CN108630371B - 一种高热稳定性的稀土永磁材料、其制备方法及含有其的磁体 - Google Patents

一种高热稳定性的稀土永磁材料、其制备方法及含有其的磁体 Download PDF

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CN108630371B
CN108630371B CN201710161808.1A CN201710161808A CN108630371B CN 108630371 B CN108630371 B CN 108630371B CN 201710161808 A CN201710161808 A CN 201710161808A CN 108630371 B CN108630371 B CN 108630371B
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rare earth
earth permanent
magnetic material
permanent magnetic
magnet
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CN108630371A (zh
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袁超
吴桂勇
李红卫
罗阳
杨远飞
于敦波
权宁涛
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Grirem Advanced Materials Co Ltd
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Grirem Advanced Materials Co Ltd
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Priority to CN201710161808.1A priority Critical patent/CN108630371B/zh
Priority to MYPI2018700030A priority patent/MY190644A/en
Priority to US15/868,063 priority patent/US11101057B2/en
Priority to ZA2018/00277A priority patent/ZA201800277B/en
Priority to KR1020180006413A priority patent/KR102096958B1/ko
Priority to DE102018200817.5A priority patent/DE102018200817A1/de
Priority to JP2018013691A priority patent/JP6503483B2/ja
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Abstract

一种高热稳定性的稀土永磁粉、其制备方法及含有其的磁体。所述稀土永磁材料以原子百分比所表示的组成成分为:SmxRaFe100‑x‑y‑z‑aMyNz,其中R为Zr、Hf中的至少一种,M为Co、Ti、Nb、Cr、V、Mo、Si、Ga、Ni、Mn、Al中的至少一种,x+a为7~10%,a为0~1.5%,y为0~5%,z为10~14%。本发明提供的稀土永磁材料具有优良的耐温性耐蚀性,有利于器件的进一步小型化,并有利于器件在特殊环境下的使用。本发明提供的稀土永磁材料的制备方法工艺简单,成本低,可提高制得的各向同性钐铁氮磁材料的实用价值。

Description

