CN108913986A - 一种高耐蚀性纳米晶稀土永磁材料及其制备方法 - Google Patents
一种高耐蚀性纳米晶稀土永磁材料及其制备方法 Download PDFInfo
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- 229910052735 hafnium Inorganic materials 0.000 claims abstract description 6
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 5
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- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 3
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- 229910052796 boron Inorganic materials 0.000 claims description 8
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- 230000000052 comparative effect Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 2
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Abstract
本发明公开了一种高耐蚀性的纳米晶稀土永磁材料及其制备方法,其中制备方法包括如下步骤:(1)制备快淬(PraNd1‑a)bFe100‑b‑c‑dBcMd粉末,其中M为Hf元素或Zr、Hf两种元素,0≤a≤1,16≤b≤20,6≤c≤8,1.5≤d≤3;其中部分Pr、Nd元素可由Dy、Tb、Ho、Gd等替代,部分Fe元素可由Co替代;(2)将上述粉料进行放电等离子烧结,获得具有高耐蚀性的纳米晶稀土永磁材料。本发明利用成分优化的快淬合金粉末,改善了永磁体的磁性能和耐腐蚀性能。此外,本发明还具有烧结时间短,工艺流程简单的特点,后续可通过热变形技术制备得到各向异性的纳米晶稀土永磁材料,从而进一步提升磁体的磁性能。
Description
技术领域
本发明属于稀土永磁材料领域,特别提供一种高耐蚀性的纳米晶稀土 永磁材料及其制备方法。
背景技术
Nd2Fe14B类稀土永磁材料由于其优异的磁性能,号称“磁王”,自发明 以来便被广泛的应用于许多领域。它已成为使用范围最为广泛的一种稀土 功能材料,被认为是高新技术及社会进步的物质基础之一。风力发电是通 过风力发电机组将风能转换为电能的发电方式,是目前风能利用的主要途 径。随着海上风力发电机、深海潮汐发电机等应用领域的快速增长,对烧 结钕铁硼磁体的耐蚀性能也提出了更高的要求。
钕铁硼磁体中除2:14:1主相外,还需含有一定量的晶间富稀土相,从 而增强主相晶粒之间的去磁耦合作用,保证磁体的矫顽力。富稀土相的标 准电化学电位比主相低,电化学活性高,在电化学环境下会优先发生腐蚀。 对于沙漠或沿海地区的风力发电类电机,磁钢多暴露于恶劣环境之中,磁 体的腐蚀快慢程度直接决定了此类器件的使用寿命。表面处理可以减缓恶 劣环境对磁体的腐蚀速率,但大大提高了磁体的生产成本。此外,表面处理工艺往往产生大量废液和废气,带来环境污染问题。因此,提高磁体基 体的耐腐蚀性也一直受到钕铁硼制备厂家和应用企业的广泛关注。合金化 是改善磁体基体耐腐蚀性能的主要方法。合理的成分设计可提高磁体基体 的耐腐蚀性能。
发明内容
本发明的目的在于通过成分的优化,改善磁钢基体的耐腐蚀性能,从 而进一步提高磁性器件的使用寿命。
本发明技术方案如下:
一种高耐蚀性纳米晶稀土永磁材料,其特征在于:其成分及含量用公 式表示为:(PraNd1-a)bFe100-b-c-dBcMd,其中M为Hf元素或Zr、Hf两种元素, 0≤a≤1,16≤b≤20,6≤c≤8,0.5≤d≤3(优选为0≤a≤1,17≤b≤18,6.5≤c≤7, 2≤d≤2.5)。
其中,(PraNd1-a)bFe100-b-c-dBcMd成分中部分(优选5%-20%,原子百分比) Pr、Nd元素可由Dy、Tb、Ho、Gd之一种或多种替代,部分(优选20%-60%, 原子百分比)Fe元素可由Co替代。
