CN113593799B - 一种细晶、高矫顽力烧结钕铁硼磁体及其制备方法 - Google Patents
一种细晶、高矫顽力烧结钕铁硼磁体及其制备方法 Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 18
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 17
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 14
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- 229910052742 iron Inorganic materials 0.000 claims abstract description 9
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Abstract
本发明提供了一种细晶、高矫顽力烧结钕铁硼磁体及其制备方法。所述钕铁硼磁体的化学式为RFeBM，其中，R为稀土元素，Fe为铁，B为硼，R的含量为26‑35wt％，B的含量为0.8‑1.3wt％，M为Co、Ga、Cu、Al、Zr、Ti中的几种，所述的烧结钕铁硼磁体的晶粒尺寸小，且减小晶粒尺寸大小的同时控制磁体中C、O、N元素的含量，从而大幅提高磁体的矫顽力。采用所述方法制备得到的磁体具有更低的C、O、N杂质含量，这样的产品进行扩散处理，可以提供更好的晶界，更好的扩散通道。因此，细晶产品再扩散后可以生产性能更高的磁体。
Description
技术领域
本发明涉及钕铁硼系烧结磁体领域，特别涉及是一种细晶、高矫顽力烧结钕铁硼磁体及其制备方法。
背景技术
钕铁硼永磁材料自发现以来以其优异的磁性能和高的性价比而被广泛应用于通讯、医疗、汽车、电子、航空等领域，但其较低的矫顽力与较差的温度稳定性和耐腐蚀性严重限制其应用范围的拓展。
目前，现有技术中常规通过如下四种方法提高钕铁硼永磁材料的矫顽力：(1)在原材料合金中添加重稀土，提高主相的磁晶各向异性；(2)双合金法，将两种不同矫顽力合金粉末混合并烧结；(3)细化晶粒的方法，随着晶粒尺寸的减小，晶粒的有效散磁场因子变小，磁体矫顽力增加；(4)晶界扩散方法，这种技术使重稀土沿晶界相发生扩散，显著提高晶界处的各向异性常数，达到在少量使用重稀土的情况下明显提高磁体矫顽力。这些方法中，方法(3)是比较优越的。此方法相对于方法(1)和(2)来说，可以不使用重稀土或使用少量的重稀土大幅提高磁体矫顽力同时保证剩磁不变。相对于方法(4)来说，磁体性能的提升不受产品尺寸的影响，并且保证磁体内外性能均匀。
现有文献中还公开了使用高压氩气热等静压烧结的方法控制磁体晶粒大小的方法。首先制备平均粒度为3μm的磁粉，通过此方法最终制备的磁体晶粒大小为5.2μm，致密度为99.5％的烧结磁体。
现有文献中还公开了使用平均粒径为2-5μm的磁粉制备烧结磁体，其中重稀土含量低于0.2％，产品方形度0.95以上。
现有文献中还公开了通过控制磁粉平均粒度为2.4μm，并采用低温烧结获得了晶粒大小为5μm左右的47H磁体，磁体矫顽力在无重稀土时达到17kOe。
上述公开了通过各种方法制备了晶粒大小为5-6μm磁体，通过细化晶粒提高了磁体矫顽力。在无重稀土情况下，产品性能可以做到47H。在无重稀土条件下，如果想继续提高产品性能，需要将晶粒减小到5μm以下。
现有文献中还公开了一种细晶钕铁硼磁体，其中c轴垂直的截面中的晶粒的粒径中值为4.5μm以下。通过减小磁体晶粒大小从而提高磁体矫顽力。
现有文献中还公开了通过细化鳞片柱状晶，制备晶粒大小为0.5-5.0μm的磁体，从而减少重稀土使用量。