一种高热稳定性的稀土永磁材料、其制备方法及含有其的 磁体
技术领域
本发明属于稀土永磁材料领域,具体而言,涉及一种高热稳定性的稀土永磁粉、其制备方法及含有其的磁体。
背景技术
稀土永磁材料是指稀土金属和过渡族金属形成的合金经一定的工艺制成的永磁材料。稀土永磁材料是现在已知的综合性能最高的一种永磁材料,它比九十世纪使用的磁钢的磁性能高100多倍,比铁氧体、铝镍钴性能优越得多,比昂贵的铂钴合金的磁性能还高一倍。由于稀土永磁材料的使用,不仅促进了永磁器件向小型化发展,提高了产品的性能,而且促使某些特殊器件的产生,所以稀土永磁材料一出现,立即引起极大重视,发展极为迅速。稀土永磁材料已在机械、电子、仪表和医疗等领域获得了广泛应用。
1990年,Hong Sun和Coey等人利用气固相反应合成了间隙原子金属间化合物Sm2Fe17Nx,具有极高的各向异性场(14T)和良好的耐温性。而TbCu7型各向同性钐铁氮于1991年由德国Katter等人首次发现,这种钐铁氮原子近似比为SmFe9Nx,TbCu7型各向同性快淬钐铁氮具有饱和磁化强度高(1.7T),居里温度高(743K)、耐腐蚀性能良好等特点,且与快淬钕铁硼相比,在工艺稳定的条件下其综合成本更低,被认为是潜在的新一代稀土永磁材料。采用各向同性钐铁氮磁粉制备的粘结磁体不但秉承磁性能高,还可以缩小所需的磁体体积,并且耐腐性良好,可应用在微型电机,传感器,启动器等各领域。然而各向同性快淬钐铁氮磁粉制备的粘结磁体在较高温度下服役,会出现磁性能下降,产生磁通损失等问题。高热稳定性的各向同性钐铁氮的研究和开发具有现实意义。
JP 2002057017公开了一系列主相为TbCu7结构的各向同性的钐铁氮及其磁性能,采用熔体快淬制备的钐铁合金渗氮后磁能积达到12~18MGOe,但大部分磁粉矫顽力仍在10kOe以下,虽然专利中获得了500~900℃不同热处理温度处理后渗氮磁粉的磁性能,但并未关注其相结构的变化和其对磁粉的热稳定性影响。CN 102208234A公开了一种元素掺杂提高快淬SmFe合金液体的浸润性,以便更容易获得非晶薄带,有利于TbCu7亚稳相的形成,然而其并未提到如何改善磁粉的热稳定性。US 5750044公开了各向同性的SmFeCoZrN磁粉具有和NdFeB接近的磁性能,这种磁粉允许含有TbCu7、Th2Zn17、Th2Ni17,α-Fe中的多种相结构,但并未关注其中Th2Zn17、Th2Ni17型相含量对磁粉性能带来的影响。
各向异性Sm2Fe17Nx磁粉具有高的矫顽力和磁能积,其制备方法主要有熔体快淬法、机械合金化、HDDR、粉末冶金法以及还原扩散法等。虽然各向异性Sm2Fe17Nx磁粉具备优异内禀矫顽力,更高的使用温度,然而这些工艺均是需要先制备出单相的母合金然后经过氮化获得Sm2Fe17Nx磁粉,且磁粉颗粒需接近单畴尺寸才能获得较高的磁性能,因此制备工艺复杂,成本较高。
CN 1953110A公开一种粘结型钐铁氮和钕铁氮复合永磁材料,具备良好的磁性能、耐温性和抗氧化性能,但是其制备方法是单纯的通过不同磁粉的复合粘结,没有从材料微观结构设计的角度改善其热稳定性。CN 106312077A同样公开了一种亚微米各向异性钐铁氮磁粉及其杂化粘结磁体,同样是从复合的角度利用高性能的单晶各向异性钐铁氮来改良磁体复合磁体磁性能,而其单晶颗粒钐铁氮磁粉的制备工艺仍然较复杂,成本较高,且复合方式仍然为物理混合粘结。
应用物理杂志“Journal of applied physics”70.6(1991):3188-3196公开了不同轮速制备的快淬SmFe合金,经过淬火渗氮处理得到磁体粉末的磁性能,获得了Th2Zn17型和TbCu7型两种晶体结构的磁粉,文章建议选择高矫顽力的Th2Zn17型(21kOe),而文章指出TbCu7型结构对于实用性磁体而言需要进一步提高矫顽力,需减小TbCu7型晶粒的尺寸。
发明内容
