CN111748783A - 一种用于磁性材料镀膜的多元系重稀土金属靶材 - Google Patents
一种用于磁性材料镀膜的多元系重稀土金属靶材 Download PDFInfo
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Abstract
本发明提出了用于磁性材料镀膜的多元系重稀土金属靶材,其特征包括重稀土元素、铁族过滤元素、元素Cu及微量杂质;所述的重稀土元素Tb或Dy或Ho中的一种或一种以上的组合,所述的铁族过渡元素为Fe、Co、Ni。本发明的合金靶材熔点降低,可以降低后续扩散温度到850摄氏度左右,兼顾了磁体毛坯一级时效,使晶界相更加连续和平直,起到去磁交换耦合作用,同时,低熔点液相还能够消除主相和晶界相边界处的缺陷,提高局域磁晶各向异性,本发明的合金电极电位高,防腐蚀能力强。
Description
【技术领域】
本发明具体设计一种用于磁性材料镀膜的多元系重稀土金属靶材.
【背景技术】
烧结钕铁硼磁体自1983年发明以来,因其优异的综合磁性能和相对低廉的价格而得到广泛的应用。近年来,随着风电、变频压缩机和混合动力等领域对高耐温电机的日益增长的需求,烧结钕铁硼材料性能、成本与可持续发展的问题日益突出。这是因为,这些领域要求钕铁硼磁体既要具有较高的剩磁以提供足够大的磁通密度,同时要具有足够高的内禀矫顽力以保证其在高温下的长期正常运行。目前传统轻稀土PrNd烧结钕铁硼磁体的性价比好,但内禀矫顽力比较低,基本上不能承受150度以上应用场合,严重限制了其应用领域的进一步扩大。众所周知,Dy/Tb等重稀土元素取代烧结钕铁硼主相Nd2Fe14B晶粒内的 Nd,形成重稀土的2:14:1相,将提高主相磁晶各向异性场,使磁体矫顽力大幅增加。所以,当前采取的通过合金熔炼时加入重稀土Tb、 Dy取代Pr、Nd的方法来制备高内禀矫顽力的钕铁硼材料,一般来说,用合金熔炼方法要制作150度下工作的电机一般要使用稀土总量的 15%左右并且价格昂贵的重稀土,成本较高。与此同时,重稀土资源稀缺,大量使用导致稀土资源使用不平衡,发展不可持续。另外,采用传统合金化法提高矫顽力会大幅增加生产成本,更严重的是,由于重稀土离子和铁离子之间的亚铁磁性和反铁磁性耦合,造成重稀土元素添加后磁体的剩磁及磁能积大幅下降。
为了减少重稀土使用量和提高性能,开发出了晶界扩散渗镝、渗铽技术对磁体进行改性处理。经该技术处理后,Tb、Dy元素有效分布于晶界周围,晶粒表层形成(PrNd,TbDy)2Fe14B改性区,避免了重稀土过多取代主相晶粒内部Pr、Nd元素,有效降低了Tb、Dy元素的使用量并避免了剩磁下降,同时提高内禀矫顽力。目前为止,多个文献报道了用蒸镀、溅射、涂覆等方法有效地在磁体表面附着含Dy2O3,DyF3等Dy、Tb化合物或纯Tb、纯Dy靶材或它们的合金进行晶界扩散提高了磁体矫顽力。但是上述方法仍存在成本高、重稀土有效利用率低、后续扩散温度高、时间长以及外观表面差等弊端。
此外,NdFeB磁体的抗腐蚀性能也是其在使用过程中的重要性能指标,尤其是在海上风力发电机和混合动力汽车电机上,磁体需要在腐蚀环境和高温的情况下长期运转。但是由于NdFeB磁体是多相结构,其中晶界富Nd相化学性质非常活泼,容易和氧气和水汽发生反应,同时副相的电极电位远远低于主相,容易在腐蚀环境下形成原电池,发生电化学腐蚀,加速磁体的腐蚀,最终使得磁体粉化失效。因此提高 NdFeB磁体的本征抗腐蚀性能成为目前亟待解决的问题。
鉴于此,用较少的重稀土提高磁体内禀矫顽力和抗腐蚀性,延长磁体的使用寿命,节约成本和缩短后续扩散时效时间,具有巨大的经济效益和社会效益。
【发明内容】
