CN113223803A - 一种低成本n35烧结钕铁硼永磁体及其制备方法 - Google Patents
一种低成本n35烧结钕铁硼永磁体及其制备方法 Download PDFInfo
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- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
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- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
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- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
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- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
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- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
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- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
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- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
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Abstract
本申请涉及磁性材料领域，具体公开了一种低成本N35烧结钕铁硼永磁体及其制备方法。低成本N35烧结钕铁硼永磁体，按质量份数计，原料包括如下组分：镨钕87‑117份，铈88‑105份，硼28‑34份，铜0.8‑1份，铝1.5‑2.5份，锆1‑3份，铁376‑383份；其制备方法为：按比例称取各原料，再依次进行真空熔炼、粉碎、压制成型和烧结，冷却后得到烧结钕铁硼永磁体。本申请的低成本N35烧结钕铁硼永磁体可用于光盘驱动器、机器人和高档音响，其具有成本低的优点。
Description
技术领域
本申请涉及磁性材料领域，更具体地说，它涉及一种低成本N35烧结钕铁硼永磁体及其制备方法。
背景技术
近年来，随着钕铁硼磁体应用领域的迅速扩张，对原材料的需求已经变得越来越大。牌号为N35的钕铁硼磁体是目前光盘驱动器、机器人、高档音响市场需求量较大的磁体材料，生产成本较高，且生产过程中的能源消耗大。
这是由于生产过程中使用价格昂贵的重稀土钆、铽、镝等元素提高磁性，从而导致生产成本居高不下。很多厂家通过采用铈替代价格昂贵的重稀土钆、铽、镝等元素以降低生产成本，但铈的添加量无法超过5wt%，因为添加量过大会导致磁性能恶化且达不到成本的明显效果。
针对上述中的相关技术，需要寻求一种铈的添加量超过5wt%以降低生产成本且烧结钕铁硼磁体的磁性能基本不发生变化的方法。
发明内容
为了在降低生产成本的同时使烧结钕铁硼磁体的磁性能基本不发生变化，本申请提供一种低成本N35烧结钕铁硼永磁体及其制备方法。
第一方面，本申请提供一种低成本N35烧结钕铁硼永磁体，采用如下的技术方案：
