CN113921263A - 一种含镧和钇的烧结钕铁硼永磁材料的制备方法 - Google Patents

一种含镧和钇的烧结钕铁硼永磁材料的制备方法 Download PDF

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CN113921263A
CN113921263A CN202111323837.6A CN202111323837A CN113921263A CN 113921263 A CN113921263 A CN 113921263A CN 202111323837 A CN202111323837 A CN 202111323837A CN 113921263 A CN113921263 A CN 113921263A
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alloy powder
permanent magnet
magnet material
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yttrium
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丰光耀
岳武卫
冯虎
陆先海
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Ganzhou Great Magnet Technology Co ltd
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Abstract

本发明公开了一种含镧和钇的烧结钕铁硼永磁材料的制备方法。该方法旨在解决镧、铈等高丰度元素得不到有效利用。该方法的具体步骤为：将PrNd、La、Y、B、Al、Cu、Ga、Co、Nb、Zr和Fe原料混合均匀后，通过速凝薄片方法制成速凝片，然后通过氢破碎处理成第一合金粉，在经气流磨磨成第二合金粉，在第二合金粉加入防氧化剂后，在磁场压机中压制成型，然后依次经过冷等静压处理、真空烧结处理和两级回火处理，得到添加了镧、钇的烧结钕铁硼永磁材料。该方法通过添加镧、钇来部分替代镨、钕、镝、鋱制备的钕铁硼永磁材料，剩磁Br可达到13.5KGs，内禀矫顽力Hcj可达到1353KA/M，最大磁能积(BH)max350KJ/M3，而且其温度系数、抗腐蚀性等指标并未降低。

