CN114864259B - 通过1:2相提高混合稀土永磁材料抗蚀性的多元晶界重构方法 - Google Patents

通过1:2相提高混合稀土永磁材料抗蚀性的多元晶界重构方法 Download PDF

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CN114864259B
CN114864259B CN202210393701.0A CN202210393701A CN114864259B CN 114864259 B CN114864259 B CN 114864259B CN 202210393701 A CN202210393701 A CN 202210393701A CN 114864259 B CN114864259 B CN 114864259B
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金佳莹
陈望
周良
俞钧耀
严密
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Zhejiang University ZJU
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Abstract

本发明公开一种通过1:2相提高混合稀土永磁材料抗蚀性的多元晶界重构方法。本发明使用多合金工艺，其中主合金富Ce，辅合金为稀土氢化物和稀土金属多元合金，旨在通过多元晶界重构方法，在烧结和热处理过程中形成高化学稳定性的1:2晶界相，取代低化学稳定性的传统富稀土晶界相，提高混合稀土永磁材料的抗蚀性。本发明提供了一种适用于低成本混合稀土永磁材料的多元晶界重构方法，充分利用不同稀土元素的扩散和偏析行为，在大幅降低原材料成本的同时，解决了长期以来混合稀土永磁材料的低抗蚀性难题。