为了解决现有技术中存在的问题,本发明提出了一种用于磁性材料镀膜的多元系重稀土金属靶材,其特征包括重稀土元素、铁族过渡元素、元素Cu;所述的重稀土元素为Tb或Dy或Ho中的一种或两种以上的组合,所述的铁族过渡元素为Fe、Co、Ni。
作为优选,所述的重稀土元素的Tb或Dy或Ho中的一种占总比量的 28%~80%,所述Cu占总比量的2.5%~10%,所述的铁族过渡元素中Co 和Ni的和占总比量的8%~20%,余量为Fe。
作为优选,所述的重稀土元素中Tb和Dy的混合之和占总比量的 28%~80%,所述Cu占总比量的2.5%~10%,所述的铁族过渡元素中Co 和Ni的混合之和占总比量的8%~20%,剩余含量为Fe。
作为优选,所述的重稀土元素中Tb和Ho的和占总比量的28%~ 80%,所述Cu占总比量的2.5%~10%,所述的铁族过渡元素中Co和Ni 的和占总比量的8%~20%,剩余含量为Fe。
作为优选,所述的重稀土元素中Dy和Ho的和占总比量的28%~ 80%,所述Cu占总比量的2.5%~10%,所述的铁族过渡元素中Co和Ni 的和占总比量的8%~20%,剩余含量为Fe。
生产工艺为:a.将上述各元素纯度为99.5wt%或以上的金属原料放入高真空熔炼炉中混合并熔炼;b.将抽真空到真空度10-3~10-1Pa 并加热熔化直到出现液体完成初步熔化;c.为防止飞溅和挥发烧损,在初步熔化完成后,充入氩气到500Pa~50000Pa;d.再采用大功率加热熔化并真空精炼;e.最后浇铸成合金铸锭,再经过精密机械加工做成各种形状的合金靶材。
本发明,成分设计加入高电极电位的元素Cu,能够提高晶界相电位并优化显微结构,是较为理想的添加元素,它是三元系合金靶材的重要组元,形成低熔点高耐腐蚀性的靶材合金,一定程度上改善了靶材与主相的润湿性,有利于降低靶材熔点,提高扩散系数,可降低设备渗镝扩散工作时间,生产效率大大提高。
传统的靶材晶界扩散后,要做一个真空中10-4~10-3Pa加热到900~ 1000℃、5~10小时的扩散退火处理。本发明的合金靶材熔点降低,可以降低后续扩散温度到850℃左右,兼顾了磁体毛坯一级时效,使晶界相更加连续和平直,起到去磁交换耦合作用,同时,低熔点液相还能够消除主相和晶界相边界处的缺陷,提高局域磁晶各向异性。
本发明设计的多元系合金靶材,通过晶界扩散渗入磁体晶粒晶界后,形成了较为稳定的新晶界相,由于其相对较高的电极电位,这些新晶界相有较强的抗腐蚀性能,图1~图6是本发明新靶材合金在各种水溶液中的极化曲线,从图中可看出,新设计的靶材合金电极电位较高。并且新合金与主相晶粒间有较好的润湿性,能够有效隔离Nd2Fel4B 主相晶粒,使其在主相晶粒边界形成富含重稀土的高磁晶各向异性薄壳层,提高晶界处的反磁化畴形核场,从而用较少的重稀土有效提高磁体的内禀矫顽力、提高电极电位和降低熔点。在保证磁性能的基础上大幅度提高了磁体的抗腐蚀性能。较低的熔点使得后续扩散退火过程可以与磁体一级时效相结合,有效缩短了生产周期,节约了生产成本。
附图说明
图1是实施例1制成的靶材在0.75M NaOH水溶液中的极化曲线
图2是实施例1制成的靶材在0.005M H2SO4水溶液中的极化曲线
图3是实施例1制成的靶材在0.6M NaCl水溶液中的极化曲线
图4是实施例2制成的靶材在0.75M NaOH水溶液中的极化曲线
图5是实施例2制成的靶材在0.005M H2SO4水溶液中的极化曲线
图6是实施例6制成的靶材在NaCl水溶液中的极化曲线
图7是采用本发明靶材对N50磁体切成45*20*5磁片PVD涂覆经880℃处理和485℃二级时效后成为48SH磁体的曲线图。
具体实施方式
实施例1
