CN112951534B - 一种烧结钕铁硼磁体及其制备方法 - Google Patents

一种烧结钕铁硼磁体及其制备方法 Download PDF

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CN112951534B
CN112951534B CN202110142574.2A CN202110142574A CN112951534B CN 112951534 B CN112951534 B CN 112951534B CN 202110142574 A CN202110142574 A CN 202110142574A CN 112951534 B CN112951534 B CN 112951534B
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曾玉军
韩明磊
刘照勇
张学良
薛志刚
曾全进
董宇翔
赵俊星
风兰
刘泽
张霞
张家良
陈湘军
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Baotou Jinmeng Magnetic Materials Co ltd
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Abstract

本发明公开了一种烧结钕铁硼磁体及其制备方法，其中，一种烧结钕铁硼磁体包括如下质量百分含量的原料：磁感应强度＞1.2T的铁粉或钢粉1％‑40％，镨钕金属氢化粉不大于10％，剩余为钕铁硼细粉，以上各组分的质量百分含量之和为百分之百。其制备方法包括：按质量百分含量称取各原料；将称取的各所述原料混合均匀，再通过磁场压制成型、等静压、烧结、回火，制备得到烧结钕铁硼磁体。利用本发明配方及制备方法制备得到的烧结钕铁硼磁体，其磁性能够达到现有技术制备的烧结钕铁硼磁体磁性的同时，大大降低了稀土元素的添加量，从而大幅度降低了烧结钕铁硼磁体的原材料成本，另外，还为国家节约大量稀缺的稀土资源。

Description

一种烧结钕铁硼磁体及其制备方法
技术领域：
本发明属于磁性材料技术领域，特别是涉及一种烧结钕铁硼磁体及其制备方法。
背景技术：
现有烧结钕铁硼制备流程是熔炼、氢碎、气流磨、压型、等静压、烧结，具体方法为：将稀土金属、硼铁、纯铁和其他元素金属，经过熔炼做成钕铁硼合金，再将钕铁硼合金置于氢碎炉中初步破碎成粗粉，将粗粉用气流磨破碎成1-10微米左右的细粉，将细粉置于磁场压机中取向成型，再用等静压在150-250MPa的压力下再次压制，最后用烧结炉经过1000-1100℃高温烧结，用880-950℃回火3小时，再在440-640℃下回火4小时制成钕铁硼磁体。钕铁硼磁体是由主相和富钕相组成，主相为Nd2Fe14B，主相中Nd的质量比为26.68％，富钕相含有大量的Nd，再加上熔炼过程中稀土会有烧损，所以熔炼配方中稀土的添加量无法低于钕铁硼中Re的质量百分比26.68％wt，由于稀土元素价格高昂，所以钕铁硼磁体的成本高昂。
发明内容：
本发明的第一个目的在于提供一种磁性好，稀土材料用量小，原材料成本低的烧结钕铁硼磁体。
本发明的第二个目的在于提供一种磁性好，稀土材料用量小，原材料成本低的烧结钕铁硼磁体的制备方法。
本发明的第一个目的由如下技术方案实施：一种烧结钕铁硼磁体，其包括如下质量百分含量的原料：磁感应强度＞1.2T的铁粉或钢粉1％-40％，镨钕金属氢化粉不大于10％，剩余为钕铁硼细粉，以上各组分的质量百分含量之和为百分之百。
进一步，所述铁粉为工业纯铁粉、羟基铁粉或碳基铁粉中的任意一种或一种以上的组合；所述钢粉为低碳钢粉或硅钢粉或低碳钢粉与硅钢粉的组合；所述铁粉或所述钢粉的粒度为1-10微米。