上述公开了通过控制鳞片柱状晶大小，细化了磁粉粒度，最终制备了磁体晶粒小于5μm的钕铁硼磁体，从而进一步提高产品矫顽力，但是其中提到的性能提高有限。这主要是因为随着晶粒小于5μm，对应的粉末活性增强，最终磁体中的C、O、N元素含量逐渐升高。C、O、N元素作为杂质消耗晶界中的稀土元素，同时作为反磁化畴的形核点，影响晶界结构，从而导致磁体矫顽力降低。
因此，如果对磁体中的C、O、N杂质元素不进行控制的话，随着磁粉粒度的降低，磁体晶粒减小，磁体矫顽力会出现先上升后下降的趋势。以往的文献中均未提到磁体晶粒减小尤其是小于5μm时，对产品中C、O、N元素的控制及控制方法。
发明内容
为了改善现有技术的不足，本发明提供一种细晶、高矫顽力烧结钕铁硼磁体及其制备方法。所述的烧结钕铁硼磁体的晶粒尺寸小于等于5μm，且减小晶粒尺寸的同时可以很好地控制烧结钕铁硼磁体的C、O、N元素的含量，从而大幅提高烧结钕铁硼磁体的矫顽力。
本发明目的是通过如下技术方案实现的：
一种钕铁硼磁体，所述钕铁硼磁体的化学式为RFeBM，其中，R为稀土元素，Fe为铁，B为硼，R的含量为26-35wt％，B的含量为0.8-1.3wt％，M为Co、Ga、Cu、Al、Zr、Ti中的几种，其中Co的含量为0.5-3.0wt％，Ga的含量为0.05-0.4wt％，Cu的含量为0.05-0.5wt％，Al的含量为0-1.5wt％，Zr或Ti的含量为0-0.3wt％，余者为铁和不可避免的杂质，且磁体中的C、O、N元素的含量满足C+O+N(ppm)≤[1500+(5.0-晶粒大小(μm))×600](ppm)。
根据本发明，所述R的含量例如为26wt％、27wt％、28wt％、29wt％、30wt％、31wt％、32wt％、33wt％、34wt％、35wt％。
根据本发明，所述B的含量例如为0.8wt％、0.9wt％、1wt％、1.1wt％、1.2wt％、1.3wt％。
根据本发明，所述Co的含量例如为0.5wt％、0.8wt％、1wt％、1.2wt％、1.5wt％、2wt％、2.5wt％、3.0wt％。
根据本发明，所述Ga的含量例如为0.05wt％、0.1wt％、0.2wt％、0.3wt％、0.4wt％。
根据本发明，所述Cu的含量例如为0.05wt％、0.1wt％、0.2wt％、0.3wt％、0.4wt％、0.5wt％。
根据本发明，所述Al的含量例如为0.01wt％、0.05wt％、0.1wt％、0.2wt％、0.5wt％、1wt％、1.2wt％、1.5wt％。
根据本发明，所述Zr或Ti的含量例如为0.01wt％、0.05wt％、0.1wt％、0.2wt％、0.3wt％。
根据本发明，所述钕铁硼磁体的晶粒大小为小于等于5μm，例如为：4.5μm、4.3μm、4.8μm、3.8μm、4μm、3μm、2μm、1μm。
本发明还提供一种上述烧结钕铁硼磁体的制备方法，所述方法包括如下步骤：
1)采用甩带-氢爆的方法获得R-Fe-B-M合金微粉；
2)将步骤1)的合金微粉进行气流磨研磨得到粒度D50≤4.0μm的磁粉，将所述磁粉和润滑剂混合，然后将磁粉压制成压坯；
3)将步骤2)的压坯在500-900℃下进行低温烧结，其中在低温烧结时通入≤10kPa氩气、氢气的混合气体，保温0.1-2h后抽真空至小于100pa，循环处理至少1次；然后在980-1040℃下进行高温烧结，保温3-8h，冷却后进行回火处理，制备得到所述烧结钕铁硼磁体。
根据本发明，步骤1)中，所述的甩带-氢爆的方法例如包括如下步骤：
将R-Fe-B-M合金在真空或惰性气体气氛、温度为1200-1600℃条件下熔化，并且将熔体浇注在转速为0.3-4m/s的急冷辊上制成R-Fe-B-M合金甩带，然后将合金甩带在HD氢爆炉内进行氢爆处理，处理前需抽真空小于100pa。
