CN110752087A - 稀土类异方性粘结磁粉的制备方法 - Google Patents
稀土类异方性粘结磁粉的制备方法 Download PDFInfo
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 60
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 36
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 19
- 150000004678 hydrides Chemical class 0.000 claims abstract description 18
- 238000009792 diffusion process Methods 0.000 claims abstract description 13
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 8
- 229910052777 Praseodymium Inorganic materials 0.000 claims abstract description 7
- 229910052751 metal Inorganic materials 0.000 claims abstract description 4
- 239000002184 metal Substances 0.000 claims abstract description 4
- 230000007704 transition Effects 0.000 claims abstract description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 32
- 229910052739 hydrogen Inorganic materials 0.000 claims description 32
- 239000001257 hydrogen Substances 0.000 claims description 32
- 230000005291 magnetic effect Effects 0.000 claims description 21
- 238000000137 annealing Methods 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 10
- 239000010949 copper Substances 0.000 claims description 9
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- 229910052746 lanthanum Inorganic materials 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 6
- 229910052684 Cerium Inorganic materials 0.000 abstract description 5
- 229910052692 Dysprosium Inorganic materials 0.000 abstract description 5
- 229910052771 Terbium Inorganic materials 0.000 abstract description 5
- 230000006872 improvement Effects 0.000 abstract description 3
- 238000006356 dehydrogenation reaction Methods 0.000 description 17
- 229910001172 neodymium magnet Inorganic materials 0.000 description 11
- 238000010521 absorption reaction Methods 0.000 description 9
- 238000007323 disproportionation reaction Methods 0.000 description 9
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 7