Description

一种含镧和钇的烧结钕铁硼永磁材料的制备方法
技术领域
本发明涉及钕铁硼永磁材料制备领域，更为具体地说，涉及一种含镧和钇的烧结钕铁硼永磁材料的制备方法。
背景技术
钕铁硼永磁材料由于其极高的磁能积、矫顽力和能量密度，被誉为“磁王”，其广泛应用于计算机的硬件驱动设备、各种家用电器、电声设备、多媒体设备、电子仪器、仪表、医疗设备、工业电动机、风力发电机、以及汽车传感器、电动汽车和混合动力汽车的驱动电机等等领域。
随着钕铁硼永磁材料应用市场的高速增长，导致稀土材料的生产规模和能力也得到了迅速提升。因为钕铁硼永磁材料中使用的主要是镨、钕、釓、镝、鋱，随之而来的是稀土元素的应用极不平衡，镧、铈等高丰度元素得不到有效利用，严重影响了稀土产业的健康发展。通过研究，利用低成本、相对过剩的镧、钇部分代替传统工艺中的镨、钕、镝、鋱等稀土元素制备中高档钕铁硼永磁材料是可行的。
发明内容
(1)要解决的技术问题
针对现有技术中的不足，本发明提供了一种含镧和钇的烧结钕铁硼永磁材料的制备方法。该方法旨在解决钕铁硼永磁材料中使用的主要是镨、钕、釓、镝、鋱，随之而来的是稀土元素的应用极不平衡，镧、铈等高丰度元素得不到有效利用，严重影响了稀土产业的健康发展。通过研究，利用低成本、相对过剩的镧、钇部分代替传统工艺中的镨、钕、镝、鋱等稀土元素制备中高档钕铁硼永磁材料是可行的问题，该方法通过添加镧、钇来部分替代镨、钕、镝、鋱制备的钕铁硼永磁材料，剩磁Br可达到13.5KGs，内禀矫顽力Hcj可达到1353KA/M，最大磁能积(BH)max350KJ/M3，产品磁性能达到中高档钕铁硼永磁材料技术指标。而且其温度系数、抗腐蚀性等指标并未降低；可节省10％-20％的镨、钕、镝、鋱用量，降低原材料成本5％-10％，并且使各种稀土资源得到平衡利用。
(2)技术方案
为了克服上述技术问题，本发明提供了这样一种含镧和钇的烧结钕铁硼永磁材料的制备方法，其特征在于，其具备以下工作步骤：
S1，将原料PrNd、La、Y、B、Al、Cu、Ga、Co、Nb、Zr和Fe按特定配比混合均匀，得到混合原料，所述特定配比为28％-29％：1％-1.5％：1％-2％：0.95％-1％：0.5％-1％：0.1％-0.2％：0.1％-0.2％：0.5％-1％：0.2％-0.4％：0.1％-0.3％：63.4％-67.55％；将所述混合原料通过速凝薄片法制备成厚度为0.15mm-0.58mm的速凝片；
S2，将所述速凝片进行氢破碎处理，得到颗粒直径0.5mm-1.5mm的第一合金粉，所述第一合金粉具备高脆性；
S3，将所述具备高脆性的第一合金粉置于N2的气氛中经气流磨进行磨粉，利用超音速N2气流的吹动，让粉末颗粒之间相互碰撞破碎，在经过高速旋转的分级轮进行筛选，获得平均粒度在2μm-10μm的第二合金粉，然后向第二合金粉中加入防氧化剂，所述第二合金粉粒度分布窄、颗粒形状规则，且具备高磁能积；
S4，将所述第二合金粉在磁场强度为2-3T的磁场压机中进行压制，随后依次进行冷等静压处理、真空烧结处理和两级回火处理，其中，控制一级回火的温度为700-940℃，控制二级回火的温度为430-650℃，控制所述一级回火的温度渐变式上升，同时控制所述二级回火的温度渐变式下降，最终得到添加了镧、钇的烧结钕铁硼永磁材料。
进一步地，所述第一合金粉的颗粒直径为1mm。
进一步地，所述氢破碎处理过程中，吸氢压力为0.1MPa-0.3MPa，吸氢时间4h-6h，脱氢温度为545℃-660℃，脱氢时间为4.5h-6.5h。
进一步地，所述氢破碎处理过程中，吸氢压力为0.2MPa，吸氢时间5h，脱氢温度为570℃，脱氢时间为5h。
进一步地，所述第二合金粉的平均粒度SMD为2.9μm。
进一步地，所述冷等静压处理中等静压的压强为200Mpa-220Mpa。
进一步地，所述真空烧结的温度为1040℃-1070℃、真空度为10-3Pa，真空烧结的保温时间为5.3-5.8h。
进一步地，特定配比为28.5％：1.2％：1.5％：0.98％：0.8％：0.15％、：0.15％：0.7％：0.3％：0.2％：65.52％。
进一步地，所述防氧化剂占第二合金粉与防氧化剂总质量的0.16％，两者通过三维混料机混合均匀。
进一步地，所述真空烧结的温度为1000℃-1200℃，真空烧结前半段时间，控制温度呈正态分布曲线先上升后下降，真空烧结后半段时间，控制温度持续保持1150℃，随后控制温度持续保持1000℃，用以提高烧结钕铁硼永磁材料的温度系数。
所述氢破碎处理步骤，在吸氢压力为0.2MPa，吸氢时间为5h，脱氢温度为560℃-580℃，脱氢时间为5h条件下时，其可以大大提高钕铁硼磁体的磁性能，同时可使所述速凝片的具有更高的脆性，利于气流磨过程中获取粒度分布较窄的磁粉，并且颗粒形状比较规则，进而获得较高磁能积；