一种低成本N35烧结钕铁硼永磁体，按质量份数计，原料包括如下组分：镨钕87-117份，铈88-105份，硼28-34份，铜0.8-1份，铝1.5-2.5份，锆1-3份，铁376-383份。
通过采用上述技术方案，本申请通过铈替代镨钕的方式降低生产成本，且原料中铈含量远大于6wt%，同时硼含量偏高，但却能够保证烧结钕铁硼永磁体的性能基本不变。
同时，原料中硼的含量较高，高硼含量能够提高烧结钕铁硼永磁体的矫顽力，从而提高烧结钕铁硼永磁体的磁性能。原料中的铝元素也能够提高烧结钕铁硼永磁体的矫顽力，同时改善烧结钕铁硼永磁体的主体界面，从而提高烧结钕铁硼永磁体的耐温性能。原料中的铜元素能够改善烧结钕铁硼永磁体的微观结构，提高烧结钕铁硼永磁体的内禀矫顽力。
优选的，还包括2-4份钆铁。
通过采用上述技术方案，采用部分钆取代镨钕的方式生产钕铁硼永磁体，能够进一步降低生产成本。添加一定数量的钆元素之后，钕铁硼合金铸片中α-Fe相得以消除或减少，主相晶粒具有明显的柱状晶特征，改善了铸片的破碎性能，使粉末粒度分布比较均匀，减少粉末中极细与极大粉末颗粒的数量。
这样，一方面可增强粉末的抗氧化能力；另一方面减小了粉末颗粒之间的磁团聚效应，使粉末的磁场取向过程顺利进行，提高烧结磁体的取向度。
优选的，所述镨钕与所述铈的质量比为（0.9-1.2）：1。
通过采用上述技术方案，控制镨钕与铈的质量比在该范围内时，制得的钕铁硼永磁体在降低生产成本的同时能够保持磁性能基本不变。
若镨钕与铈的质量比小于0.9:1，则镨钕的含量过低，导致铈的含量偏高，生产成本虽然降低，但是磁性能随之大幅度下降。
优选的，所述硼与所述镨钕的质量比为（0.27-0.33）：1。
通过采用上述技术方案，控制硼与镨钕的质量比在该范围时，有利于获得高矫顽力，制得的钕铁硼永磁体具有良好的磁性能。
若硼含量偏高，制得的钕铁硼永磁体剩磁大大下降，但是矫顽力高。若硼含量偏低，制得的钕铁硼永磁体矫顽力偏低。
第二方面，本申请提供一种低成本N35烧结钕铁硼永磁体的制备方法，采用如下的技术方案：
一种低成本N35烧结钕铁硼永磁体的制备方法，包括如下制备步骤：
S1、按比例称取各原料；
S2、将各原料进行真空熔炼，得到铸片；
S3、将铸片进行氢破碎，得到合金粉末；
S4、将合金粉末在1350-1400kA/m的磁场中取向，然后压制成型，得到坯体；
S5、将坯体在1050-1100℃下烧结3-5h，然后在800-850℃下保温2-3h进行一级回火，于510-560℃下保温2-3h进行二级回火，冷却后得到钕铁硼永磁体。
通过采用上述技术方案，经过上述步骤制得的钕铁硼永磁体能够获得优异的综合磁性能，在降低生产成本的同时能够保持磁性能基本不变。
其中，氢破碎是利用稀土金属间化合物的吸氢特性，将钕铁硼合金置于氢气环境下，氢气沿富钕相薄层进入合金，使之膨胀爆裂而破碎，沿富钕相层处开裂，从而使铸片变为合金粉末。
合金粉末压制成型后，颗粒之间的接触并不紧密，结合强度较低，通过烧结时能够提高坯体的密度，提高钕铁硼永磁体的强度，改善钕铁硼永磁体的显微结构。
优选的，S2中，各原料在进行真空熔炼之前，先进行去污除杂。
通过采用上述技术方案，原料表面的油污和杂质先除去，减少原料中杂质的含量，有利于提高原料的纯度。
优选的，S3中，合金粉末的粒径为3-5μm。
通过采用上述技术方案，3-5μm的粒径为宜，粒径变小相应矫顽力和剩磁会提高，钕铁硼永磁体的耐腐蚀性也会提高，但是后续的工艺不好控制，这是由于粒径过小会导致合金粉末的比表面积过大，容易发生氧化。
优选的，S4中，压制成型采用垂直钢模压和冷等静压的方式成型。
通过采用上述技术方案，采用上述方式制得的坯体密度高，密度均匀一致，且上述方式不需要在粉料中添加润滑剂，能够减少污染，简化了制备工序，同时等静压成型的坯体，性能优异，且烧结温度低于其他成型方法制得的坯体，从而降低了生产成本。