- 229910045601 alloy Inorganic materials 0.000 description 7
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
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- 230000005290 antiferromagnetic effect Effects 0.000 description 1
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- 238000005859 coupling reaction Methods 0.000 description 1
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- 229910052742 iron Inorganic materials 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
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Abstract
一种稀土类异方性粘结磁粉的制备方法,包括以下步骤:(1)制备以RTBH为主成分的原粉;其中,所述R为Nd或Pr/Nd,T为含Fe的过渡族金属;(2)在所述原粉中加入La/Ce氢化物和铜粉制成混合物;(3)将所述混合物进行气氛扩散热处理得到稀土类异方性粘结磁粉。本发明选用La、Ce高丰度稀土元素代替Dy、Tb、Nd、Pr等中重稀土元素,能够在达到相同矫顽力提升效果的同时,还可显著降低成本,从而可实现廉价高丰度稀土的高效应用。
Description
技术领域
本发明涉及磁性材料领域,具体涉及一种稀土类异方性粘结磁粉的制备方法。
背景技术
用于粘结钕铁硼永磁材料的磁粉主要分为各向同性和异方性两大类。当前,各向同性钕铁硼磁粉采用熔体快淬法制备,最大磁能积为12-16MGOe,由此制备的同性钕铁硼粘结磁体最大磁能积不超过12MGOe。而异方性钕铁硼粘结磁粉,通常采用HDDR(即氢化-歧化-脱氢-复合)法制备,由于其微观组织的特殊性,即细小晶粒(200-500nm)在[001]易磁化轴方向的平行排列,使得其最大磁能积可达到各向同性粘结磁粉的2-3倍,经模压或者注塑成型工艺,可以制备高性能异方性粘结磁体,符合电机器件小型化、轻量化和精密化的发展趋势,因此,市场对高性能异方性磁粉的需求越来越迫切。
但是,由HDDR磁粉制备的粘结钕铁硼磁体存在耐热性不够高的问题。例如,在汽车那样暴露于高温的用途中,如果磁体的耐热性低,则产生不可逆退磁的可能性高。因此就HDDR磁粉而言,充分改善其耐热性,才能使其应用于汽车等领域,从而拓展其应用范围。
要改善异方性磁粉的耐热性,即降低高温下退磁可能性,就是要提升磁粉在高温下的矫顽力,主要有两种途径:第一种是提高异方性磁粉本身的矫顽力(室温矫顽力),这样在温度系数不发生改变的条件下,其高温矫顽力也相应得到提升;第二种是提高异方性磁粉的温度系数,这样在室温矫顽力不发生变化的条件下,其高温矫顽力也相应得到提升。
目前,主要集中在第一种途径,即通过提高异方性磁粉本身的矫顽力来改善耐热性。而提升磁粉本身矫顽力的方法主要有两类:一类是直接添加Tb、Dy等中重稀土元素,另一类是通过晶界扩散添加中重稀土元素或者低熔点合金元素。前者由于重稀土的添加无疑会带来生产成本的大幅提高不仅消耗了稀缺的重稀土战略资源,大幅提高了生产成本,而且由于Tb、Dy与Fe原子之间的反铁磁耦合作用,降低了磁体的剩磁和磁能积;后者由于晶界扩散工序的增加,需要增加扩散源制备、混粉以及扩散热处理等步骤,造成生产过程比较复杂,加工成本也随之提高。
例如,在CN107424694A中,公开了通过将至少Nd和Cu的供给源的扩散原料和异方性磁铁原料混合,进行扩散工序,得到高矫顽力异方性磁粉,但该发明生产过程复杂,加工成本高,而且未对高丰度稀土元素La、Ce未做任何记载。在CN1345073A中,通过晶界扩散,使得中重稀土元素(Dy、Tb、Nd、Pr一种以上)进入到晶界相,显著提高了矫顽力,同时生产成本也大幅提高。
因此,开发不含重稀土的高矫顽力稀土类异方性粘结磁粉成为当前研究热点。
发明内容
(一)发明目的
本发明的目的是提供一种稀土类异方性粘结磁粉的制备方法,不仅能够提高稀土类异方性粘结磁粉的矫顽力,而且还可降低生产成本。
(二)技术方案
为解决上述问题,本发明的提供了一种稀土类异方性粘结磁粉的制备方法,包括以下步骤:
(1)制备以RTBH为主成分的原粉;其中,所述R为Nd或Pr/Nd,T为含Fe的过渡族金属;
(2)在所述原粉中加入La/Ce氢化物和铜粉制成混合物;
(3)将所述混合物进行扩散热处理得到稀土类异方性粘结磁粉。
钕铁硼由主相Nd2Fe14B和晶界相组成。对于粘结钕铁硼磁粉来说,其晶界相的含量以及非磁性程度直接影响了矫顽力的高低。
在本发明中,通过异方性钕铁硼磁粉与La/Ce氢化物和铜粉混合之后进行晶界扩散,使得La、Ce高丰度稀土元素和铜元素进入到晶界相,在增加晶界相宽度的同时,还有效降低晶界相的磁性,提升其去交换耦合作用,从而提高磁粉矫顽力。
由此可见,本发明通过使用高丰度稀土La/Ce,而不使用中重稀土Dy/Tb/Pr/Nd的前提下,依然能够有效提升异方性磁粉的矫顽力,从而改善其耐热性。
(三)有益效果
本发明的上述技术方案具有如下有益的技术效果:选用的La、Ce高丰度稀土元素储量高,价格低,相比添加Dy、Tb、Nd、Pr等中重稀土元素,能够在达到相同矫顽力提升效果的同时,还可明显降低成本,从而可实现廉价高丰度稀土的高效应用。
附图说明
图1是实施例1制得以RTBH为主成分的原粉的低放大倍数组织结构图;
图2为实施例1制得以RTBH为主成分的原粉的高放大倍数组织结构图;
图3是实施例4制得稀土类异方性粘结磁粉的低放大倍数组织结构图;
图4是实施例4制得稀土类异方性粘结磁粉的高放大倍数组织结构图。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚明了,下面结合具体实施方式并参照附图,对本发明进一步详细说明。应该理解,这些描述只是示例性的,而并非要限制本发明的范围。此外,在以下说明中,省略了对公知结构和技术的描述,以避免不必要地混淆本发明的概念。
本发明提供一种稀土类异方性粘结磁粉的制备方法,包括以下步骤:
(1)制备以RTBH为主成分的原粉;其中,所述R为Nd或Pr/Nd,T为含Fe的过渡族金属;
(2)在所述原粉中加入La/Ce氢化物和铜粉制成混合物;
(3)将所述混合物进行气氛扩散热处理得到稀土类异方性粘结磁粉。
在本发明中,以RTBH为主成分的原粉是采用HDDR法制得,可包括以下步骤:
a、吸氢歧化阶段:将RTBH系合金置于旋转气固反应炉中,在0-0.1MPa氢气压力下加热至760-860℃,然后保持氢气压力在20-100kPa,保温1h-4h,完成吸氢歧化阶段的处理;
b、缓慢脱氢再聚合阶段:在吸氢歧化阶段完成后,保持炉内温度至800-900℃,并调整炉内氢气压力至1-10kPa,保温保压10-60分钟,完成缓慢脱氢再聚合阶段的处理;
c、完全脱氢阶段:在缓慢脱氢再聚合阶段完成后,迅速抽真空至氢压1Pa以下,完成完全脱氢阶段;
d、冷却阶段:在完全脱氢阶段完成后,冷却至室温,得到以RTBH为主成分的原粉。
在本发明步骤(1)中,以原粉的重量为基准,所述R含量≤28.9wt%,晶界相可沿晶粒边界均匀分布,并包围主相晶粒,使得相邻晶粒磁分割开来,可有效起到去磁交换耦合作用。优选地,所述R含量为26.68~28.9wt%,例如,R含量可以为28.9wt%%、28.5wt%、28.0wt%、27.5wt%、27wt%、26.68wt%,以及这些点值中的任意两个所构成的范围中的任意值。
在本发明步骤(1)中,所述原粉的平均粒度D50为80-120μm。
本发明中,La/Ce氢化物是作为晶界扩散元素,在步骤(3)热处理过程中,La/Ce元素将进入晶界相中。
在本发明步骤(2)中,以原粉的重量为基准,所述La/Ce氢化物的加入比例不高于5wt%,优选为0.5~5wt%,例如,可以为0.5wt%,1.0wt%,1.5wt%,2.0wt%,2.5wt%,3.0wt%,3.5wt%,4.0wt%,4.5wt%,5.0wt%,以及这些点值中的任意两个所构成的范围中的任意值。
本发明中,铜粉主要用来降低La/Ce氢化物的熔点,从而有效降低热处理过程所需使得晶界相熔化的温度。
在本发明步骤(2)中,以La/Ce氢化物的重量为基准,所述铜粉的加入比例为25~100wt%。
在本发明步骤(2)中,所述铜粉的平均粒度D50小于10μm,有利于铜粉较好地扩散到晶界相。
本发明中,在气氛扩散热处理过程中,熔化成液态的晶界相为扩散通道,有利于La、Ce高丰度稀土元素和铜元素从以RTBH为主成分的原粉表面扩散到原粉内部,进入晶界相,在增加晶界相宽度的同时,还有效降低晶界相的磁性,提升其去交换耦合作用,从而提高以RTBH为主成分原粉的矫顽力。