其中，所述合金甩带的厚度为0.1-0.5mm。
根据本发明，步骤2)中，具体包括如下步骤：
将步骤1)的合金微粉进行气流磨研磨处理，其中，气流磨过程中氧含量小于50ppm。
根据本发明，步骤2)中，所述润滑剂的加入量为所述磁粉质量的0.1-0.5wt％。
根据本发明，步骤2)中，所述混合的时间为0.1-3h。所述混合的温度是室温。
根据本发明，步骤2)中，将磁粉在氧含量小于500ppm，取向磁场强度为1-2T的磁取向成型装置中压制成压坯。压坯的大小和尺寸没有特别的定义，可以根据最终产品的所需量进行调整。
根据本发明，步骤3)中，所述低温烧结是在氩气和氢气的混合气氛下进行的，所述混合气氛中，氩气占混合气氛总体积的95-99％，氢气占混合气氛总体积的1-5％。通过在低温烧结过程中通入氩气、氢气的混合气氛，并在特定温度段保温处理，使氢通过磁体的间隙与磁体中的润滑剂及磁粉表面吸附的氧、氮反应，最终反应物被排出，从而降低了磁体中的碳、氧、氮杂质含量，提高产品性能。
根据本发明，步骤3)中，所述低温烧结的温度为500℃、600℃、700℃、800℃、900℃。所述高温烧结的温度为980℃、990℃、1000℃、1010℃、1020℃、1030℃、1040℃。
根据本发明，所述回火处理包括一级回火处理和二级回火处理。
其中，所述一级回火处理的温度为700-900℃，所述一级回火处理的时间为3-7h。所述二级回火处理的温度为450-600℃，所述二级回火处理的时间为3-7h。
根据本发明，采用上述方法可以得到晶粒尺寸小于等于5.0μm的烧结钕铁硼磁体，并且所述钕铁硼磁体中的C+O+N含量(ppm)≤[1500+(5.0-晶粒大小)(μm)×600](ppm)。
本发明的有益效果：
本发明提供了一种细晶、高矫顽力烧结钕铁硼磁体及其制备方法。所述的烧结钕铁硼磁体的晶粒尺寸小，且减小晶粒尺寸大小的同时控制磁体中C、O、N元素的含量，从而大幅提高磁体的矫顽力。采用所述方法制备得到的磁体具有更低的C、O、N杂质含量，这样的产品进行扩散处理，可以提供更好的晶界，更好的扩散通道。因此，细晶产品再扩散后可以生产性能更高的磁体。
附图说明
图1：实施例1中的磁粉粒度测试结果。
图2：实施例1中的磁体使用扫描电镜扫描的断口照片。
具体实施方式
下文将结合具体实施例对本发明做更进一步的详细说明。应当理解，下列实施例仅为示例性地说明和解释本发明，而不应被解释为对本发明保护范围的限制。凡基于本发明上述内容所实现的技术均涵盖在本发明旨在保护的范围内。
下述实施例中所使用的实验方法如无特殊说明，均为常规方法；下述实施例中所用的试剂、材料等，如无特殊说明，均可从商业途径得到。
仪器和设备
本发明中的晶粒大小计算方法如下：利用扫描电镜扫描毛坯断口图片，在断口图片中计算晶粒的个数，然后计算这些晶粒个数在金相图片面积下的平均等面积，根据等面积计算晶粒大小。
本发明中的磁粉粒径D50是采用激光衍射的粒度分布仪进行的测试。
实施例1
(1)通过使用至少99％重量纯度的NdPr、Co、Al、Fe、Cu、Ga、Zr和硼铁在氩气气氛中高频熔化，并将熔体浇注到急冷辊上制成合金，合金的质量百分比为31％NdPr、0.8％Co、0.5％Al、0.2％Cu、0.15％Ga、0.10Zr％、0.96％B、余者为铁和不可避免的杂质。将该合金进行氢化粉碎成粗粉，然后将粗粉进行气流磨研磨，得到的磁粉粒度D50＝3.5μm。将上述气流磨粉添加0.2wt％的润滑剂后混料2h，在常温和磁场强度为2T的取向场的环境下成型。