进一步，所述镨钕金属氢化粉按如下方法制备：
(1)将镨钕金属装入旋转氢破炉中，抽真空度小于2Pa后，通入纯度大于99.99％的氢气破碎氢化后形成镨钕氢化物；
(2)将所述镨钕氢化物用气流磨磨成1-10微米，制得镨钕金属氢化粉。
进一步，所述钕铁硼磁粉按如下方法制备：
(1)按质量份数称取如下原料：稀土金属RE为29-33份；添加金属M为1-3份；B为0.9-1份；Fe为63-69.1份；
(2)将称取的各所述原料用熔炼炉经过1400-1600℃融化后精炼5分钟，再浇筑冷却制成厚度为1-5mm的钕铁硼合金；
(3)将所述钕铁硼合金装入旋转氢破炉中，抽真空度小于2Pa后，通入纯度大于99.99％的氢气破碎后制得粗粉；然后将所述粗粉用气流磨磨成1-10微米，制得钕铁硼细粉。
进一步，所述添加金属M为Co、Cu、Al、Ga、Nb或Zr中的任意一种或一种以上的组合。
本发明的第二个目的由如下技术方案实施：一种烧结钕铁硼磁体的制备方法，其包括如下步骤：
步骤一、按如下质量百分含量称取各原料：磁感应强度＞1.2T的铁粉或钢粉1％-40％，镨钕金属氢化粉不大于10％，剩余为钕铁硼细粉，以上各组分的质量百分含量之和为百分之百；
步骤二、将称取的各所述原料混合均匀，再通过磁场压制成型、等静压、烧结、回火，制备得到烧结钕铁硼磁体。
进一步，所述铁粉为工业纯铁粉、羟基铁粉或碳基铁粉中的任意一种或一种以上的组合；所述钢粉为低碳钢粉或硅钢粉或低碳钢粉与硅钢粉的组合；所述铁粉或所述钢粉的粒度为1-10微米。
进一步，所述镨钕金属氢化粉按如下方法制备：
(1)将镨钕金属装入旋转氢破炉中，抽真空度小于2Pa后，通入纯度大于99.99％的氢气破碎氢化后形成镨钕氢化物；
(2)将所述镨钕氢化物用气流磨磨成1-10微米，制得镨钕金属氢化粉。
进一步，所述钕铁硼细粉按如下方法制备：
(1)按质量份数称取如下原料：稀土金属RE为29-33份；添加金属M为1-3份；B为0.9-1份；Fe为63-69.1份；
(2)将称取的各所述原料用熔炼炉经过1400-1600℃融化后精炼5分钟，再浇筑冷却制成厚度为1-5mm的钕铁硼合金；
(3)将所述钕铁硼合金装入旋转氢破炉中，抽真空度小于2Pa后，通入纯度大于99.99％的氢气破碎后制得粗粉；然后将所述粗粉用气流磨磨成1-10微米，制得钕铁硼细粉。
进一步，所述添加金属M为Co、Cu、Al、Ga、Nb或Zr中的任意一种或一种以上的组合。
本发明中，钕铁硼细粉、铁粉和镨钕金属氢化粉混合均匀后，经过烧结形成致密化的硬磁体。钕铁硼晶粒作为该硬磁体的磁性能的来源，铁粉颗粒属于软磁体起到磁性能过度的作用，所以基本不影响剩磁的降低。由于大量铁粉的加入，在烧结过程中势必会导致冨钕相的不足，进而导致矫顽力的下降，镨钕金属氢化粉的添加，一是为了补充富钕相，二也是为了消耗铁粉中的氧，降低对矫顽力的影响；从而保证制备得到的钕铁硼磁体的磁性能够达到现有技术制备的烧结钕铁硼磁体磁性的同时，大大降低了稀土元素的添加量，从而大幅度降低了烧结钕铁硼磁体的原材料成本。
本发明的优点：利用本发明配方及制备方法制备得到的烧结钕铁硼磁体，其磁性能够达到现有技术制备的烧结钕铁硼磁体磁性的同时，大大降低了稀土元素的添加量，从而大幅度降低了烧结钕铁硼磁体的原材料成本，另外，还为国家节约大量稀缺的稀土资源。
附图说明：
图1为背景技术中记载的制备方法制备得到的烧结钕铁硼磁体的磁性能检测图。
图2为实施例2制备得到的烧结钕铁硼磁体的磁性能检测图。
图3为实施例4制备得到的烧结钕铁硼磁体的磁性能检测图。
图4为实施例6制备得到的烧结钕铁硼磁体的磁性能检测图。
具体实施方式：