Description

通过1:2相提高混合稀土永磁材料抗蚀性的多元晶界重构 方法
技术领域
本发明涉及稀土永磁材料领域，具体涉及通过1:2相提高混合稀土永磁材料抗蚀性的多元晶界重构方法。
背景技术
钕铁硼稀土永磁材料具有优异的综合磁性能，广泛应用于能源、信息、交通和国防等领域，是最重要的稀土功能材料和国民经济的关键基础材料。钕铁硼具有多相结构，除了提供内禀铁磁性的Nd2Fe14B主相，富Nd晶界相的形态和分布也显著影响磁体性能。富Nd相电极电位远低于主相，在腐蚀介质中作为阳极优先溶解，呈现“小阳极大阴极”晶间腐蚀，磁体抗蚀性因而很差。近年来，钕铁硼年消耗稀土总用量的40％，导致我国稀土资源的利用极不平衡，Nd/Pr/Dy/Tb等需求量大，价格昂贵，而La/Ce/Y等高丰度稀土极少使用，大量积压。上述问题难以解决，长期制约了钕铁硼的发展和应用。
(La/Ce/Y)2Fe14B四方相内禀磁性远低于Nd2Fe14B，富La/Ce/Y磁体磁稀释效应显著，是限制La/Ce/Y应用的主要问题。针对高丰度稀土永磁磁性能和廉价稀土用量偏低的现状，通过NdHx和NdPrHx等晶界重构，在Nd-Ce-Fe-B磁体主相晶粒边界层形成富Pr/Nd的硬磁壳层，增强局域磁晶各向异性，可改善磁体的矫顽力，如公告号为CN106252009A的中国发明专利。但引入大量非磁性富稀土晶界相后，不仅降低了剩磁和最大磁能积，而且形成了更多的腐蚀通道，磁体的抗腐蚀性能严重恶化。因此，如何解决矫顽力和抗腐蚀性能之间的矛盾，不以牺牲抗蚀性为代价提高矫顽力，已成为限制高丰度稀土永磁材料发展的关键难题。
发明内容
有鉴于此，为解决现有技术中存在的不足，本发明提供了一种通过1:2相提高混合稀土永磁材料抗蚀性的多元晶界重构方法，充分利用多元晶界重构过程中不同稀土元素的扩散和偏析行为，充分发挥混合稀土永磁材料体系中1:2相的作用，实现抗蚀性的提高。
为实现上述目的，本发明提供了如下的技术方案：
通过1:2相提高混合稀土永磁材料抗蚀性的多元晶界重构方法，包括如下步骤：
1)制备主合金粉末，粒径为2.0～3.8μm；
2)制备辅合金粉末，包括稀土氢化物粉末和稀土金属多元合金粉末；
3)主合金粉末和辅合金粉末均匀混合后进行磁场取向压型和等静压，得到生坯，其中，辅合金粉末占磁体总重量的0.2～8％；
4)对生坯进行真空烧结和热处理；
5)最终得到高1:2相含量的高抗蚀混合稀土永磁材料；
其中主合金富Ce，以质量百分数计，成分为(CeaNdbREcRE’1-a-b-c)xFe100-x-y-zMyBz，Ce为铈元素，Nd为钕元素，RE为La、Y、Gd、Pr中的一种或者几种，RE’为除去Ce、Nd、La、Y、Gd、Pr以外的其它镧系元素或者Sc中的一种或者几种，Fe为铁元素，M为Al、C、Co、Cr、Cu、F、Ga、Mn、Mo、N、Nb、Ni、P、Pb、S、Si、Ta、Ti、V、W、Zn、Zr元素中的一种或几种，B为硼元素；a、b、c、x、y、z分别满足以下关系：0.3≤a≤0.9，0≤b≤0.6，0.1≤c≤0.7，26≤x≤35，0.5≤y≤2.5，0.75≤z≤1.35；
其中辅合金中稀土氢化物以质量百分数计，成分为RE”1-uHu，RE”为镧系元素或者Sc或者Y中的一种或者几种，H为氢元素，0＜u≤0.05；辅合金中稀土金属多元合金以质量百分数计，成分为R1-vM’v，R为Nd、Pr、Dy、Tb、Ho、Gd、Ce、La、Y中的一种或者几种，M’为Fe、Ga、Cu、Co、Ni、Al元素中的一种或者几种，0.05≤v＜1。
优选地：主合金富Ce，为单一成分的主合金，或多种不同成分的主合金。
优选地：多种不同成分的主合金，其平均成分与单一成分的主合金的成分相同。
优选地：步骤4)中的真空烧结温度为900～1100℃，烧结时间为2～5h；热处理温度为400～900℃，热处理时间为0～12h。
优选地：步骤4)中的热处理为一级热处理，或多级循环热处理。
本发明与现有技术相比的有益效果：
1)主合金富Ce，利用高丰度、廉价的Ce取代紧缺的Nd/Pr/Dy/Tb等稀土元素，不仅大幅降低原材料成本，更重要的是，充分利用了CeFeB与NdFeB等体系成相规律的差异。发明人经过大量实验发现，本发明成分区间富Ce稀土永磁材料中会形成1:2相，1:2相的电极电位较高，与2:14:1主相电位更相近，因此引入1:2相可提高富Ce磁体的抗蚀性。
2)进一步地，主合金成分设计中除了Ce和Nd，还包括La、Y、Gd、Pr中的一种或者几种等，即多元稀土共存，这种混合稀土永磁材料的成分设计，关乎不同稀土元素的占位和成相，可充分发挥稀土元素间的交互效应，以及稀土元素-合金元素间的交互效应，在多元晶界重构过程中促进1:2晶界相的形成。
3)更进一步地，本发明创新提出了多元晶界重构方法，稀土氢化物高温脱氢活化后加速稀土元素的互扩散，稀土金属多元合金在本发明中起关键作用，一方面调控各相间的成分梯度，另一方面提供有效的扩散通道，在烧结和热处理过程中为1:2晶界相的形成提供大的驱动力，更多1:2相凝固析出。
4)新形成的1:2晶界相化学稳定性高，取代低化学稳定性的传统富稀土晶界相，延缓了腐蚀介质沿晶界向磁体内部渗入，抑制了裂纹的沿晶扩展，提高了混合稀土永磁材料的抗蚀性。即使磁体表层的富稀土晶界相全部被腐蚀，未被腐蚀的1:2连续晶界相仍可连接相邻的主相晶粒，使其不分离不脱落，从而维持磁体的完整性。最终本发明提供了1:2晶界相含量更高的高抗蚀混合稀土永磁材料。
