3
- 238000004220 aggregation Methods 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000004615 ingredient Substances 0.000 abstract 1
- 239000011572 manganese Substances 0.000 description 13
- 230000005415 magnetization Effects 0.000 description 6
- 238000009792 diffusion process Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 150000002910 rare earth metals Chemical class 0.000 description 3
- KYAZRUPZRJALEP-UHFFFAOYSA-N bismuth manganese Chemical compound [Mn].[Bi] KYAZRUPZRJALEP-UHFFFAOYSA-N 0.000 description 2
- 229910001172 neodymium magnet Inorganic materials 0.000 description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 2
- 229910001152 Bi alloy Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000001808 coupling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
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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
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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