实施例1：一种烧结钕铁硼磁体，其包括如下质量百分含量的原料：磁感应强度＞1.2T、粒度为1-10微米的工业纯铁粉18.5％，镨钕金属氢化粉1.5％，钕铁硼细粉80％，以上各组分的质量百分含量之和为百分之百，并加入总原料质量1‰的润滑剂。
其中，镨钕金属氢化粉按如下方法制备：
(1)将镨钕金属装入旋转氢破炉中，抽真空度小于2Pa后，通入纯度大于99.99％的氢气破碎氢化后形成镨钕氢化物；
(2)将镨钕氢化物用气流磨磨成1-10微米，制得镨钕金属氢化粉。
钕铁硼细粉按如下方法制备：
(1)按质量份数称取如下原料：稀土金属RE为31份；添加金属M为2份；B为0.9份；Fe为66.1份；本实施例中，稀土金属RE按质量份计包括镨钕合金29份、Dy2.0份，添加金属M按质量份计包括Co1份，Cu0.15份，Al 0.4份，Ga 0.2份，Zr0.1份，Nb0.15份。
(2)将称取的各原料用熔炼炉经过1400-1600℃融化后精炼5分钟，再浇筑冷却制成厚度为1-5mm的钕铁硼合金；
(3)将钕铁硼合金装入旋转氢破炉中，抽真空度小于2Pa后，通入纯度大于99.99％的氢气破碎后制得粗粉；然后将粗粉用气流磨磨成1-10微米，制得钕铁硼细粉。
实施例2：实施例1中烧结钕铁硼磁体的制备方法，其包括如下步骤：
步骤一、按如下质量百分含量称取各原料：磁感应强度＞1.2T、粒度为1-10微米的工业纯铁粉18.5％，镨钕金属氢化粉1.5％，钕铁硼细粉80％，以上各组分的质量百分含量之和为百分之百，并加入总原料质量1‰的润滑剂；
步骤二、将称取的各原料混合均匀，再通过磁场压制成型、等静压、烧结、回火，制备得到烧结钕铁硼磁体；具体制备方法为：将称取的各原料混合均匀后，置于磁场＞1.2T的成型压机中取向成型，让粉末颗粒的磁场方向与压机磁场方向一致，再用0.1-1MPa的压力压制到密度为3.6-4.5g/立方厘米，再用等静压机在150-250Mpa的压力下压制成4.3-4.7g/立方厘米，然后置于真空烧结炉中用1000-1100℃烧结4小时，用880-950℃回火3小时，再用440-640℃回火4小时，制备得到烧结钕铁硼磁体。
本实施例与现有技术(即背景技术中记载的制备方法)比较，稀土元素的使用量降低13.66％。
实施例3：一种烧结钕铁硼磁体，其包括如下质量百分含量的原料：磁感应强度＞1.2T、粒度为1-10微米的碳基铁粉40％，镨钕金属氢化粉4％，钕铁硼细粉56％，以上各组分的质量百分含量之和为百分之百，并加入总原料质量1‰的润滑剂。
镨钕金属氢化粉按如下方法制备：
(1)将镨钕金属装入旋转氢破炉中，抽真空度小于2Pa后，通入纯度大于99.99％的氢气破碎氢化后形成镨钕氢化物；
(2)将镨钕氢化物用气流磨磨成1-10微米，制得镨钕金属氢化粉。
钕铁硼细粉按如下方法制备：
(1)按质量份数称取如下原料：稀土金属RE为32份；添加金属M为2份；B为1份；Fe为65份；本实施例中，稀土金属RE按质量份计包括镨钕合金30份、Tb2份，添加金属M按质量份计包括Co1份，Cu0.15份，Al 0.4份，Ga 0.2份，Zr0.1份，Nb0.15份。
(2)将称取的各原料用熔炼炉经过1400-1600℃融化后精炼5分钟，再浇筑冷却制成厚度为1-5mm的钕铁硼合金；
(3)将钕铁硼合金装入旋转氢破炉中，抽真空度小于2Pa后，通入纯度大于99.99％的氢气破碎后制得粗粉；然后将粗粉用气流磨磨成1-10微米，制得钕铁硼细粉。
实施例4：实施例3烧结钕铁硼磁体的制备方法，其包括如下步骤：
步骤一、按如下质量百分含量称取各原料：磁感应强度＞1.2T、粒度为1-10微米的碳基铁粉40％，镨钕金属氢化粉4％，钕铁硼细粉56％，以上各组分的质量百分含量之和为百分之百，并加入总原料质量1‰的润滑剂。