5)本发明提供了一种适用于低成本混合稀土永磁材料的多元晶界重构方法，充分利用不同稀土元素的扩散和偏析行为，在大幅降低原材料成本的同时，解决了长期以来混合稀土永磁材料的低抗蚀性难题。这对于高丰度混合稀土永磁材料的商业化推广应用，尤其是在海洋船舶等腐蚀环境中的应用具有重要意义。
具体实施方式
下面结合具体实施例对本发明做进一步说明，但本发明并不仅仅局限于以下实施例：
实施例1：
1)制备主合金粉末，粒径为3.0μm，以质量百分数计，成分为(Ce0.3Nd0.6La0.1)30.1Febal(Al0.4Cu0.3Zr0.15Mo0.1Cr0.05)1.4B1.02；
2)制备辅合金粉末，其中稀土氢化物粉末，以质量百分数计，成分为(Pr0.8Nd0.2)0.98H0.02；稀土金属多元合金粉末，以质量百分数计，成分为(Pr0.8Nd0.2)0.7Cu0.25Fe0.05；
3)主合金粉末和辅合金粉末均匀混合后进行磁场取向压型和等静压，得到生坯，其中，辅合金粉末占磁体总重量的2％；
4)对生坯进行真空烧结和热处理，真空烧结温度为1050℃，烧结时间为4h；热处理温度为660℃，热处理时间为4h；
5)最终得到高抗蚀混合稀土永磁材料。慢扫XRD精修结果显示，磁体的1:2相含量为4.6wt.％。在湿热环境中(100％相对湿度，两个大气压，120℃)暴露96h后，磁体的质量损失为1.1mg/cm3。
对比例1：
与实施例1的不同之处在于，磁体未经多元晶界重构处理。慢扫XRD精修结果显示，未处理磁体的1:2相含量为2.4wt.％，小于实施例1。在湿热环境中(100％相对湿度，两个大气压，120℃)暴露96h后，未处理磁体的质量损失为11.5mg/cm3，远大于实施例1。
对比例2：
与实施例1的不同之处在于，磁体经稀土氢化物晶界重构处理，即辅合金仅为(Nd0.8Pr0.2)0.98H0.02。慢扫XRD精修结果显示，磁体的1:2相含量为2.1wt.％，小于实施例1。在湿热环境中(100％相对湿度，两个大气压，120℃)暴露96h后，磁体的质量损失为38.2mg/cm3，远大于实施例1。
对比例3：
与实施例1的不同之处在于，磁体经稀土金属多元合金晶界重构处理，即辅合金仅为(Nd0.8Pr0.2)0.7Cu0.25Fe0.05。慢扫XRD精修结果显示，磁体的1:2相含量为2.8wt.％，小于实施例1。在湿热环境中(100％相对湿度，两个大气压，120℃)暴露96h后，磁体的质量损失为13.5mg/cm3，远大于实施例1。
实施例2：
1)制备主合金粉末，粒径为3.3μm，以质量百分数计，成分为(Ce0.5Nd0.25Y0.15La0.05Gd0.05)31.0Febal(Co0.35Cu0.3Nb0.2Al0.1Si0.05)1.5B1.05；
2)制备辅合金粉末，其中稀土氢化物粉末，以质量百分数计，成分为(Pr0.65Y0.35)0.97H0.03；稀土金属多元合金粉末，以质量百分数计，成分为(Pr0.65Y0.35)0.5Cu0.25Fe0.25；
3)主合金粉末和辅合金粉末均匀混合后进行磁场取向压型和等静压，得到生坯，其中，辅合金粉末占磁体总重量的3％；
4)对生坯进行真空烧结和热处理，真空烧结温度为1030℃，烧结时间为5h；一级热处理温度为820℃，一级热处理时间为3h；二级热处理温度为520℃，二级热处理时间为4h；
5)最终得到高抗蚀混合稀土永磁材料。慢扫XRD精修结果显示，磁体的1:2相含量为8.7wt.％。在湿热环境中(100％相对湿度，两个大气压，120℃)暴露96h后，磁体的质量损失为0.8mg/cm3。
对比例4：
与实施例2的不同之处在于，磁体未经多元晶界重构处理。慢扫XRD精修结果显示，未处理磁体的1:2相含量为5.4wt.％，小于实施例2。在湿热环境中(100％相对湿度，两个大气压，120℃)暴露96h后，未处理磁体的质量损失为15.5mg/cm3，远大于实施例2。
实施例3：
1)制备主合金粉末，粒径为3.4μm，以质量百分数计，成分为(Ce0.65Nd0.15La0.1Ho0.1)30.5Febal(Al0.3Ga0.3Zr0.15Cu0.1Ti0.1Ta0.05)2.0B0.95；
2)制备辅合金粉末，其中稀土氢化物粉末，以质量百分数计，成分为(Pr0.75Ce0.25)0.98H0.02；稀土金属多元合金粉末，以质量百分数计，成分为(Pr0.75Ce0.25)0.45Fe0.45Al0.1；
3)主合金粉末和辅合金粉末均匀混合后进行磁场取向压型和等静压，得到生坯，其中，辅合金粉末占磁体总重量的5％；
4)对生坯进行真空烧结和热处理，真空烧结温度为1000℃，烧结时间为3.5h；热处理温度为650℃，热处理时间为6h；
5)最终得到高抗蚀混合稀土永磁材料。慢扫XRD精修结果显示，磁体的1:2相含量为16.8wt.％。在湿热环境中(100％相对湿度，两个大气压，120℃)暴露96h后，磁体的质量损失为0.5mg/cm3。
对比例5：
与实施例3的不同之处在于，磁体未经多元晶界重构处理。慢扫XRD精修结果显示，未处理磁体的1:2相含量为11.0wt.％，小于实施例3。在湿热环境中(100％相对湿度，两个大气压，120℃)暴露96h后，未处理磁体的质量损失为9.6mg/cm3，远大于实施例3。