本发明还提供了所述高耐蚀性纳米晶复合永磁材料的制备方法,其特 征在于:将(PraNd1-a)bFe100-b-c-dBcMd粉末通过放电等离子烧结技术制备得到 纳米晶永磁体,放电等离子烧结前及整个烧结过程真空度小于10Pa,烧结 温度为600~850℃,烧结压力为20~100MPa,烧结时间为0~20min;作为优 选的技术方案,放电等离子烧结温度为650~750℃,烧结压力为60~80MPa, 烧结时间为3~10min。
采用该方法制备得到的永磁材料中主相晶粒尺寸在纳米级别。本发明 微量Hf元素的添加有效改善了磁体的磁性能和耐腐蚀性能。
本发明所述高耐蚀性纳米晶复合永磁材料的制备方法,其特征在于, 具体步骤如下:
①、快淬磁粉的制备:将元素Pr、Nd、Fe、B、M按照要求配比,其 中部分Pr、Nd元素可由Dy、Tb、Ho、Gd等替代,部分Fe元素可由Co 替代;将配好的原材料放入电弧炉中,在氩气气氛下进行熔炼得到母合金 铸锭,并通过熔体快淬的方式制备得到快淬合金带材,其中甩带机辊速为 12-18m/s,在气氛保护下将合金带破碎成粉末,得到(PraNd1-a)bFe100-b-c-dBcMd粉末;
②、放电等离子烧结:将(PraNd1-a)bFe100-b-c-dBcMd粉末倒入石墨模具中, 利用放电等离子烧结设备进行真空烧结,制备得到纳米晶稀土永磁材料。
本发明通过微量Hf元素的添加优化合金成分,采用放电等离子快速烧 结技术制备得到了高耐蚀性的纳米晶稀土永磁体。放电等离子烧结技术可 在较低温度、较短时间内快速实现磁体的致密化,可最大程度抑制晶粒的 异常长大,有利于保持晶粒的纳米晶形态,所得磁体的耐腐蚀性能优于传 统烧结磁体和未改善成分前的纳米晶稀土永磁体,磁体的磁性能也有所改 善。本发明烧结时间短,工艺流程简单,磁体致密度高,耐腐蚀性能强,后续可通过热变形技术制备得到各向异性的纳米晶稀土永磁材料,从而进 一步提升磁体的磁性能。
具体实施方式
以下结合实施例对本发明作进一步详细描述,但本发明不限于这些实 施例,以下实施例只为说明目的,不应当被用来限制本发明以及权利要求 的范围。
实施例1
将元素Pr、Nd、Fe、B、Hf按照(Pr0.2Nd0.8)16Fe76.5B6Hf1.5配比,将配好 的原材料放入电弧炉中在氩气气氛下进行熔炼得到合金铸锭,并通过熔体 快淬的方式制备得到快淬合金带材,其中甩带机辊速为18m/s,在氩气保护 下将合金带破碎成粉末;将(Pr0.2Nd0.8)16Fe76.5B6Hf1.5粉末倒入石墨模具中, 通过放电等离子烧结设备快速烧结制得磁体。烧结前及整个烧结过程真空 度小于10Pa,烧结温度为700℃,烧结压力为50MPa,烧结时间为5min。此烧结样品记为1号样。
磁体在3.5wt.%NaCl溶液中的自腐蚀电位和自腐蚀电流密度列于表1。
对比例1
将元素Pr、Nd、Fe、B按照(Pr0.2Nd0.8)16Fe78B6配比,将配好的原材料 放入电弧炉中在氩气气氛下进行熔炼得到合金铸锭,并通过熔体快淬的方 式制备得到快淬合金带材,其中甩带机辊速为19m/s,在氩气保护下将合金 带破碎成粉末;将(Pr0.2Nd0.8)16Fe78B6粉末倒入石墨模具中,通过放电等离子 烧结设备快速烧结制得磁体。烧结前及整个烧结过程真空度小于10Pa,烧 结温度为700℃,烧结压力为50MPa,烧结时间为5min。此烧结样品记为 2号样。
磁体在3.5wt.%NaCl溶液中的自腐蚀电位和自腐蚀电流密度列于表1。
实施例2
将元素Pr、Nd、Fe、B、Hf按照(Pr0.25Nd0.75)18Fe72B8Hf2配比,将配好 的原材料放入电弧炉中在氩气气氛下进行熔炼得到合金铸锭,并通过熔体 快淬的方式制备得到快淬合金带材,其中甩带机辊速为16m/s,在氩气保护 下将合金带破碎成粉末;将(Pr0.25Nd0.75)18Fe72B8Hf2粉末倒入石墨模具中,通 过放电等离子烧结设备快速烧结制得磁体。烧结前及整个烧结过程真空度 小于10Pa,烧结温度为700℃,烧结压力为60MPa,烧结时间为5min。此烧结样品记为3号样。
磁体在3.5wt.%NaCl溶液中的自腐蚀电位和自腐蚀电流密度列于表1。
对比例2
将元素Pr、Nd、Fe、B按照(Pr0.25Nd0.75)18Fe74B8配比,将配好的原材料 放入电弧炉中在氩气气氛下进行熔炼得到合金铸锭,并通过熔体快淬的方 式制备得到快淬合金带材,其中甩带机辊速为19m/s,在氩气保护下将合金 带破碎成粉末;将(Pr0.25Nd0.75)18Fe74B8粉末倒入石墨模具中,通过放电等离 子烧结设备快速烧结制得磁体。烧结前及整个烧结过程真空度小于10Pa, 烧结温度为700℃,烧结压力为60MPa,烧结时间为5min。此烧结样品记为4号样。