为此,本发明的目的之一在于提供一种高热稳定性的各向同性稀土永磁粉。本发明提供的稀土永磁粉具有耐温性、耐蚀性。
为达上述目的,本发明采用如下技术手段:
一种稀土永磁材料,以原子百分比所表示的组成成分为:
SmxRaFe100-x-y-z-aMyNz
其中R为Zr、Hf中的至少一种,M为Co、Ti、Nb、Cr、V、Mo、Si、Ga、Ni、Mn、Al中的至少一种,x+a为7~10%,a为0~1.5%,y为0~5%,z为10~14%。上述范围均包括端点值。其中N即为氮元素。
作为优选,所述稀土永磁材料含有TbCu7相、任选地Th2Zn17相和软磁相α-Fe。
作为优选,所述稀土永磁材料中TbCu7相的含量为50%以上,优选为80%以上,进一步优选为95%以上。
作为优选,所述稀土永磁材料中Th2Zn17相的含量为0~50%,不包括0,优选为1~50%。
作为优选,所述稀土永磁材料中软磁相α-Fe的含量为0~5%,不包括0。
作为优选,所述稀土永磁材料由平均尺寸为10nm~1μm,优选为10~200nm的晶粒组成。
本发明提供的稀土永磁材料的磁性能Hcj达到10kOe以上,磁能积BH在14MGOe以上。由本发明的稀土永磁材料制得的磁体不可逆磁通损失小于5%(其热稳定性能是通过粘结磁体的不可逆磁通损失来表征,120℃下空气中暴露2h)。
本发明的目的之二在于提供一种本发明所述的稀土永磁材料的制备方法,包括以下步骤:
(1)将Sm、R、Fe、M进行母合金熔炼;
(2)将步骤(1)所得母合金进行快淬制备快淬薄带;
(3)将步骤(2)所得快淬薄带进行晶化处理;
(4)将步骤(3)晶化后的永磁材料进行氮化得到所述稀土永磁材料。
为了从材料本身微观组织结构上设计改善各向同性钐铁氮磁粉的磁性能和热稳定性,本发明进行了研究并开发出一种低成本,工艺简单的晶化处理方法,引入高矫顽力第二相来提高磁粉的内禀矫顽力,因而获得一种有一定实际应用价值的钐铁氮磁粉。本发明中的各向同性钐铁氮磁粉主要通过快淬制备的钐铁薄带,经过热处理调整合金相结构,最后渗氮作用后得到。
作为优选,步骤(1)中熔炼通过中频或电弧等方式进行。
优选地,熔炼所得铸锭经过初破碎至毫米级铸锭块。
作为优选,步骤(2)中快淬过程如下:将母合金装入带喷嘴的石英管,经过感应熔炼熔化成合金液通过喷嘴喷射到旋转的水冷铜模上得到快淬薄带。
优选地,快淬时的轮速为20~80m/s,优选为40~50m/s。
优选地,所得快淬薄带的宽度为0.5~8mm,优选为1~4mm,厚度为10~40μm。
作为优选,步骤(3)中晶化处理过程如下:将快淬薄带包裹后进行热处理,然后淬火处理。
优选地,所述热处理在管式电阻炉中进行。
优选地,所述热处理在氩气氛围中进行。
优选地,所述淬火处理采用水冷的方式。
优选地,所述热处理的温度为700~900℃,时间为5min以上,优选为10~90min。
作为优选,步骤(3)中晶化处理后的材料进行破碎处理。
优选地,破碎至50目以上,优选为80目以上。
作为优选,步骤(4)中氮化在氮化炉中进行。
优选地,在1~2atm,优选为1.4atm高纯氮气氛围中进行。
优选地,氮化的温度为350~600℃,优选为430~470℃,时间为12h以上,优选为24h。
作为优选,本发明的稀土永磁材料的制备方法,包括以下步骤:
(1)按一定配比将钐铁以及掺杂元素单质金属配料,经过中频、电弧等方式进行熔炼均匀得到母合金铸锭,铸锭经过初破碎得到几个mm大小的铸锭块;
(2)将小块母合金铸锭装入带喷嘴的石英管,经过感应熔炼熔化成合金液通过喷嘴喷射到旋转的水冷铜模上,轮速40~50m/s,获得宽度为1~4mm,厚度10~40μm的快淬薄带;
(3)用钽薄将快淬SmFe薄带包裹后放入管式电阻炉进行热处理,温度为700~900℃,热处理时间为10~90min,在氩气氛围中,然后采用水冷的方式淬火处理;