所述气流磨处理步骤，是将具有高脆性的第一合金粉置于N2的气氛中，在超音速气流的吹动下，让粉末颗粒之间相互碰撞破碎，再经过高速旋转的分级轮进行筛选；
所述真空烧结处理步骤，可获得致密化程度接近理论密度的磁体，同时采用两级回火工艺，使晶界变得平滑规整，增加了反磁化畴形核的难度，减少主相晶粒的退磁场。
(3)有益效果
本工艺率先在国内工业规模化生产中添加镧、钇来部分替代镨、钕、镝、鋱制备的钕铁硼永磁材料，剩磁Br可达到13.5KGs，内禀矫顽力Hcj可达到1353KA/M，最大磁能积(BH)max350KJ/M3，产品磁性能达到中高档钕铁硼永磁材料技术指标。而且其温度系数、抗腐蚀性等指标并未降低。
本工艺可节省10％-20％的镨、钕、镝、鋱用量，降低原材料成本5％-10％，并且使各种稀土资源得到平衡利用。
具体实施方式
为使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解，下面对本发明具体实施方式中的技术方案进行清楚、完整的描述，以进一步阐述本发明，显然，所描述的具体实施方式仅仅是本发明的一部分实施方式，而不是全部的样式。
实施例1
首先将原料PrNd、La、Y、B、Al、Cu、Ga、Co、Nb、Zr和Fe按配比28％：1％：1％：0.95％：0.5％：0.1％：0.1％：0.5％：0.2％：0.1％：67.55％混合均匀，然后将其通过速凝薄片法制备成厚度为0.15mm的速凝片，之后让速凝片进行氢破碎处理，得到颗粒直径0.5mm且具备高脆性的第一合金粉，之后将其在N2的气氛中经气流磨进行磨粉，获得平均粒度在2μm第二合金粉，然后向第二合金粉中加入防氧化剂，并将其混合物放入磁场强度为2T的磁场压机中进行压制，随后依次进行冷等静压处理、真空烧结处理和两级回火处理，最终得到添加了镧、钇的烧结钕铁硼永磁材料。
实施例2
首先将原料PrNd、La、Y、B、Al、Cu、Ga、Co、Nb、Zr和Fe按配比28.5％：1.2％：1.5％：0.98％：0.8％：0.15％：0.15％：0.7％：0.3％：0.2％：65.52％混合均匀，然后将其通过速凝薄片法制备成厚度为0.3mm的速凝片，之后让速凝片进行氢破碎处理，得到颗粒直径1mm且具备高脆性的第一合金粉，之后将其在N2的气氛中经气流磨进行磨粉，获得平均粒度在3μm第二合金粉，然后向第二合金粉中加入防氧化剂，并将其混合物放入磁场强度为2.5T的磁场压机中进行压制，随后依次进行冷等静压处理、真空烧结处理和两级回火处理，最终得到添加了镧、钇的烧结钕铁硼永磁材料。
实施例3
首先将原料PrNd、La、Y、B、Al、Cu、Ga、Co、Nb、Zr和Fe按配比29％：1.5％：2％：1％：1％：0.2％：0.2％：1％：0.4％：0.3％：63.4％混合均匀，然后将其通过速凝薄片法制备成厚度为0.58mm的速凝片，之后让速凝片进行氢破碎处理，得到颗粒直径1.5mm且具备高脆性的第一合金粉，之后将其在N2的气氛中经气流磨进行磨粉，获得平均粒度在5μm第二合金粉，然后向第二合金粉中加入防氧化剂，并将其混合物放入磁场强度为3T的磁场压机中进行压制，随后依次进行冷等静压处理、真空烧结处理和两级回火处理，最终得到添加了镧、钇的烧结钕铁硼永磁材料。
通过将实施例1-3中得到的磁体进行性能测试，其性能如下：
剩磁Br:13.33-13.52KGs，内禀矫顽力HcJ:1350-1400KA/M，最大磁能积(BH)max:340-360KJ/M3，产品磁性能达到中高档钕铁硼永磁材料技术指标，而且其温度系数、抗腐蚀性等指标并未降低。并且，通过本发明的工艺可节省10％-20％的镨、钕、镝、鋱用量，降低原材料成本5％-10％，使各种稀土资源得到平衡利用。
以上描述了本发明的主要技术特征和基本原理及相关优点，对于本领域技术人员而言，显然本发明不限于上述示范性具体实施方式的细节，而且在不背离本发明的构思或基本特征的情况下，能够以其他的具体形式实现本发明。因此，无论从哪一点来看，均应将上述具体实施方式看作是示范性的，而且是非限制性的，本发明的范围由所附权利要求而不是上述说明限定，因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。
此外，应当理解，虽然本说明书按照各实施方式加以描述，但并非每个实施方式仅包含一个独立的技术方案，说明书的这种叙述方式仅仅是为清楚起见，本领域技术人员应当将说明书作为一个整体，各实施方式中的技术方案也可以经适当组合，形成本领域技术人员可以理解的其他实施方式。