在本发明步骤(3)中,优选实施方式是,所述气氛扩散热处理包括含氢气氛热处理或真空热处理。
优选情况下,所述含氢气氛热处理的条件包括:氢气压力≤1kPa,退火温度为700-900℃,退火时间为20-180min。
优选情况下,所述真空处理的条件包括:真空度≤5Pa,退火温度为700-900℃,退火时间为20-180min。
在本发明步骤(3)中,所述稀土类异方性粘结磁粉的平均粒度D50为80-120μm。
在本发明步骤(3)中,所述稀土类异方性粘结磁粉包括晶界相和R2T14B磁性相的晶粒。
优选情况下,在稀土类异方性粘结磁粉中,所述晶界相中La/Ce含量与R2T14B磁性相中La/Ce含量的比例大于5。此时La/Ce元素主要集中在晶界相内,R2T14B磁性相内含量较少,这样可以有效增加晶界相的宽度,降低晶界相的磁性,提升矫顽力,同时不会造成剩磁的明显降低。
优选情况下,在稀土类异方性粘结磁粉中,所述晶界相中Cu含量与R2T14B磁性相中Cu含量的比例大于10。此时Cu元素主要集中在晶界相内,R2T14B磁性相内含量较少,这样可以有效增加晶界相的宽度,降低晶界相的磁性,提升矫顽力,同时不会造成剩磁的明显降低。
以下将通过实施例对本发明进行详细描述。以下实施例中,
粒度分布测试参数通过PSA-激光粒度分析仪测得;
矫顽力参数通过磁性能测量仪测得;
最大磁能积通过磁性能测量仪测得;
剩磁通过磁性能测量仪测得。
在没有特别说明的情况下,所用原料均采用市售产品。
实施例1
以NdFeBH为主成分的原粉采用HDDR法制备,包括以下步骤:
(1)吸氢歧化阶段:将NdFeBH系合金置于旋转气固反应炉中,在0.1MPa氢气压力下加热至800℃,然后保持氢气压力在50kPa,保温2h,完成吸氢歧化阶段的处理;
(2)缓慢脱氢再聚合阶段:在吸氢歧化阶段完成后,保持炉内温度至800℃,并调整炉内氢压至5kPa,保温保压30分钟,完成缓慢脱氢再聚合阶段的处理;
(3)完全脱氢阶段:在缓慢脱氢再聚合阶段完成后,迅速抽真空至氢压1Pa以下,完成完全脱氢阶段;
(4)冷却阶段:在完全脱氢阶段完成后,冷却至室温,得到以NdFeBH为主成分的原粉,其低放大倍数组织结构图和高放大倍数组织结构图分别见图1和图2。图1中主体为等轴状的Nd2Fe14B晶粒,晶间之间分布的白色相为晶界相;图2为透射电子显微镜拍摄的高分辨图,图中两个明显的区域为相邻的两个Nd2Fe14B晶粒,其相邻处为厚度为2nm的晶界相。
实施例2
以PrNdFeBH为主成分的原粉采用HDDR法制备,包括以下步骤:
(1)吸氢歧化阶段:将NdFeBH系合金置于旋转气固反应炉中,在0.05MPa氢气压力下加热至760℃,然后保持氢气压力在30kPa,保温4h,完成吸氢歧化阶段的处理;
(2)缓慢脱氢再聚合阶段:在吸氢歧化阶段完成后,保持炉内温度至900℃,并调整炉内氢压至3kPa,保温保压60分钟,完成缓慢脱氢再聚合阶段的处理;
(3)完全脱氢阶段:在缓慢脱氢再聚合阶段完成后,迅速抽真空至氢压1Pa以下,完成完全脱氢阶段;
(4)冷却阶段:在完全脱氢阶段完成后,冷却至室温,得到以PrNdFeBH为主成分的原粉。
实施例3
稀土类异方性粘结磁粉的制备方法,包括以下步骤:
(1)在实施例1制得的以NdFeBH为主成分的原粉中加入0.5wt%La/Ce氢化物和0.125wt%铜粉制成混合物;
(2)将所述混合物进行含氢气氛热处理得到稀土类异方性粘结磁粉,其中,在含氢气氛热处理过程中,氢气压力为0.6kPa,退火温度为700℃,退火时间为20min。
实施例4
稀土类异方性粘结磁粉的制备方法,包括以下步骤:
(1)在实施例2制得的以PrNdFeBH为主成分的原粉中加入5.0wt%La/Ce氢化物和1.25wt%铜粉制成混合物;
(2)将所述混合物进行真空热处理得到稀土类异方性粘结磁粉,其中,在真空处理过程中,真空度保持在5Pa,退火温度为700℃,退火时间为180min,制得的稀土类异方性粘结磁粉的低放大倍数组织结构图和高放大倍数组织结构图分别见图3和图4。图3中主体为等轴状的Nd2Fe14B晶粒,晶粒之间分布的白色相为晶界相;图4为透射电子显微镜拍摄的高分辨图,图中两个明显的区域为相邻的两个Nd2Fe14B晶粒,其相邻处为厚度为5nm左右的晶界相。
实施例5
稀土类异方性粘结磁粉的制备方法,包括以下步骤:
(1)在实施例2制得的以NdFeBH为主成分的原粉中加入3.0wt%La/Ce氢化物和3.0wt%铜粉制成混合物;
(2)将所述混合物进行含氢气氛热处理得到稀土类异方性粘结磁粉,其中,在含氢气氛热处理过程中,氢气压力为0.5kPa,退火温度为800℃,退火时间为60min。