(4)将步骤(3)得到的样品破碎至80目以上,用铁盅盛好放入氮化炉中,在1.4atm高纯氮气氛围中渗氮处理,温度430~470℃,时间24h,即得目标产品。
本发明的目的之三在于提供一种磁体,其包含本发明所述的稀土永磁材料。
优选地,所述磁体由本发明所述稀土永磁材料与粘结剂粘结而成。
优选地,所述磁体通过如下方法制备:将本发明的稀土永磁材料和环氧树脂混合得到混料,向混料中添加润滑剂,然后处理得到粘结磁体,最后将所得粘结磁体热固化。
优选地,稀土永磁材料和环氧树脂的重量比为100:1~10,优选为100:4。
优选地,所述润滑剂的添加量为0.2~1wt%,优选为0.5wt%。
优选地,所述处理为模压、注射、压延或挤出等方法
优选地,所述模压使用压片机进行。
制得的粘结磁体可以为块状,环状或其他形式。例如φ10×7mm的粘结磁体。
优选地,所述热固化的温度为150~200℃,优选为175℃,时间为0.5~5h,优选为1.5h。
本发明提供的稀土永磁材料具有优良的耐温性耐蚀性,有利于器件的进一步小型化,并有利于器件在特殊环境下的使用。本发明提供的稀土永磁材料的制备方法工艺简单,成本低,可提高制得的各向同性钐铁氮磁材料的实用价值。
具体实施方式
为便于理解本发明,本发明列举实施例如下。本领域技术人员应该明了,所述实施例仅仅用于帮助理解本发明,不应视为对本发明的具体限制。
需要说明的是,在不冲突的情况下,本申请中的实施例及实施例中的特征可以相互组合。下面结合实施例来详细说明本申请。
需要注意的是,这里所使用的术语仅是为了描述具体实施方式,而非意图限制根据本申请的示例性实施方式。如在这里所使用的,除非上下文另外明确指出,否则单数形式也意图包括复数形式,此外,还应当理解的是,当在本说明书中使用术语“包含”和/或“包括”时,其指明存在特征、步骤、操作、器件、组件和/或它们的组合。
本发明提供了一种稀土永磁材料,以原子百分比所表示的组成成分为:
SmxRaFe100-x-y-z-aMyNz
其中R为Zr、Hf中的至少一种,M为Co、Ti、Nb、Cr、V、Mo、Si、Ga、Ni、Mn、Al中的至少一种,x+a为7~10%,a为0~1.5%,y为0~5%,z为10~14%。上述范围均包括端点值。其中N即为氮元素。
本发明中稀土元素Sm含量对快淬SmFe合金薄带物相结构影响很大,Sm含量在7at%以下时容易形成软磁相,Sm含量在10at%以上时,容易形成富钐相,均不利于要求主相TbCu7结构95%以上的快淬合金的制备,且Zr或Hf可以取代Sm元素,取代量在1.5at%以下,M元素对Fe元素的取代则可拓宽形成TbCu7的Sm/Fe比例。而本发明优选Sm含量在7~10at%。
本发明提供的稀土永磁材料的磁性能Hcj达到10kOe以上,磁能积BH在14MGOe以上。由本发明的稀土永磁材料制得的磁体不可逆磁通损失小于5%(其热稳定性能是通过粘结磁体的不可逆磁通损失来表征,120℃下空气中暴露2h)。
本发明还提供了一种本发明所述的稀土永磁材料的制备方法,包括以下步骤:
(1)将Sm、R、Fe、M进行母合金熔炼;
(2)将步骤(1)所得母合金进行快淬制备快淬薄带;
(3)将步骤(2)所得快淬薄带进行晶化处理;
(4)将步骤(3)晶化后的永磁材料进行氮化得到所述稀土永磁材料。
在上述制备工艺中,关键的步骤为第(3)步骤快淬薄带的晶化处理,快淬SmFe合金中含TbCu7型SmFe9相、少量软磁相α-Fe和非晶,且组织中含有因过急冷时留下的空位和缺陷,晶化热处理一方面使非晶态的组织变成晶体组织,另一方面改善微观组织均匀性。在较低温度的晶化热处理过程中,TbCu7型结构形成的同时也产生少量的软磁相α-Fe,组织中晶粒相对细小,钐铁氮磁粉的剩磁和磁能积虽然较高,但是其矫顽力仍然较低。