(2)将坯体放入真空烧结炉内，在600℃下充入10kPa的氩气和氢气的混合气体，其中氩气和氢气的比例为98:2，保温0.5h。保温结束后抽真空至0.1kPa继续升温，在1030℃下烧结6h。保温结束后冷却处理，在900℃进行一级回火处理，时间为3h。在520℃进行二级回火处理，时间为5h。冷却出炉后得到细晶钕铁硼磁体。此磁体称作A1，在A1磁体上加工D10-10mm的样柱(直径10mm，长度10mm)，进行性能测试。
对比例1
其他步骤同实施例1，区别仅在于步骤(2)：
将压坯放入真空烧结炉内，在1030℃下烧结6h。保温结束后冷却处理，在900℃进行一级回火处理，时间为3h。在520℃进行二级回火处理，时间为5h。冷却出炉后得到细晶钕铁硼磁体。此磁体称作B1，在B1磁体上加工D10-10mm的样柱，进行性能测试。
表1给出了A1、B1的各项磁性能指标及CON含量情况
从表1可以看出；按照本发明的方法，在无重稀土、晶粒大小为4.5μm的条件下，实施例1的磁体A1达到了高矫顽力的46H水平。实施例1与对比例1的Br相当，Hcj更高，这主要是实施例的方法较好的控制了杂质含量(C+O+N)的原因。
实施例1与对比例1的杂质含量对比看，实施例1<1500+(5.0-晶粒大小)×600<对比例1。
实施例2
(1)通过使用至少99％重量纯度的NdPr、Dy、Co、Al、Fe、Cu、Ga、Ti和硼铁在氩气气氛中高频熔化，并将熔体浇注到急冷辊上制成合金，合金的质量百分比为32％NdPr、0.3％Dy、1.0％Co、0.8％Al、0.15％Cu、0.15％Ga、0.15Ti％、0.98％B、余者为铁和不可避免的杂质。将该合金进行氢化粉碎成粗粉，然后将粗粉进行气流磨研磨，得到的磁粉粒度D50＝3.2μm。将上述气流磨粉添加0.3wt％的润滑剂后混料2h，在常温和磁场强度为2T的取向场的环境下成型。
(2)将坯体放入真空烧结炉内，在650℃下充入8kPa的氩气和氢气的混合气体，其中氩气和氢气的比例为99:1，保温1h。保温结束后抽真空至小于100pa继续升温至700℃充入5kPa的氩气和氢气的混合气体，其中氩气和氢气的比例为99:1，保温0.5h。保温结束后抽真空至0.1KPa继续升温，在1020℃下烧结5.5h。保温结束后冷却处理，在850℃进行一级回火处理，时间为4h。在550℃进行二级回火处理，时间为5h。冷却出炉后得到细晶钕铁硼磁体。此磁体称作A2，在A2磁体上加工D10-10mm的样柱，进行性能测试。
对比例2
其他步骤同实施例2，区别仅在于步骤(2)：
将压坯放入真空烧结炉内，在1020℃下烧结5.5h。保温结束后冷却处理，在850℃进行一级回火处理，时间为4h。在550℃进行二级回火处理，时间为5h。冷却出炉后得到细晶钕铁硼磁体。此磁体称作B2，在B2磁体上加工D10-10mm的样柱，进行性能测试。
表2给出了A2、B2的各项磁性能指标及CON含量情况
从表2可以看出；按照本发明的方法，在低重稀土的条件下，实施例2的磁体A2达到了高矫顽力的42SH水平。实施例2与对比例2的Br相当，Hcj更高，这主要是实施例2的方法较好的控制了杂质含量(C+O+N)的原因。实施例2与对比例2的杂质含量对比看，实施例2<1500+(5.0-晶粒大小)×600<对比例2。
实施例3
(1)通过使用至少99％重量纯度的NdPr、Dy、Co、Al、Fe、Cu、Ga、Ti和硼铁在氩气气氛中高频熔化，并将熔体浇注到急冷辊上制成合金，合金的质量百分比为31.5％NdPr、0.5％Dy、1.0％Co、0.6％Al、0.2％Cu、0.10％Ga、0.2Ti％、0.98％B、余者为铁和不可避免的杂质。将该合金进行氢化粉碎成粗粉，然后将粗粉进行气流磨研磨，得到的磁粉粒度D50＝2.6μm。将上述气流磨粉添加0.15wt％的润滑剂后混料2h，在常温和磁场强度为2T的取向场的环境下成型。