而单向或双向压制的模压成型，由于粉料与钢模之间的摩擦阻力的存在及成型压力在传递过程中的递减，会出现坯体密度分布不均匀的现象。
优选的，S5中，钕铁硼永磁体烧结完毕后，对其进行镀层处理。
通过采用上述技术方案，经过镀层处理后的钕铁硼永磁体能够提高耐腐蚀性能，从而延长使用寿命。
综上所述，本申请具有以下有益效果：
1、由于本申请采用铈替代镨钕的方式降低生产成本，同时保证烧结钕铁硼永磁体的性能基本不变；
2、本申请中优选采用钆与铈共同替代镨钕的方式，进一步降低了生产成本；
3、本申请的方法，经过熔炼、氢破、压制成型、烧结等步骤制得的钕铁硼永磁体能够获得优异的综合磁性能，在降低生产成本的同时能够保持磁性能基本不变。
具体实施方式
以下结合实施例对本申请作进一步详细说明。
实施例
一种低成本N35烧结钕铁硼永磁体的制备方法，包括如下制备步骤：
S1、按比例称取各原料，原料的组分和用量具体见表1所示；
S2、将除硼之外的各原料置于丙酮溶剂中进行超声磁选清洗，去除表面油污以及非磁性杂质，清洗干净后将各原料置于氩气氛保护下进行真空熔炼，得到铸片；
S3、将铸片进行氢破碎，得到粒径为3-5μm的合金粉末；
S4、将合金粉末在1350-1400kA/m的磁场中取向，然后采用垂直钢模压和冷等静压的方式将合金粉末压制成型，得到坯体；
S5、将坯体置于10-2-10-3Pa真空条件下，在1050-1100℃下烧结3-5h，然后在850-950℃下保温2-3h进行一级回火，于510-560℃下保温2-3h进行二级回火，冷却后得到钕铁硼永磁体；
S6、对钕铁硼永磁体进行镀锌处理。
实施例1
一种低成本N35烧结钕铁硼永磁体的制备方法，包括如下制备步骤：
S1、按比例称取各原料，原料的组分和用量具体见表1所示；
S2、将除硼之外的各原料置于丙酮溶剂中进行超声磁选清洗，去除表面油污以及非磁性杂质，清洗干净后将各原料置于氩气氛保护下进行真空熔炼，得到铸片；
S3、将铸片进行氢破碎，得到粒径为3-5μm的合金粉末；
S4、将合金粉末在1350kA/m的磁场中取向，然后采用垂直钢模压和冷等静压的方式将合金粉末压制成型，得到坯体；
S5、将坯体置于10-2Pa真空条件下，在1100℃下烧结4h，然后在900℃下保温3h进行一级回火，于530℃下保温3h进行二级回火，冷却后得到钕铁硼永磁体；
S6、对钕铁硼永磁体进行镀锌处理。
实施例2
一种低成本N35烧结钕铁硼永磁体的制备方法，包括如下制备步骤：
S1、按比例称取各原料，原料的组分和用量具体见表1所示；
S2、将除硼之外的各原料置于丙酮溶剂中进行超声磁选清洗，去除表面油污以及非磁性杂质，清洗干净后将各原料置于氩气氛保护下进行真空熔炼，得到铸片；
S3、将铸片进行氢破碎，得到粒径为3-5μm的合金粉末；
S4、将合金粉末在1350kA/m的磁场中取向，然后采用垂直钢模压和冷等静压的方式将合金粉末压制成型，得到坯体；
S5、将坯体置于10-2Pa真空条件下，在1050℃下烧结5h，然后在850℃下保温3h进行一级回火，于510℃下保温2h进行二级回火，冷却后得到钕铁硼永磁体；
S6、对钕铁硼永磁体进行镀锌处理。
实施例3
一种低成本N35烧结钕铁硼永磁体的制备方法，包括如下制备步骤：
S1、按比例称取各原料，原料的组分和用量具体见表1所示；
S2、将除硼之外的各原料置于丙酮溶剂中进行超声磁选清洗，去除表面油污以及非磁性杂质，清洗干净后将各原料置于氩气氛保护下进行真空熔炼，得到铸片；
S3、将铸片进行氢破碎，得到粒径为3-5μm的合金粉末；
S4、将合金粉末在1400kA/m的磁场中取向，然后采用垂直钢模压和冷等静压的方式将合金粉末压制成型，得到坯体；
S5、将坯体置于10-2Pa真空条件下，在1100℃下烧结3h，然后在950℃下保温2h进行一级回火，于560℃下保温2h进行二级回火，冷却后得到钕铁硼永磁体；
S6、对钕铁硼永磁体进行镀锌处理。