发明人发现,在本实验条件下,晶化热处理温度较低,时间较短时,合金中的TbCu7型亚稳相向Th2Zn17型斜六方相转变量极少;而温度提高,处理时间增加,TbCu7型亚稳相向Th2Zn17型斜六方相转变量增加,但是同时软磁相α-Fe的比例也增加,将此类磁粉制备粘结磁体后,钐铁氮磁体的不可逆磁通损失得到减少。通过调整快淬SmFe晶化热处理的温度和处理时间,改善TbCu7型SmFe合金中的Th2Zn17型结构比例,可获得高热稳定性的钐铁氮磁性材料。
本发明中材料的主相为TbCu7型结构,具有该结构的钐铁氮磁粉的内禀磁性能比快淬NdFeB磁粉还要高,耐腐蚀性比其他磁粉也好。而TbCu7结构钐铁为亚稳相,其形成需要严格的成分控制和工艺条件控制,需要通过急冷的方式形成,但是在制备中也会出现其他结构的化合物,如ThMn12或者Th2Ni17或者Th2Zn17结构。熔体快淬制备钐铁合金一般为Th2Zn17结构,这种结构的磁粉尺寸需要达到微米级别,并在磁场取向成型才能获得较好的磁性能,通常Th2Zn17结构快淬磁粉的剩磁和磁能积很低,甚至小于8MGOe,但其矫顽力Hcj可以达到20kOe以上。TbCu7结构钐铁为亚稳相经过一定晶化热处理和渗氮处理可以向Th2Zn17结构转变,同时也会产生软磁相α-Fe,所以过高的热处理温度会导致过多稳定的Th2Zn17结构,大幅降低磁性能。本发明通过晶化工艺的优化,调整合金中Th2Zn17结构相和α-Fe软磁相的含量,规定α-Fe软磁相的含量在5%以下,Th2Zn17结构相在1%以上,TbCu7结构相为主相,含量在50%以上,因此优选晶化热处理温度为700~900℃。
本发明还规定了所述钐铁氮磁材料的平均厚度在10~40μm,由平均尺寸在10~200nm的纳米晶组成,由于快淬钐铁合金的厚度和制备方法有关,TbCu7型结构需要大的冷却速度,但过快的冷却速度并不利于薄带的形成,因此制备的钐铁合金的厚度在规定的适宜厚度;磁粉的晶粒尺寸直接影响磁性能,晶粒细小均匀的合金的矫顽力较高,磁粉的热稳定性也能提高,一般晶粒尺寸保持在10nm~1μm之间能保持磁粉获得较好的磁性能,为了磁粉达到较好的矫顽力水平,改善热稳定性,磁粉的晶粒尺寸优选在10~200nm。
实施例1~15
制备方法包括如下步骤:
(1)按表1中比例将各实施例列出的金属混合后放入感应熔炼炉中,在Ar气保护下进行熔炼得到合金铸锭;
(2)将合金铸锭粗破碎后放入快淬炉中进行快淬,保护气体为Ar气,喷射压力为80kPa,喷嘴直径为0.8,水冷辊线速度为20-80m/s,快淬后得到片状合金粉;
(3)将上述合金在Ar气保护下热处理后进入1个大气压的N2气下进行氮化处理,得到氮化物磁粉;晶化时的热处理和氮化处理条件见表2;
(4)将所得氮化物磁粉进行相比例及磁性能的检测。
表1
实施例 成分
1 Sm<sub>8.5</sub>Zr<sub>1.2</sub>Fe<sub>77.7</sub>Si<sub>1.0</sub>N<sub>11.6</sub>
2 Sm<sub>8.5</sub>Zr<sub>1.2</sub>Fe<sub>76.9</sub>Al<sub>1.0</sub>N<sub>12.4</sub>
3 Sm<sub>8.5</sub>Zr<sub>1.2</sub>Fe<sub>79.2</sub>Mn<sub>1.0</sub>N<sub>10.1</sub>
4 Sm<sub>8.5</sub>Zr<sub>1.2</sub>Fe<sub>72.3</sub>Co<sub>4.5</sub>N<sub>13.5</sub>
5 Sm<sub>8.5</sub>Zr<sub>1.2</sub>Fe<sub>73.3</sub>Co<sub>4.5</sub>N<sub>12.5</sub>
6 Sm<sub>8.5</sub>Hf<sub>1.2</sub>Fe<sub>74.3</sub>Co<sub>4.5</sub>N<sub>11.5</sub>