(2)将坯体放入真空烧结炉内，在800℃下充入6kPa的氩气和氢气的混合气体，其中氩气和氢气的比例为96:4，保温1h。保温结束后抽真空至小于100pa继续在800℃充入6kPa的氩气和氢气的混合气体，其中氩气和氢气的比例为96:4，保温1h。保温结束后抽真空至0.1kPa继续升温，在1000℃下烧结7h。保温结束后冷却处理，在850℃进行一级回火处理，时间为4h。在500℃进行二级回火处理，时间为6h。冷却出炉后得到细晶钕铁硼磁体。此磁体称作A3，在A3磁体上加工D10-10mm的样柱，进行性能测试。
对比例3
其他步骤同实施例3，区别仅在于步骤(2)：
将压坯放入真空烧结炉内，在1000℃下烧结7h。保温结束后冷却处理，在850℃进行一级回火处理，时间为4h。在500℃进行二级回火处理，时间为6h。冷却出炉后得到细晶钕铁硼磁体。此磁体称作B3，在B3磁体上加工D10-10mm的样柱，进行性能测试。
表3：A3、B3的各项磁性能指标及CON含量情况
从表3可以看出；实施例A3与对比例B3的Br相当，Hcj更高，这主要是实施例的方法较好的控制了杂质含量(C+O+N)的原因。随着磁粉粒度减小，理论上对比例磁体矫顽力会增加，但是杂质含量也急剧增加，导致最终的产品的性能降低。实施例与对比例的杂质含量对比看，实施例3<1500+(5.0-晶粒大小)×600<对比例3。
实施例4
(1)通过使用至少99％重量纯度的Nd、Co、Al、Fe、Cu、Ga和硼铁在氩气气氛中高频熔化，并将熔体浇注到急冷辊上制成合金，合金的质量百分比为31％Nd、0.8％Co、0.3％Al、0.2％Cu、0.1Ga％、1％B、余者为铁和不可避免的杂质。将该合金进行氢化粉碎成粗粉，然后将粗粉进行气流磨研磨，得到的磁粉粒度D50＝3.5μm。将上述气流磨粉添加0.1wt％的润滑剂后混料2h，在常温和磁场强度为2T的取向场的环境下成型。
(2)将坯体放入真空烧结炉内，在600℃下充入10kPa的氩气和氢气的混合气体，其中氩气和氢气的比例为99:1，保温0.5h。保温结束后抽真空至0Pa继续升温，在1030℃下烧结6h。保温结束后冷却处理，在900℃进行一级回火处理，时间为3h。在510℃进行二级回火处理，时间为5h。冷却出炉后得到细晶钕铁硼磁体，该磁体标记为基材A4。
将磁体加工成尺寸为20-10-5mm的方片，方片经除油酸洗后进行Tb晶界扩散处理，Tb的扩散量为0.4wt％，此实施例晶界扩散选用热喷涂方法处理，扩散处理后的该产品被称为A5。
对比例4
其他步骤同实施例4，区别仅在于步骤(2)：
将压坯放入真空烧结炉内，在1030℃下烧结6h。保温结束后冷却处理，在900℃进行一级回火处理，时间为3h。在510℃进行二级回火处理，时间为5h。冷却出炉后得到细晶钕铁硼磁体，该磁体标记为基材B4。
将磁体加工成尺寸为20-10-5mm的方片，方片经除油酸洗后进行Tb晶界扩散处理，Tb的扩散量为0.4wt％，此对比例晶界扩散选用热喷涂方法处理，扩散处理后的该产品被称为B5。
表4：A4、A5、B4、B5的各项磁性能指标及CON含量情况
从表4可以看出：A4与B4的Br相当，Hcj更高，这主要是实施例4的方法较好的控制了杂质含量(C+O+N)的原因。A与B4的杂质含量对比看，A4<1500+(5.0-晶粒大小)×600<B4。另外，A4与A5的矫顽力看，A5的矫顽力增加798kA/m。B4与B5的矫顽力看，B5矫顽力增加721kA/m。A4的磁体由于具有更低的C、O、N杂质含量，因此更有利于重稀土的扩散，A5的磁体的矫顽力更高。
以上，对本发明的实施方式进行了说明。但是，本发明不限定于上述实施方式。凡在本发明的精神和原则之内，所做的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (9)