将32.5份的Tb或Dy或Ho、5份的Cu、6份的Co、6份的Ni,余量为Fe的金属原料,加入高真空熔炼炉中混合,真空熔炼炉抽真空到真空度10-3~10-1Pa,并加热熔化直到出现液体完成初步熔化,为防止飞溅和挥发烧损,在初步熔化完成后,充入氩气到500Pa~50000Pa;d. 再采用大功率加热熔化并真空精炼;e.最后浇铸成合金铸锭。
实施例2
将2.5份的Ho和30份的Dy或Tb、5份的Cu、6份的Co、6份的 Ni,余量为Fe的金属原料,加入高真空熔炼炉中混合,真空熔炼炉抽真空到真空度10-3~10-1Pa,并加热熔化直到出现液体完成初步熔化,为防止飞溅和挥发烧损,在初步熔化完成后,充入氩气到500Pa~50000Pa;d.再采用大功率加热熔化并真空精炼;e.最后浇铸成合金铸锭。
下面是本发明采用重稀土元素与其他两元素制造的靶材在镀膜设备中对磁体进行镀膜的效果:
参阅图7,对商用N50磁体进行晶界扩散,其磁性能Br 14.18kGs, (BH)m49.10MGOe,Hcj 12.49kOe。
(1)用金刚石多线切割机或内圆切片机将块状N50磁体切成 45×20×5的方片试样。
(2)经过超声波除油清洗干净磁片并即刻干燥。
(3)将干净磁片放入真空PVD炉子,设备靶材采用本发明实施例1 或实施例2的靶材,在真空下磁控溅射大约60分钟,磁体表面得到平均厚度25微米左右的涂层。
(4)冷却后取出磁片,放入真空扩散炉,在880℃氩气气氛下对试样进行6小时的晶界扩散处理。扩散完成后再在485℃氩气气氛中对试样进行4小时的二级回火处理,测得试样的磁性能为Br 13.81kGs, (BH)m 46.28MGOe,Hcj 23.39kOe。
上述实施例是对本发明的说明,不是对本发明的限定,任何对本发明简单变换后的方案均属于本发明的保护范围。
Claims (6)
1.一种用于磁性材料镀膜的多元系重稀土金属靶材,其特征包括重稀土元素、铁族过滤元素、元素Cu;所述的重稀土元素为Tb或Dy或Ho中的一种或两种以上的组合,所述的铁族过渡元素为Fe、Co、Ni。
2.如权利要求1所述的一种用于磁性材料镀膜的多元系重稀土金属靶材,其特征在于:所述的重稀土元素的Tb或Dy或Ho中的一种占总比量的28%~80%,所述Cu占总比量的2.5%~10%,所述的铁族过滤元素中Co和Ni的占总比量的8%~20%,余量为Fe。
3.如权利要求1所述的一种用于磁性材料镀膜的多元系重稀土金属靶材,其特征在于:所述的重稀土元素中Tb和Dy的混合之和占总比量的28%~80%,所述Cu占总比量的2.5%~10%,所述的铁族过滤元素中Co和Ni的混合之和占总比量的8%~20%,剩余含量为Fe。
4.如权利要求1所述的一种用于磁性材料镀膜的多元系重稀土金属靶材,其特征在于:所述的重稀土元素中Tb和Ho的和占总比量的28%~80%,所述Cu占总比量的2.5%~10%,所述的铁族过滤元素中Co和Ni的和占总比量的8%~20%,剩余含量为Fe。
5.如权利要求1所述的一种用于磁性材料镀膜的多元系重稀土金属靶材,其特征在于:所述的重稀土元素中Dy和Ho的和占总比量的28%~80%,所述Cu占总比量的2.5%~10%,所述的铁族过滤元素中Co和Ni的和占总比量的8%~20%,剩余含量为Fe。
6.如权利要求1所述的一种用于磁性材料镀膜的多元系重稀土金属靶材,其特征在于:所述的生产工艺为:a.将上述三元素纯度为99.5wt%或以上的金属原料放入高真空熔炼炉中混合;b.抽真空到真空度10-3~10-1Pa并加热熔化直到出现液体完成初步熔化;c.为防止飞溅和挥发烧损,在初步熔化完成后,充入氩气到500Pa~50000Pa;d.再采用大功率加热熔化并真空精炼;e.最后浇铸成合金铸锭,再经过精密机械加工做成各种形状的合金靶材。
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