7 Sm<sub>8.5</sub>Zr<sub>1.2</sub>Fe<sub>82.8</sub>Co<sub>4.5</sub>Nb<sub>1.2</sub>N<sub>1.8</sub>
8 Sm<sub>8.5</sub>Zr<sub>1.2</sub>Fe<sub>73.4</sub>Co<sub>4.5</sub>Ti<sub>1.2</sub>N<sub>11.2</sub>
9 Sm<sub>8.5</sub>Zr<sub>1.2</sub>Fe<sub>73.8</sub>Co<sub>4.5</sub>Mo<sub>1.2</sub>N<sub>10.8</sub>
10 Sm<sub>8.5</sub>Hf<sub>1.2</sub>Fe<sub>73.7</sub>Ni<sub>4.5</sub>N<sub>12.1</sub>
11 Sm<sub>8.5</sub>Zr<sub>1.2</sub>Fe<sub>77.6</sub>Ga<sub>0.3</sub>N<sub>12.4</sub>
12 Sm<sub>8.5</sub>Zr<sub>1.2</sub>Fe<sub>75.8</sub>V<sub>1.5</sub>N<sub>13</sub>
13 Sm<sub>8.5</sub>Zr<sub>1.2</sub>Fe<sub>75.3</sub>Nb<sub>1.5</sub>N<sub>13.5</sub>
14 Sm<sub>8.5</sub>Zr<sub>1.2</sub>Fe<sub>78.3</sub>Cr<sub>1.5</sub>N<sub>10.5</sub>
15 Sm<sub>8.5</sub>Zr<sub>1.2</sub>Fe<sub>74.9</sub>Cr<sub>1.5</sub>N<sub>13.9</sub>
表2
Figure BDA0001248766780000101
Figure BDA0001248766780000111
性能测试
将实施例1~15所得永磁材料进行性能测试,测试结果见下表3。
表3
Figure BDA0001248766780000112
Figure BDA0001248766780000121
2h@120FL%是在120℃空气中暴露2h的不可逆磁通损失。
实施例制得磁粉的高热稳定性通过其粘结磁体的不可逆磁通损失表征,将粘结磁体在25~120℃空气中暴露2h。
从表2中可以看出,实施例1和9中TbCu7型相、Th2Zn17型相、α-Fe相的比例不在本发明权利要求优选范围呢,性能稍差些。其余实施例制得的磁粉的不可逆磁通损失基本在5%以下,磁性能Hcj基本达到10kOe以上,磁能积BH在12MGOe以上。
显然,上述实施例仅仅是为清楚地说明所作的举例,而并非对实施方式的限定。对于所属领域的普通技术人员来说,在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引伸出的显而易见的变化或变动仍处于本发明创造的保护范围之中。

Claims (31)

1.一种稀土永磁材料,其特征在于,所述稀土永磁材料以原子百分比所表示的组成成分为:
SmxRaFe100-x-y-z-aMyNz
其中R为Zr、Hf中的至少一种,M为Co、Ti、Nb、Cr、V、Mo、Ga、Ni、Mn、Al中的至少一种,x+a为7~10%,a为0~1.5%,y为0~5%,z为10~14%;其中,a和y不为0;
所述稀土永磁材料含有TbCu7相、Th2Zn17相和软磁相α-Fe;
所述稀土永磁材料中TbCu7相的含量为80%以上;所述稀土永磁材料中软磁相α-Fe的含量为0~5%,不包括0。
2.根据权利要求1所述的稀土永磁材料,其特征在于,所述稀土永磁材料中TbCu7相的含量为95%以上。
3.根据权利要求1所述的稀土永磁材料,其特征在于,所述稀土永磁材料中Th2Zn17相的含量为0~50%,不包括0。