Claims (10)

1.一种含镧和钇的烧结钕铁硼永磁材料的制备方法，其特征在于，其具备以下工作步骤：
S1，将原料PrNd、La、Y、B、Al、Cu、Ga、Co、Nb、Zr和Fe按特定配比混合均匀，得到混合原料，所述特定配比为28％-29％：1％-1.5％：1％-2％：0.95％-1％：0.5％-1％：0.1％-0.2％：0.1％-0.2％：0.5％-1％：0.2％-0.4％：0.1％-0.3％：63.4％-67.55％；将所述混合原料通过速凝薄片法制备成厚度为0.15mm-0.58mm的速凝片；
S2，将所述速凝片进行氢破碎处理，得到颗粒直径0.5mm-1.5mm的第一合金粉，所述第一合金粉具备高脆性；
S3，将所述具备高脆性的第一合金粉置于N2的气氛中经气流磨进行磨粉，利用超音速N2气流的吹动，让粉末颗粒之间相互碰撞破碎，在经过高速旋转的分级轮进行筛选，获得平均粒度在2μm-10μm的第二合金粉，然后向第二合金粉中加入防氧化剂，所述第二合金粉粒度分布窄、颗粒形状规则，且具备高磁能积；
S4，将所述第二合金粉在磁场强度为2-3T的磁场压机中进行压制，随后依次进行冷等静压处理、真空烧结处理和两级回火处理，其中，控制一级回火的温度为700-940℃，控制二级回火的温度为430-650℃，控制所述一级回火的温度渐变式上升，同时控制所述二级回火的温度渐变式下降，最终得到添加了镧、钇的烧结钕铁硼永磁材料。
2.根据权利要求1所述的一种含镧和钇的烧结钕铁硼永磁材料的制备方法，其特征在于，所述第一合金粉的颗粒直径为1mm。
3.根据权利要求1所述的一种含镧和钇的烧结钕铁硼永磁材料的制备方法，其特征在于，所述氢破碎处理过程中，吸氢压力为0.1MPa-0.3MPa，吸氢时间4h-6h，脱氢温度为545℃-660℃，脱氢时间为4.5h-6.5h。
4.根据权利要求1所述的一种含镧和钇的烧结钕铁硼永磁材料的制备方法，其特征在于，所述氢破碎处理过程中，吸氢压力为0.2MPa，吸氢时间5h，脱氢温度为570℃，脱氢时间为5h。
5.根据权利要求1所述的一种含镧和钇的烧结钕铁硼永磁材料的制备方法，其特征在于，所述第二合金粉的平均粒度SMD为2.9μm。
6.根据权利要求1所述的一种含镧和钇的烧结钕铁硼永磁材料的制备方法，其特征在于，所述冷等静压处理中等静压的压强为210Mpa。
7.根据权利要求1所述的一种含镧和钇的烧结钕铁硼永磁材料的制备方法，其特征在于，所述真空烧结的温度为1040℃-1070℃、真空度为10-3Pa，真空烧结的保温时间为5.3-5.8h。
8.根据权利要求1所述的一种含镧和钇的烧结钕铁硼永磁材料的制备方法，其特征在于，特定配比为28.5％：1.2％：1.5％：0.98％：0.8％：0.15％、：0.15％：0.7％：0.3％：0.2％：65.52％。
9.根据权利要求1所述的一种含镧和钇的烧结钕铁硼永磁材料的制备方法，其特征在于，所述防氧化剂占第二合金粉与防氧化剂总质量的0.16％，两者通过三维混料机混合均匀。
10.根据权利要求1所述的一种含镧和钇的烧结钕铁硼永磁材料的制备方法，其特征在于，所述真空烧结的温度为1000℃-1200℃，真空烧结前半段时间，控制温度呈正态分布曲线先上升后下降，真空烧结后半段时间，控制温度持续保持1150℃，随后控制温度持续保持1000℃，用以提高烧结钕铁硼永磁材料的温度系数。
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