实施例4
一种低成本N35烧结钕铁硼永磁体的制备方法，包括如下制备步骤：
S1、按比例称取各原料，原料的组分和用量具体见表1所示；
S2、将除硼之外的各原料置于丙酮溶剂中进行超声磁选清洗，去除表面油污以及非磁性杂质，清洗干净后将各原料置于氩气氛保护下进行真空熔炼，得到铸片；
S3、将铸片进行氢破碎，得到粒径为3-5μm的合金粉末；
S4、将合金粉末在1350kA/m的磁场中取向，然后采用垂直钢模压和冷等静压的方式将合金粉末压制成型，得到坯体；
S5、将坯体置于10-2Pa真空条件下，在1100℃下烧结4h，然后在900℃下保温3h进行一级回火，于530℃下保温3h进行二级回火，冷却后得到钕铁硼永磁体；
S6、对钕铁硼永磁体进行镀锌处理。
上述实施例1-4中低成本N35烧结钕铁硼永磁体的原料组分和用量具体如表1所示，其中实施例4中不添加钆铁。
表1 实施例1-4中原料组分和用量
| 实施例1 | 实施例2 | 实施例3 | 实施例4 | |
| 镨钕 | 107 | 116.9 | 87 | 110 |
| 铈 | 96 | 88 | 105 | 96 |
| 钆铁 | 3 | 2 | 4 | - |
| 硼 | 32 | 28 | 34 | 32 |
| 铜 | 0.93 | 0.8 | 1 | 0.93 |
| 铝 | 2 | 1.5 | 2.5 | 2 |
| 锆 | 1.5 | 1 | 2 | 1.5 |
| 钴 | 1.5 | 1 | 2 | 1.5 |
| 铁 | 376.07 | 380.8 | 382.5 | 376.07 |
实施例5
本实施例中低成本N35烧结钕铁硼永磁体的制备方法与实施例1相同，区别仅在于镨钕与铈的质量比为0.8:1。
实施例6
本实施例中低成本N35烧结钕铁硼永磁体的制备方法与实施例1相同，区别仅在于硼与镨钕的质量比为0.17:1。
对比例
对比例1
本对比例中低成本N35烧结钕铁硼永磁体的制备方法与实施例1相同，区别仅在于镨钕与铈的质量比为0.7:1。
对比例2
本对比例中低成本N35烧结钕铁硼永磁体的制备方法与实施例1相同，区别仅在于S2中各原料直接进行熔炼，不进行去污除杂。
性能检测试验
剩磁Br：使用AMT-4磁化特性自动测量仪进行检测；
内禀矫顽力Hcj：使用AMT-4磁化特性自动测量仪进行检测。
表2 实施例1-6和对比例1-3的试验结果
| Br（kGs） | Hcj（kOe） | |
| 实施例1 | 11.8 | 12.31 |
| 实施例2 | 12.0 | 12.37 |
| 实施例3 | 11.2 | 12.07 |
| 实施例4 | 11.9 | 12.33 |
| 实施例5 | 11.4 | 11.84 |
| 实施例6 | 11.5 | 12.91 |
| 对比例1 | 10.9 | 11.21 |
| 对比例2 | 11.6 | 12.27 |
| N35 | 11.8-12.2 | 12 |
结合实施例1-3并结合表2可以看出，利用本申请的配方制得的低成本N35烧结钕铁硼永磁体具有良好的磁性能，且由于采用钆和铈替代部分镨钕的方式，降低了低成本N35烧结钕铁硼永磁体的生产成本，且其磁性能与N35相近，说明本申请的低成本N35烧结钕铁硼永磁体在降低成本的同时保持了磁性能基本不变。
其中实施例1为优选方案，铈占比高，镨钕的占比相对实施2和实施例3而言较低，且实施例1的磁性能符合N35磁性能。实施例2中虽然性能稍由于实施例1，但是其添加的铈含量比实施例1少，生产成本降低的没有实施例1多，综合考量，优选实施例1。
结合实施例1和实施例4并结合表2可以看出，实施例4中不添加钆铁，对应的镨钕的添加量有所增加，实施例4中低成本N35烧结钕铁硼永磁体的磁性能略高于实施例1中低成本N35烧结钕铁硼永磁体的磁性能，但总体相差不大，说明少量的添加钆铁，对低成本N35烧结钕铁硼永磁体的磁性能无较大影响，但是添加钆铁，相应减少镨钕的添加量，总体降低了低成本N35烧结钕铁硼永磁体的生产成本。
