CN104464996B - 一种烧结钕铁硼永磁材料及其制备方法 - Google Patents

一种烧结钕铁硼永磁材料及其制备方法 Download PDF

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CN104464996B
CN104464996B CN201410757138.6A CN201410757138A CN104464996B CN 104464996 B CN104464996 B CN 104464996B CN 201410757138 A CN201410757138 A CN 201410757138A CN 104464996 B CN104464996 B CN 104464996B
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王栩
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Jiangmen Xinlike Magnetoelectric Co ltd
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Abstract

制备该烧结钕铁硼永磁材料的方法，包括以下步骤：将步骤（1）步骤（2）中的甩片，按质量1:4比例混合，并在581℃脱氢9h制成氢爆粉；然后经过气流磨后制成平均粒度均为3.5～4μm的磁粉；（4）将步骤（3）中的磁粉、粒径30nm纳米氧化钇、粒径50nm纳米钨粉、粒径50nm纳米碳化锆粉末按质量比为1000:5:2:3加入到三维混合机中混合均匀，得混合粉料；（5）将步骤（4）中的混合粉料在磁场压机中取向，应用垂直钢磨压、加冷等静压方式成型，放入高真空烧结炉内1151℃烧结3.5h,经一次回火952℃处理2.5 h,以及二级回火748℃处理3小时。