Claims (4)

1.通过1:2相提高混合稀土永磁材料抗蚀性的多元晶界重构方法，其特征在于，包括如下步骤：
1） 制备主合金粉末，粒径为2.0~3.8μm；
2）制备辅合金粉末，包括稀土氢化物粉末和稀土金属多元合金粉末；
3）主合金粉末和辅合金粉末均匀混合后进行磁场取向压型和等静压，得到生坯，其中，辅合金粉末占磁体总重量的0.2~8%;
4） 对生坯进行真空烧结和热处理；
5） 最终得到高1:2相含量的高抗蚀混合稀土永磁材料；
其中主合金富Ce，以质量百分数计，成分为(CeaNdbREcRE’1-a-b-c)xFe100-x-y-zMyBz，Ce为铈元素，Nd为钕元素，RE为La、Y、Gd、Pr中的一种或者几种，RE’为除去Ce、Nd、La、Y、Gd、Pr以外的其它镧系元素或者Sc中的一种或者几种，Fe为铁元素，M为Al、C、Co、Cr、Cu、F、Ga、Mn、Mo、N、Nb、Ni、P、Pb、S、Si、Ta、Ti、V、W、Zn、Zr元素中的一种或几种，B为硼元素；a、b、c、x、y、z分别满足以下关系：0.3≤a≤0.9，0≤b≤0.6，0.1≤c≤0.7，26≤x≤35，0.5≤y≤2.5，0.75≤z≤1.35；
其中辅合金中稀土氢化物以质量百分数计，成分为RE’’1-uHu，RE’’为镧系元素或者Sc或者Y中的一种或者几种，H为氢元素，0＜u≤0.05；辅合金中稀土金属多元合金以质量百分数计，成分为R1-vM’v，R为Nd、Pr、Dy、Tb、Ho、Gd、Ce、La、Y中的一种或者几种，M’为Fe、Ga、Cu、Co、Ni、Al元素中的一种或者几种，0.05≤v＜1。
2.根据权利要求1所述通过1:2相提高混合稀土永磁材料抗蚀性的多元晶界重构方法，其特征在于：主合金富Ce，为单一成分的主合金，或多种不同成分的主合金。
3.根据权利要求1所述通过1:2相提高混合稀土永磁材料抗蚀性的多元晶界重构方法，其特征在于：步骤4）中的真空烧结温度为900~1100℃，烧结时间为2~5h；热处理温度为400~900℃，热处理时间为0~12h。
4.根据权利要求3所述通过1:2相提高混合稀土永磁材料抗蚀性的多元晶界重构方法，其特征在于：步骤4）中的热处理为一级热处理，或多级循环热处理。
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