4.根据权利要求3所述的稀土永磁材料,其特征在于,所述稀土永磁材料中Th2Zn17相的含量为1~20%。
5.根据权利要求1所述的稀土永磁材料,其特征在于,所述稀土永磁材料由平均尺寸为10nm~1μm的晶粒组成。
6.根据权利要求5所述的稀土永磁材料,其特征在于,所述稀土永磁材料由平均尺寸为10~200nm的晶粒组成。
7.一种权利要求1-6任一项 所述的稀土永磁材料的制备方法,包括以下步骤:
(1)将Sm、R、Fe、M进行母合金熔炼;
(2)将步骤(1)所得母合金进行快淬制备快淬薄带;
(3)将步骤(2)所得快淬薄带进行晶化处理;
(4)将步骤(3)晶化后的永磁材料进行氮化得到所述稀土永磁材料。
8.根据权利要求7所述的制备方法,其特征在于,步骤(1)中熔炼通过中频或电弧进行。
9.根据权利要求8所述的制备方法,其特征在于,熔炼所得铸锭经过初破碎至毫米级铸锭块。
10.根据权利要求7-9任一项所述的制备方法,其特征在于,步骤(2)中快淬过程如下:将母合金装入带喷嘴的石英管,经过感应熔炼熔化成合金液通过喷嘴喷射到旋转的水冷铜模上得到快淬薄带。
11.根据权利要求10所述的制备方法,快淬时的轮速为20~80m/s。
12.根据权利要求11所述的制备方法,快淬时的轮速为40~50m/s。
13.根据权利要求7-9任一项所述的制备方法,其特征在于,步骤(3)中晶化处理过程如下:将快淬薄带包裹后进行热处理,然后淬火处理。
14.根据权利要求13所述的制备方法,其特征在于,所述热处理在管式电阻炉中进行;所述热处理在氩气氛围中进行;所述淬火处理采用水冷的方式。
15.根据权利要求14所述的制备方法,其特征在于,所述热处理的温度为700~900℃,时间为5min以上。
16.根据权利要求15所述的制备方法,其特征在于,所述热处理的时间为10~90min。
17.根据权利要求7-9任一项所述的制备方法,其特征在于,步骤(3)中晶化处理后的材料进行破碎处理;破碎至50目以上。
18.根据权利要求17所述的制备方法,其特征在于,破碎至80目以上。
19.根据权利要求7-9任一项所述的制备方法,其特征在于,步骤(4)中氮化在氮化炉中进行;在1~2atm高纯氮气氛围中进行。
20.根据权利要求19所述的制备方法,其特征在于,在1.4atm高纯氮气氛围中进行。
21.根据权利要求19所述的制备方法,其特征在于,氮化的温度为350~600℃,时间为12h以上。
22.根据权利要求21所述的制备方法,其特征在于,氮化的温度为430~470℃,时间为24h。
23.一种磁体,其特征在于,所述磁体包含权利要求1-6任一项所述的稀土永磁材料。
24.根据权利要求23所述的磁体,其特征在于,所述磁体由所述稀土永磁材料与粘结剂粘结而成。
25.根据权利要求24所述的磁体,其特征在于,所述磁体通过如下方法制备:将所述稀土永磁材料和环氧树脂混合得到混料,向混料中添加润滑剂,然后处理得到粘结磁体,最后将所得粘结磁体热固化。
26.根据权利要求25所述的磁体,其特征在于,稀土永磁材料和环氧树脂的重量比为100:1~10。
27.根据权利要求26所述的磁体,其特征在于,稀土永磁材料和环氧树脂的重量比为100:4。
28.根据权利要求25所述的磁体,其特征在于,所述润滑剂的添加量为0.2~1wt%。
29.根据权利要求28所述的磁体,其特征在于,所述润滑剂的添加量为为0.5wt%。
30.根据权利要求25所述的磁体,其特征在于,所述处理为模压、注射、压延或挤出;所述模压使用压片机进行;所述热固化的温度为150~200℃,时间为0.5~5h。
31.根据权利要求30所述的磁体,其特征在于,所述热固化的温度为175℃,时间为1.5h。
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