Description

一种烧结钕铁硼永磁材料及其制备方法
技术领域
本发明属于磁性功能材料领域，具体涉及一种烧结钕铁硼永磁材料及其制备方法。
背景技术
钕铁硼，简单来讲是一种磁铁，和我们平时见到的磁铁所不同的是，其优异的磁性能而被称为“磁王”。钕铁硼中含有大量的稀土元素钕、铁及硼，其特性硬而脆。由于表面极易被氧化腐蚀，钕铁硼必须进行表面涂层处理。表面化学钝化是很好的解决方法之一。钕铁硼作为稀土永磁材料的一种具有极高的磁能积和矫顽力，同时高能量密度的优点使钕铁硼永磁材料在现代工业和电子技术中获得了广泛应用，从而使仪器仪表、电声电机、磁选磁化等设备的小型化、轻量化、薄型化成为可能。钕铁硼的优点是性价比高，具良好的机械特性；不足之处在于工作温度低，温度特性差，且易于粉化腐蚀，必须通过调整其化学成分和采取表面处理方法使之得以改进，才能达到实际应用的要求。
发明内容
本发明目的在于克服现有技术中的不足，提供一种烧结钕铁硼永磁材料，该烧结钕铁硼永磁材料，具有较高的磁体矫顽力，较高的磁体工作温度，尤其是提高了晶界的耐蚀性能，磁体的耐蚀性能得到提高。
本发明烧结钕铁硼永磁材料；由以下组分及质量百分比的原料制成：Nd 21～23%、B 0.8～0.9%、Cu 0.3～0.4%、Co 0.8～0.9%、Ga 0.3～0.4%、Nb 0.6～0.7%、Pr 3～4%、Al0.5～0.6%、余量为Fe。
作为优化，该烧结钕铁硼永磁材料，在所述的组份及质量百分比基础上，还加入有纳米氧化钇、纳米钨粉、纳米碳化锆按照质量比5:2:3的混合粉末，其占总质量百分比为0.9～ 1.1%。
制备该烧结钕铁硼永磁材料的方法，包括以下步骤：
（1）按照质量百分比Nd 21.2%、B 0.83%、Cu 0.35%、Co 0.82%、Nb 0.95%、Pr 3.1%、Al 0.32%、余量为Fe配比原料，将该原料放入真空速凝甩带炉中，甩片厚度控制在0.2～0.3mm；
（2）按照质量百分比Nd 23%、B 0.91%、Cu 0.41%、Co 0.89%、Ga 0.45%、Nb 0.55%、Pr 3.9%、Al 0.55%、余量为Fe配比原料，将该原料放入真空速凝甩带炉中，甩片厚度控制在0.1～0.2mm；
（3）将步骤（1）步骤（2）中的甩片，按质量1:4比例混合，然后加入氢破炉，并在575～595℃脱氢9 h 制成氢爆粉；然后经过气流磨后制成平均粒度均为3.5～4μm 的磁粉；
（4）将步骤（3）中的磁粉、纳米氧化钇、纳米钨粉、纳米碳化锆按质量比为1000:5:2:3加入到三维混合机中混合均匀，得混合粉料；
（5）将步骤（4）中的混合粉料在磁场压机中取向，应用垂直钢磨压加冷等静压方式成型，放入高真空烧结炉内1120～1170℃烧结3.5h ,经一次回火930～980℃处理2.5 h ,以及二级回火725～775℃处理3小时。
作为优化，制备该烧结钕铁硼永磁材料的方法，包括以下步骤：
（1）按照质量百分比Nd 21.2%、B 0.83%、Cu 0.35%、Co 0.82%、Nb 0.95%、Pr 3.1%、Al 0.32%、余量为Fe配比原料，将该原料放入真空速凝甩带炉中，甩片厚度控制在0.2～0.3mm；
（2）按照质量百分比Nd 23%、B 0.91%、Cu 0.41%、Co 0.89%、Ga 0.45%、Nb 0.55%、Pr 3.9%、Al 0.55%、余量为Fe配比原料，将该原料放入真空速凝甩带炉中，甩片厚度控制在0.1～0.2mm；
（3）将步骤（1）步骤（2）中的甩片，按质量1:4比例混合，然后加入氢破炉，并在581℃脱氢9 h 制成氢爆粉；然后经过气流磨后制成平均粒度均为3.5～4μm 的磁粉；
（4）将步骤（3）中的磁粉、粒径30nm纳米氧化钇、粒径50nm纳米钨粉、粒径50nm纳米碳化锆粉末按质量比为1000:5:2:3加入到三维混合机中混合均匀，得混合粉料；
（5）将步骤（4）中的混合粉料在磁场压机中取向，应用垂直钢磨压、加冷等静压方式成型，放入高真空烧结炉内1151℃烧结3.5h ,经一次回火952℃处理2.5 h ,以及二级回火748℃处理3小时。
该烧结钕铁硼永磁材料，由两种不同组分的合金粉末，添加粒径30nm纳米氧化钇、粒径50nm纳米钨粉、粒径50nm纳米碳化锆粉末，混合均匀后，通过特殊工艺烧结而成，提高了烧结钕铁硼的工作温度和耐蚀性，使混有粒径30nm纳米氧化钇、粒径50nm纳米钨粉、粒径50nm纳米碳化锆粉末的非磁性晶界相均匀分散于主相晶粒表面层，阻碍了硬磁性相之间的交换耦合作用，改善了微观结构，提高了磁体的矫顽力，提高了磁体的工作温度，而且添加纳米粉末后，其腐蚀电位与主相相差减小，从而提高了晶界的耐蚀性能，磁体的耐蚀性能得到提高。恒温恒压试验箱，96小时 ，（130±2℃（0.27MPa） 失重率＜2mg/cm2。
具体实施方式