1.一种烧结钕铁硼磁体，其中，所述烧结钕铁硼磁体的化学式为RFeBM，其中，R为稀土元素，Fe为铁，B为硼，R的含量为26-35wt%，B的含量为0.8-1.3wt%，M为Co、Ga、Cu、Al、Zr、Ti中的几种，其中Co的含量为0.5-3.0wt%，Ga的含量为0.05-0.4wt%，Cu的含量为0.05-0.5wt%，Al的含量为0-1.5wt%，Zr或Ti的含量为0-0.3wt%，且Zr或Ti的含量不为0，余者为铁和不可避免的杂质，且磁体中的C、O、N元素的含量满足C+O+N（ppm）≤[1500+（5.0-晶粒大小（μm））×600]（ppm）；
所述烧结钕铁硼磁体的制备方法包括如下步骤：
1）采用甩带-氢爆的方法获得R-Fe-B-M合金微粉；
2）将步骤1）的合金微粉进行气流磨研磨得到粒度D50≤4.0μm的磁粉，将所述磁粉和润滑剂混合，然后将磁粉压制成压坯；
3）将步骤2）的压坯在500-900℃下进行低温烧结，其中在低温烧结时通入≤10kPa氩气、氢气的混合气体，保温0.1-2h后抽真空至小于100pa，循环处理至少1次；然后在980-1040℃下进行高温烧结，保温3-8h，冷却后进行回火处理，制备得到所述烧结钕铁硼磁体；
步骤3）中，所述低温烧结是在氩气和氢气的混合气氛下进行的，所述混合气氛中，氩气占混合气氛总体积的95-99%，氢气占混合气氛总体积的1-5%。
2.根据权利要求1所述的烧结钕铁硼磁体，其中，所述烧结钕铁硼磁体的晶粒大小为小于等于5μm。
3.权利要求1或2所述的烧结钕铁硼磁体的制备方法，所述方法包括如下步骤：
1）采用甩带-氢爆的方法获得R-Fe-B-M合金微粉；
2）将步骤1）的合金微粉进行气流磨研磨得到粒度D50≤4.0μm的磁粉，将所述磁粉和润滑剂混合，然后将磁粉压制成压坯；
3）将步骤2）的压坯在500-900℃下进行低温烧结，其中在低温烧结时通入≤10kPa氩气、氢气的混合气体，保温0.1-2h后抽真空至小于100pa，循环处理至少1次；然后在980-1040℃下进行高温烧结，保温3-8h，冷却后进行回火处理，制备得到所述烧结钕铁硼磁体；
步骤3）中，所述低温烧结是在氩气和氢气的混合气氛下进行的，所述混合气氛中，氩气占混合气氛总体积的95-99%，氢气占混合气氛总体积的1-5%。
4.根据权利要求3所述的制备方法，其中，步骤1）中，所述的甩带-氢爆的方法包括如下步骤：
将R-Fe-B-M合金在真空或惰性气体气氛、温度为1200-1600℃条件下熔化，并且将熔体浇注在转速为0.3-4m/s的急冷辊上制成R-Fe-B-M合金甩带，然后将合金甩带在HD氢爆炉内进行氢爆处理，处理前需抽真空小于100pa。
5.根据权利要求3-4任一项所述的制备方法，其中，步骤2）中，具体包括如下步骤：
将步骤1）的合金微粉进行气流磨研磨处理，其中，气流磨过程中氧含量小于50ppm。
6.根据权利要求3-4任一项所述的制备方法，其中，步骤2）中，所述润滑剂的加入量为所述磁粉质量的0.1-0.5wt%。
7.根据权利要求3-4任一项所述的制备方法，其中，步骤2）中，将磁粉在氧含量小于500ppm，取向磁场强度为1-2T的磁取向成型装置中压制成压坯。
8.根据权利要求3-4任一项所述的制备方法，其中，所述回火处理包括一级回火处理和二级回火处理。
9.根据权利要求8所述的制备方法，其中，所述一级回火处理的温度为700-900℃，所述一级回火处理的时间为3-7h;所述二级回火处理的温度为450-600℃，所述二级回火处理的时间为3-7h。
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