其原因可能在于：添加钆铁能够减少甚至消除铸片中的α-Fe使主相晶粒具有明显的柱状晶特征，从而改善了铸片的破碎性能，使氢破碎后的合金粉末粒度分布比较均匀。
结合实施例1、实施例5和对比例1并结合表2可以看出，实施例5中镨钕与铈的质量比为0.8:1，对比例1中镨钕与铈的质量比为0.7:1，实施例1中镨钕与铈的质量比为1.11:1，实施例8中低成本N35烧结钕铁硼永磁体的磁性能较实施例1有所下降，对比例1中低成本N35烧结钕铁硼永磁体的磁性能较实施例1大幅度下降。
这是由于实施例5的原料中镨钕含量偏低，铈的含量偏高，导致磁性能发生恶化，从而降低了低成本N35烧结钕铁硼永磁体的磁性能。而对比例1的原料中镨钕含量过低，铈的含量过高，导致磁性能恶化，从而大大降低了低成本N35烧结钕铁硼永磁体的磁性能。
结合实施例1和实施例6并结合表2可以看出，实施例6中硼与镨钕的质量比为0.17:1，实施例1中硼与镨钕的质量比为0.3:1，实施例6中硼的含量不够高，导致无法获得较高的矫顽力，且低成本N35烧结钕铁硼永磁体中的硼还会影响磁性能，导致总体的磁性能下降。
结合实施例1和对比例2并结合表2可以看出，对比例2中低成本N35烧结钕铁硼永磁体的制备过程中，各原料直接进行熔炼，不进行去污除杂，对比例2中低成本N35烧结钕铁硼永磁体的磁性能较实施例1中略有下降，说明在进行真空熔炼之前，对原料进行去污除杂有利于提高后续工序对低成本N35烧结钕铁硼永磁体的磁性能的提高。
本具体实施例仅仅是对本申请的解释，其并不是对本申请的限制，本领域技术人员在阅读完本说明书后可以根据需要对本实施例做出没有创造性贡献的修改，但只要在本申请的权利要求范围内都受到专利法的保护。
Claims (9)
1.一种低成本N35烧结钕铁硼永磁体，其特征在于，按质量份数计，原料包括如下组分：镨钕87-117份，铈88-105份，硼28-34份，铜0.8-1份，铝1.5-2.5份，钴1-2份，锆1-3份，铁376-383份。
2.根据权利要求1所述的低成本N35烧结钕铁硼永磁体，其特征在于：还包括2-4份钆铁。
3.根据权利要求1所述的低成本N35烧结钕铁硼永磁体，其特征在于：所述镨钕与所述铈的质量比为（0.9-1.2）：1。
4.根据权利要求1所述的低成本N35烧结钕铁硼永磁体，其特征在于：所述硼与所述镨钕的质量比为（0.27-0.33）：1。
5.如权利要求1-4中任一项所述的一种低成本N35烧结钕铁硼永磁体的制备方法，其特征在于，包括如下制备步骤：
S1、按比例称取各原料；
S2、将各原料进行真空熔炼，得到铸片；
S3、将铸片进行氢破碎，得到合金粉末；
S4、将合金粉末在1350-1400kA/m的磁场中取向，然后压制成型，得到坯体；
S5、将坯体在1050-1100℃下烧结3-5h，然后在800-850℃下保温2-3h进行一级回火，于510-560℃下保温2-3h进行二级回火，冷却后得到钕铁硼永磁体。
6.根据权利要求6所述的低成本N35烧结钕铁硼永磁体的制备方法，其特征在于：S2中，各原料在进行真空熔炼之前，先对各原料进行去污除杂。
7.根据权利要求6所述的低成本N35烧结钕铁硼永磁体的制备方法，其特征在于：S3中，合金粉末的粒径为3-5μm。
8.根据权利要求6所述的低成本N35烧结钕铁硼永磁体的制备方法，其特征在于：S4中，压制成型采用垂直钢模压和冷等静压的方式成型。
9.根据权利要求6所述的低成本N35烧结钕铁硼永磁体的制备方法，其特征在于：S5中，钕铁硼永磁体烧结完毕后，对其进行镀层处理。
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