下面给出的实施例拟对本发明作进一步说明，但不能理解为是对本发明保护范围的限制，本领域技术人员根据本发明内容对本发明的一些非本质的改进和调整，仍属于本发明的保护范围。
实施例1：（1）按照质量百分比Nd 21.2%、B 0.83%、Cu 0.35%、Co 0.82%、Nb 0.95%、Pr 3.1%、Al 0.32%、余量为Fe配比原料，将该原料放入真空速凝甩带炉中，甩片厚度控制在0.2～0.3mm；
（2）按照质量百分比Nd 23%、B 0.91%、Cu 0.41%、Co 0.89%、Ga 0.45%、Nb 0.55%、Pr 3.9%、Al 0.55%、余量为Fe配比原料，将该原料放入真空速凝甩带炉中，甩片厚度控制在0.1～0.2mm；
（3）将步骤（1）步骤（2）中的甩片，按质量1:4比例混合，然后加入氢破炉，并在581℃脱氢9 h 制成氢爆粉；然后经过气流磨后制成平均粒度均为3.5～4μm 的磁粉；
（4）取步骤（3）中的磁粉500公斤、粒径30nm纳米氧化钇2.5公斤、粒径50nm纳米钨粉1公斤、粒径50nm纳米碳化锆粉末1.5公斤，加入到SYH系列三维运动混合机中混合均匀，得混合粉料；
（5）将步骤（4）中的混合粉料在磁场压机中取向，应用垂直钢磨压、加冷等静压方式成型，放入高真空烧结炉内1151℃烧结3.5h ,经一次回火952℃处理2.5 h ,以及二级回火748℃处理3小时；
该烧结钕铁硼永磁材料性能如下：剩磁(Br) 1.39T ；磁感应矫顽力(bHc) 985kA/m ；内禀矫顽力(jHc) 1665 kA/m；最大磁能积(BH)max 382kJ/m3；居里温度(Tc) 369℃；恒温恒压试验箱，96小时 ，（130±2℃（0.27MPa） 失重率1.8mg/cm2。
实施例2：（1）按照质量百分比Nd 20.1%、B 0.85%、Cu 0.32%、Co 0.80%、Nb 0.95%、Pr 3.0%、Al 0.32%、余量为Fe配比原料，将该原料放入真空速凝甩带炉中，甩片厚度控制在0.2～0.3mm；
（2）按照质量百分比Nd 23%、B 0.91%、Cu 0.42%、Co 0.90%、Ga 0.45%、Nb 0.55%、Pr 3.9%、Al 0.55%、余量为Fe配比原料，将该原料放入真空速凝甩带炉中，甩片厚度控制在0.1～0.2mm；
（3）将步骤（1）步骤（2）中的甩片，按质量1:4比例混合，然后加入氢破炉，并在575℃脱氢9 h 制成氢爆粉；然后经过气流磨后制成平均粒度均为3.5～4μm 的磁粉；
（4）取步骤（3）中的磁粉500公斤、粒径30nm纳米氧化钇2.5公斤、粒径50nm纳米钨粉1公斤、粒径50nm纳米碳化锆粉末1.5公斤，加入到三维混合机中混合均匀，得混合粉料；
（5）将步骤（4）中的混合粉料在磁场压机中取向，应用垂直钢磨压、加冷等静压方式成型，放入高真空烧结炉内1120℃烧结3.5h ,经一次回火930℃处理2.5 h ,以及二级回火725℃处理3小时；
该烧结钕铁硼永磁材料性能如下：剩磁(Br) 1.38T ；磁感应矫顽力(bHc) 981kA/m ；内禀矫顽力(jHc) 1647 kA/m；最大磁能积(BH)max 378kJ/m3；居里温度(Tc) 368℃；恒温恒压试验箱，96小时 ，（130±2℃（0.27MPa） 失重率1.8mg/cm2。
实施例3：（1）按照质量百分比Nd 19.1%、B 0.83%、Cu 0.35%、Co 0.82%、Nb 0.95%、Pr 2.8%、Al 0.32%、余量为Fe配比原料，将该原料放入真空速凝甩带炉中，甩片厚度控制在0.2～0.3mm；
（2）按照质量百分比Nd 23.2%、B 0.91%、Cu 0.41%、Co 0.89%、Ga 0.45%、Nb0.55%、Pr 4.0%、Al 0.55%、余量为Fe配比原料，将该原料放入真空速凝甩带炉中，甩片厚度控制在0.1～0.2mm；
（3）将步骤（1）步骤（2）中的甩片，按质量1:4比例混合，然后加入氢破炉，并在595℃脱氢9 h 制成氢爆粉；然后经过气流磨后制成平均粒度均为3.5～4μm 的磁粉；
（4）取步骤（3）中的磁粉500公斤、粒径30nm纳米氧化钇2.5公斤、粒径50nm纳米钨粉1公斤、粒径50nm纳米碳化锆粉末1.5公斤，加入到三维混合机中混合均匀，得混合粉料；
（5）将步骤（4）中的混合粉料在磁场压机中取向，应用垂直钢磨压、加冷等静压方式成型，放入高真空烧结炉内1170℃烧结3.5h ,经一次回火980℃处理2.5 h ,以及二级回火775℃处理3小时；
该烧结钕铁硼永磁材料性能如下：剩磁(Br) 1.37T ；磁感应矫顽力(bHc) 989kA/m ；内禀矫顽力(jHc) 1651 kA/m；最大磁能积(BH)max 379kJ/m3；居里温度(Tc) 367℃；恒温恒压试验箱，96小时 ，（130±2℃（0.27MPa） 失重率1.9mg/cm2。