磁体在3.5wt.%NaCl溶液中的自腐蚀电位和自腐蚀电流密度列于表1。
实施例3
将元素Pr、Fe、B、Hf按照Pr17Fe75B6Zr0.5Hf1.5配比,将配好的原材料 放入电弧炉中在氩气气氛下进行熔炼得到合金铸锭,并通过熔体快淬的方 式制备得到快淬合金带材,其中甩带机辊速为16m/s,在氩气保护下将合 金带破碎成粉末;将Pr17Fe75B6Zr0.5Hf1.5粉末倒入石墨模具中,通过放电等 离子烧结设备快速烧结制得磁体。烧结前及整个烧结过程真空度小于10Pa, 烧结温度为750℃,烧结压力为40MPa,烧结时间为6min。此烧结样品记 为5号样。
磁体在3.5wt.%NaCl溶液中的自腐蚀电位和自腐蚀电流密度列于表1。
对比例3
将元素Pr、Fe、B按照Pr17Fe77B6配比,将配好的原材料放入电弧炉中 在氩气气氛下进行熔炼得到合金铸锭,并通过熔体快淬的方式制备得到快 淬合金带材,其中甩带机辊速为18m/s,在氩气保护下将合金带破碎成粉末; 将Pr17Fe77B6粉末倒入石墨模具中,通过放电等离子烧结设备快速烧结制得 磁体。烧结前及整个烧结过程真空度小于10Pa,烧结温度为750℃,烧结 压力为40MPa,烧结时间为6min。此烧结样品记为6号样。
磁体在3.5wt.%NaCl溶液中的自腐蚀电位和自腐蚀电流密度列于表1。
表1不同成分烧结磁体在3.5wt.%NaCl溶液中的自腐蚀电位和自腐蚀 电流密度
从表1可以看出,添加Hf元素的磁体在3.5wt.%NaCl溶液中的自腐蚀 电位和自腐蚀电流密度的绝对值均比对比磁体的自腐蚀电位和自腐蚀电流 密度的绝对值小,意味着添加Hf元素的磁体具有更优异的耐腐蚀性能。因 此,本发明通过微量Hf元素的添加,并优化各元素的配比,在提高磁体磁 性能的同时,进一步改善了磁体的耐蚀性,制备得到了一种高耐蚀性的纳 米晶稀土永磁材料。
上述实施例只为说明本发明的技术构思及特点,其目的在于让熟悉此 项技术的人士能够了解本发明的内容并据以实施,并不能以此限制本发明 的保护范围。凡根据本发明精神实质所作的等效变化或修饰,都应涵盖在 本发明的保护范围之内。
Claims (8)
1.一种高耐蚀性纳米晶稀土永磁材料,其特征在于:其成分及含量用公式表示为:(PraNd1-a)bFe100-b-c-dBcMd,其中M为Hf元素或Zr、Hf两种元素,0≤a≤1,16≤b≤20,6≤c≤8,1.5≤d≤3。
2.按照权利要求1所述高耐蚀性纳米晶稀土永磁材料,其特征在于:(PraNd1-a)bFe100-b-c-dBcMd成分中0≤a≤1,17≤b≤18,6.5≤c≤7,2≤d≤2.5。
3.按照权利要求1或2所述高耐蚀性纳米晶稀土永磁材料,其特征在于:(PraNd1-a)bFe100-b-c-dBcMd成分中部分的Pr、Nd元素由Dy、Tb、Ho、Gd之一种或多种替代,部分Fe元素由Co替代。
4.按照权利要求3所述高耐蚀性纳米晶稀土永磁材料,其特征在于:(PraNd1-a)bFe100-b-c-dBcMd成分中5%-20%的Pr、Nd元素由Dy、Tb、Ho、Gd之一种或多种替代,20%-60%的Fe元素由Co替代。
5.一种权利要求1所述高耐蚀性纳米晶稀土永磁材料的制备方法,其特征在于:将(PraNd1-a)bFe100-b-c-dBcMd粉末通过放电等离子烧结技术制备得到纳米晶永磁体,放电等离子烧结前及整个烧结过程真空度小于10Pa,烧结温度为600~850℃,烧结压力为20~100MPa,烧结时间为0~20min。
6.按照权利要求5所述高耐蚀性纳米晶稀土永磁材料的制备方法,其特征在于:放电等离子烧结温度为650~750℃,烧结压力为60~80MPa,烧结时间为3~10min。
7.按照权利要求5所述高耐蚀性纳米晶稀土永磁材料的制备方法,其特征在于,(PraNd1-a)bFe100-b-c-dBcMd粉末的制备方法为:将元素Pr、Nd、Fe、B、M按照要求配比,将配好的原材料放入电弧炉中,在氩气气氛下进行熔炼得到母合金铸锭,并通过熔体快淬的方式制备得到快淬合金带材,其中甩带机辊速为12-18m/s,在气氛保护下将合金带破碎成粉末,得到(PraNd1-a)bFe100-b-c-dBcMd粉末。
8.按照权利要求5所述高耐蚀性纳米晶稀土永磁材料的制备方法,其特征在于:所得永磁材料中主相晶粒尺寸在纳米级别。
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