实施例6
按照实施例4的方法制备稀土类异方性粘结磁粉,不同的是,加入5wt%La/Ce氢化物和1.25wt%铜粉制成混合物。
实施例7
按照实施例4的方法制备稀土类异方性粘结磁粉,不同的是,加入5.0wt%La/Ce氢化物和5.0wt%铜粉制成混合物。
实施例8
按照实施例4的方法制备稀土类异方性粘结磁粉,不同的是,加入4.0wt%La/Ce氢化物和2.0wt%铜粉制成混合物。
对比例1
采用与实施例3制得的稀土类异方性粘结磁粉化学成分完全相同的稀土合金,按照实施例1的方法制备稀土类异方性粘结磁粉。
对比例2
采用与实施例4制得的稀土类异方性粘结磁粉化学成分完全相同的稀土合金,按照实施例1的方法制备稀土类异方性粘结磁粉。
对比例3
采用与实施例5制得的稀土类异方性粘结磁粉化学成分完全相同的稀土合金,按照实施例1的方法制备稀土类异方性粘结磁粉。
测试例
分别测试实施例1-2制得以RTBH为主成分的原粉的平均粒度D50、矫顽力、最大磁能积和剩磁,测试结果见表1。分别测试测试实施例3-8和对比例1-3制得稀土类异方性粘结磁粉的平均粒度D50、矫顽力、最大磁能积和剩磁,测试结果见表1。测试过程需要将磁粉在磁场中进行取向,取向磁场不小于30kOe,确保其取向完全,此时磁粉易磁化方向沿外场方向平行排列。
表1
通过表1的结果可以看出,本发明的实施例通过在HDDR法制备的异方性磁粉磁粉原粉基础上,添加La/Ce氢化物和Cu粉,进行热处理,在有效提升磁粉矫顽力的同时,不造成剩磁的明显降低。由此制备了剩磁、矫顽力和最大磁能积较高的磁粉。相比对比例1-3,在同等化学成分的前提下,采用本发明的实施例3-8制备的磁粉具有较高的磁性能,效果明显。
综上,本发明旨在保护一种既能提高矫顽力又能降低成本的稀土类异方性粘结磁粉的制备方法。
应当理解的是,本发明的上述具体实施方式仅仅用于示例性说明或解释本发明的原理,而不构成对本发明的限制。因此,在不偏离本发明的精神和范围的情况下所做的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。此外,本发明所附权利要求旨在涵盖落入所附权利要求范围和边界、或者这种范围和边界的等同形式内的全部变化和修改例。
Claims (13)
1.一种稀土类异方性粘结磁粉的制备方法,其特征在于,包括以下步骤:
(1)制备以RTBH为主成分的原粉;其中,所述R为Nd或Pr/Nd,T为含Fe的过渡族金属;
(2)在所述原粉中加入La/Ce氢化物和铜粉制成混合物;
(3)将所述混合物进行气氛扩散热处理得到稀土类异方性粘结磁粉。
2.根据权利要求1所述的制备方法,其特征在于,步骤(1)中,所述原粉的平均粒度D50为80-120μm。
3.根据权利要求1所述的制备方法,其特征在于,步骤(1)中,以原粉的重量为基准,所述R含量≤28.9wt%。
4.根据权利要求1所述的制备方法,其特征在于,步骤(2)中,以原粉的重量为基准,所述La/Ce氢化物的加入比例不高于5wt%。
5.根据权利要求1所述的制备方法,其特征在于,步骤(2)中,以La/Ce氢化物的重量为基准,所述铜粉的加入比例为25-100wt%。
6.根据权利要求1所述的制备方法,其特征在于,步骤(2)中,所述铜粉的平均粒度D50小于10μm。
7.根据权利要求1-6中任意一项所述的制备方法,其特征在于,步骤(3)中,所述气氛扩散热处理包括含氢气氛热处理或真空热处理。
8.根据权利要求7所述的制备方法,其特征在于,所述含氢气氛热处理的条件包括:氢气压力≤1kPa,退火温度为700-900℃,退火时间为20-180min。
9.根据权利要求7所述的制备方法,其特征在于,所述真空热处理的条件包括:真空度≤5Pa,退火温度700-900℃,退火时间为20-180min。
10.根据权利要求1-6中任意一项所述的制备方法,其特征在于,步骤(3)中,所述稀土类异方性粘结磁粉的平均粒度D50为80-120μm。
11.根据权利要求1-6中任意一项所述的制备方法,其特征在于,步骤(3)中,所述稀土类异方性粘结磁粉包括晶界相和R2T14B磁性相的晶粒。
12.根据权利要求11所述的的制备方法,其特征在于,所述晶界相中La/Ce含量与R2T14B磁性相中La/Ce含量的比例大于5。
13.根据权利要求11所述的的制备方法,其特征在于,所述晶界相中Cu含量与R2T14B磁性相中Cu含量的比例大于10。
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