Claims (2)

1.一种烧结钕铁硼永磁材料，其特征在于由以下组分通过以下步骤制成：
（1）按照质量百分比Nd 21.2%、B 0.83%、Cu 0.35%、Co 0.82%、Nb 0.95%、Pr 3.1%、Al0.32%、余量为Fe配比原料，将该原料放入真空速凝甩带炉中，甩片厚度控制在0.2～0.3mm；
（2）按照质量百分比Nd 23%、B 0.91%、Cu 0.41%、Co 0.89%、Ga 0.45%、Nb 0.55%、Pr3.9%、Al 0.55%、余量为Fe配比原料，将该原料放入真空速凝甩带炉中，甩片厚度控制在0.1～0.2mm；
（3）将步骤（1）步骤（2）中的甩片，按质量1:4比例混合，然后加入氢破炉，并在575～595℃脱氢9 h 制成氢爆粉；然后经过气流磨后制成平均粒度均为3.5～4μm 的磁粉；
（4）将步骤（3）中的磁粉、纳米氧化钇、纳米钨粉、纳米碳化锆按质量比为1000:5:2:3加入到三维混合机中混合均匀，得混合粉料；
（5）将步骤（4）中的混合粉料在磁场压机中取向，应用垂直钢磨压加冷等静压方式成型，放入高真空烧结炉内1120～1170℃烧结3.5h，经一次回火930～980℃处理2.5 h，以及二级回火725～775℃处理3小时。
2.根据权利要求1所述的烧结钕铁硼永磁材料，其特征在于通过以下步骤制成：
（1）按照质量百分比Nd 21.2%、B 0.83%、Cu 0.35%、Co 0.82%、Nb 0.95%、Pr 3.1%、Al0.32%、余量为Fe配比原料，将该原料放入真空速凝甩带炉中，甩片厚度控制在0.2～0.3mm；
（2）按照质量百分比Nd 23%、B 0.91%、Cu 0.41%、Co 0.89%、Ga 0.45%、Nb 0.55%、Pr3.9%、Al 0.55%、余量为Fe配比原料，将该原料放入真空速凝甩带炉中，甩片厚度控制在0.1～0.2mm；
（3）将步骤（1）步骤（2）中的甩片，按质量1:4比例混合，然后加入氢破炉，并在581℃脱氢9 h 制成氢爆粉；然后经过气流磨后制成平均粒度均为3.5～4μm 的磁粉；
（4）将步骤（3）中的磁粉、粒径30nm纳米氧化钇、粒径50nm纳米钨粉、粒径50nm纳米碳化锆粉末按质量比为1000:5:2:3加入到三维混合机中混合均匀，得混合粉料；
（5）将步骤（4）中的混合粉料在磁场压机中取向，应用垂直钢磨压、加冷等静压方式成型，放入高真空烧结炉内1151℃烧结3.5h ,经一次回火952℃处理2.5 h，以及二级回火748℃处理3小时。
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