步骤二、将称取的各原料混合均匀，再通过磁场压制成型、等静压、烧结、回火，制备得到烧结钕铁硼磁体；具体制备方法为：将称取的各原料混合均匀后，置于磁场＞1.2T的成型压机中取向成型，让粉末颗粒的磁场方向与压机磁场方向一致，再用0.1-1MPa的压力压制到密度为3.6-4.5g/立方厘米，再用等静压机在150-250Mpa的压力下压制成4.3-4.7g/立方厘米，然后置于真空烧结炉中用1000-1100℃烧结4小时，用880-950℃回火3小时，再用440-640℃回火4小时，制备得到烧结钕铁硼磁体。
本实施例与现有技术(即背景技术中记载的制备方法)比较，稀土元素的使用量降低31.5％。
实施例5：一种烧结钕铁硼磁体，其包括如下质量百分含量的原料：磁感应强度＞1.2T、粒度为1-10微米的低碳钢粉8％，镨钕金属氢化粉1％，钕铁硼细粉91％，以上各组分的质量百分含量之和为百分之百，并加入总原料质量1‰的润滑剂。
镨钕金属氢化粉按如下方法制备：
(1)将镨钕金属装入旋转氢破炉中，抽真空度小于2Pa后，通入纯度大于99.99％的氢气破碎氢化后形成镨钕氢化物；
(2)将镨钕氢化物用气流磨磨成1-10微米，制得镨钕金属氢化粉。
钕铁硼细粉按如下方法制备：
(1)按质量份数称取如下原料：稀土金属RE为30份；添加金属M为1份；B为0.9份；Fe为68.1份；本实施例中，稀土金属RE为按质量份计包括镨钕合金27份和Tb3份，添加金属M按质量份计包括Co0.2份，Cu0.15份，Al0.45份，Ga0.1份，Zr0.1份。
(2)将称取的各原料用熔炼炉经过1400-1600℃融化后精炼5分钟，再浇筑冷却制成厚度为1-5mm的钕铁硼合金；
(3)将钕铁硼合金装入旋转氢破炉中，抽真空度小于2Pa后，通入纯度大于99.99％的氢气破碎后制得粗粉；然后将粗粉用气流磨磨成1-10微米，制得钕铁硼细粉。
实施例6：实施例5烧结钕铁硼磁体的制备方法，其包括如下步骤：
步骤一、按如下质量百分含量称取各原料：磁感应强度＞1.2T、粒度为1-10微米的低碳钢粉8％，镨钕金属氢化粉1％，钕铁硼细粉91％，以上各组分的质量百分含量之和为百分之百，并加入总原料质量1‰的润滑剂。
步骤二、将称取的各原料混合均匀，再通过磁场压制成型、等静压、烧结、回火，制备得到烧结钕铁硼磁体；具体制备方法为：将称取的各原料混合均匀后，置于磁场＞1.2T的成型压机中取向成型，让粉末颗粒的磁场方向与压机磁场方向一致，再用0.1-1MPa的压力压制到密度为3.6-4.5g/立方厘米，再用等静压机在150-250Mpa的压力下压制成4.3-4.7g/立方厘米，然后置于真空烧结炉中用1000-1100℃烧结4小时，用880-950℃回火3小时，再用440-640℃回火4小时，制备得到烧结钕铁硼磁体。
本实施例与现有技术(即背景技术中记载的制备方法)比较，稀土元素的使用量降低5.55％。
实施例2、4、6与现有技术(即背景技术中记载的制备方法)制备得到的烧结钕铁硼磁体的磁性能对比如下表及图1-4所示。
Figure BDA0002929467440000091
Figure BDA0002929467440000101
测试方法依据《GB/T 13560-2017烧结钕铁硼永磁材料》。
通过上表数据可以看出，利用本发明配方及制备方法制备得到的烧结钕铁硼磁体的磁性能与现有技术制备得到的烧结钕铁硼磁体的磁性能相当，但稀土的用量大幅度降低，进而降低了原材料成本，同时节省了大量的稀土资源。
以上仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (10)

1.一种烧结钕铁硼磁体，其特征在于，其包括如下质量百分含量的原料：磁感应强度＞1.2T的铁粉或钢粉8％-40％，镨钕金属氢化粉4％-10％，剩余为钕铁硼细粉，以上各组分的质量百分含量之和为百分之百；所述铁粉为工业纯铁粉、羟基铁粉或碳基铁粉中的任意一种或一种以上的组合；所述钢粉为低碳钢粉或硅钢粉或低碳钢粉与硅钢粉的组合。
2.根据权利要求1所述的一种烧结钕铁硼磁体，其特征在于，所述铁粉或所述钢粉的粒度为1-10微米。
3.根据权利要求1所述的一种烧结钕铁硼磁体，其特征在于，所述镨钕金属氢化粉按如下方法制备：
(1)将镨钕金属装入旋转氢破炉中，抽真空度小于2Pa后，通入纯度大于99.99％的氢气破碎氢化后形成镨钕氢化物；
(2)将所述镨钕氢化物用气流磨磨成1-10微米，制得镨钕金属氢化粉。
4.根据权利要求1所述的一种烧结钕铁硼磁体，其特征在于，所述钕铁硼细粉按如下方法制备：
(1)按质量份数称取如下原料：稀土金属RE为29-33份；添加金属M为1-3份；B为0.9-1份；Fe为63-69.1份；
(2)将称取的各所述原料用熔炼炉经过1400-1600℃融化后精炼5分钟，再浇筑冷却制成厚度为1-5mm的钕铁硼合金；
(3)将所述钕铁硼合金装入旋转氢破炉中，抽真空度小于2Pa后，通入纯度大于99.99％的氢气破碎后制得粗粉；然后将所述粗粉用气流磨磨成1-10微米，制得钕铁硼细粉。
5.根据权利要求4所述的一种烧结钕铁硼磁体，其特征在于，所述添加金属M为Co、Cu、Al、Ga、Nb或Zr中的任意一种或一种以上的组合。
6.一种烧结钕铁硼磁体的制备方法，其特征在于，其包括如下步骤：
步骤一、按如下质量百分含量称取各原料：磁感应强度＞1.2T的铁粉或钢粉8％-40％，镨钕金属氢化粉4％-10％，剩余为钕铁硼细粉，以上各组分的质量百分含量之和为百分之百；所述铁粉为工业纯铁粉、羟基铁粉或碳基铁粉中的任意一种或一种以上的组合；所述钢粉为低碳钢粉或硅钢粉或低碳钢粉与硅钢粉的组合；
步骤二、将称取的各所述原料混合均匀，再通过磁场压制成型、等静压、烧结、回火，制备得到烧结钕铁硼磁体。
7.根据权利要求6所述的一种烧结钕铁硼磁体的制备方法，其特征在于，所述铁粉或所述钢粉的粒度为1-10微米。
8.根据权利要求6所述的一种烧结钕铁硼磁体的制备方法，其特征在于，所述镨钕金属氢化粉按如下方法制备：
(1)将镨钕金属装入旋转氢破炉中，抽真空度小于2Pa后，通入纯度大于99.99％的氢气破碎氢化后形成镨钕氢化物；
(2)将所述镨钕氢化物用气流磨磨成1-10微米，制得镨钕金属氢化粉。
9.根据权利要求6所述的一种烧结钕铁硼磁体的制备方法，其特征在于，所述钕铁硼细粉按如下方法制备：
(1)按质量份数称取如下原料：稀土金属RE为29-33份；添加金属M为1-3份；B为0.9-1份；Fe为63-69.1份；
(2)将称取的各所述原料用熔炼炉经过1400-1600℃融化后精炼5分钟，再浇筑冷却制成厚度为1-5mm的钕铁硼合金；
(3)将所述钕铁硼合金装入旋转氢破炉中，抽真空度小于2Pa后，通入纯度大于99.99％的氢气破碎后制得粗粉；然后将所述粗粉用气流磨磨成1-10微米，制得钕铁硼细粉。
10.根据权利要求9所述的一种烧结钕铁硼磁体的制备方法，其特征在于，所述添加金属M为Co、Cu、Al、Ga、Nb或Zr中的任意一种或一种以上的组合。
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添加钆及钇的钕铁硼永磁材料制备工艺研究;孟凡伟;《中国优秀硕士学位论文全文数据库》;20100815;C042-11 *

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