CN111276309A - 一种热压成型制备稀土永磁体的方法 - Google Patents

一种热压成型制备稀土永磁体的方法 Download PDF

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CN111276309A
CN111276309A CN201811471014.6A CN201811471014A CN111276309A CN 111276309 A CN111276309 A CN 111276309A CN 201811471014 A CN201811471014 A CN 201811471014A CN 111276309 A CN111276309 A CN 111276309A
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alloy
rare earth
permanent magnet
hot press
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董元
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Ningbo Jinke Automation Equipment Co ltd
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Abstract

本发明涉及钕铁硼稀土永磁材料的制备方法，具体为一种热压成型制备稀土永磁体的方法。解决现有技术制备的稀土永磁体剩磁和矫顽力不能同时高的问题。本发明在HD处理过程中渗入RTM合金，RTM粘在粗粉末表面和沿着晶界渗入粗粉末内部，热压温度较低，晶粒几乎没有长大，在没有Dy、Tb的条件下，得到了较高的矫顽力。如果渗入的是含Dy、Tb的合金，这些原子在预热和热处理时扩散到主相的表层、实现晶界硬化。在剩磁降低很小的前提下，极大的提高了矫顽力。

Description

一种热压成型制备稀土永磁体的方法
技术领域
本发明涉及钕铁硼稀土永磁材料的制备方法，具体为一种热压成型制备稀土永磁体的方法。
背景技术
专利号为201410094229 .6的中国专利公开了一种使用热压来制造用于永磁体的磁材料的方法，该方法将包含Nd、Fe和B的核粉末形式的第一材料，和包含金属合金形式的Dy、Tb或此两者的表面粉末形式的第二材料进行组合，使得形成涂覆的、类复合物材料，其具有组成所述第二材料的Dy或Tb的非均匀分布，然后再进行热压成型。对于1-5微米的颗粒，在其表面涂覆1-10nm的膜是现有技术所做不到的，或工业化生产所做不到的。给出的机械研磨、漩涡涂覆、离子溅射、高压粒子溅射等涂敷方案在实际中很难实施。其描述是涂敷1-100微米，其厚度已经和颗粒的大小接近，过多的富相一定会降低材料的性能。甚至会低于现有的烧结磁体的性能。
发明内容
本发明解决上述现有技术存在的缺陷和问题，提供一种热压成型制备稀土永磁体的方法。
本发明是采用如下技术方案实现的：一种热压成型制备稀土永磁体的方法，包括如下步骤：
1）熔炼RFeB合金，R是Nd、Pr、Dy、Tb、Ce、La、Gd、Ho、Y的一种或多种的组合，RFeB合金中稀土R含量在27.5--30.5%质量百分比；RFeB合金中还包含0.2-2%质量百分比的金属组合物，金属组合物是Al、Cu、Ga、Zr、Nb的一种或多种任意比例的组合；用Co替代1%-10%的Fe；
2）对母合金进行HD处理，并在这个过程中渗入RTM合金；其中RT是Nd、Pr、Dy、Tb、Gd、Ho、Y、Sc的一种或任几种以任意比例的组合，M是Cu、Al、Ga的一种或任几种以任意比例的组合；
3）将步骤2）的产物进行气流粉碎；
4）在常温下进行磁场成型；
5）真空预热；
6）热压，进一步提高密度；
7）时效，得到磁体。
在HD工艺的饱和吸氢后，将温度提高到750-950℃，进行渗透，RTM会粘在碎末的表面和沿着晶界渗入到合金内部。
在此后进行气流粉碎中，破碎到1-6微米。
在磁场取向成型后，在真空中充分预热，650-950℃，排出吸附的气体、挥发各种有机添加剂和残余的氢。
将预热后的生坯立即放入和预热温度接近的膜具中，施加25-120MPa的压力，进行热压。密度达到理论密度的99.8-99.9%。熔化的富相在压力下挤入缝隙，提高了密度。
在这个温度下，晶粒几乎没有长大，保持气流磨后的大小。如果渗入的是和主相不同的稀土元素，在预热和时效处理时，会部分扩散到主相的表层。如果渗入的是Dy、Tb、Ho等高各向异性场的元素，起到了硬化晶界的作用。矫顽力大幅度提高，而剩磁降低很少。
热压成型技术是现有公知的技术，在陶瓷、硬质合金等领域已经得到了广泛的应用。和现有的钕铁硼技术的结合，可以做到在不添加重稀土元素的条件下，矫顽力可达到1350KA/m以上。渗入微量Dy、Tb、Ho等高各向异性场的元素，矫顽力可达到2388KA/m以上。
进一步地，步骤2）中RTM合金渗入量是母合金质量的0.5-4.5%，是根据对磁体性能的要求来选择渗入的元素和量，即保证了磁材性能又优化了材料用量，从而降低成本。
再进一步，步骤2）中渗入物RTM合金， RT占65--100%，M占0--35%，通过添加金属Cu、Al、Ga可提高液相侵润性和流动性，有益于降低热压的压力。稀土元素的选择，根据所需磁体性能而定，对于矫顽力1350KA/m以下产品，选择Nd、Pr、Gd。对于要求1350KA/m矫顽力以上产品，要选择Dy、Tb、Ho元素。
本发明所述方法得到的磁材性能与上述现有技术相比有很大提高。降低或完全省去重稀土的使用量。
具体实施方式
一种热压成型制备稀土永磁体的方法，包括如下步骤：
1）熔炼RFeB合金，R是Nd、Pr、Dy、Tb、Ce、La、Gd、Ho、Y的一种或多种的组合，RFeB合金中稀土R含量在27.5--30.5%质量百分比（例如，可选用27.5%、28%、28.5%、29%、30.5%）；RFeB合金中还包含0.2-2%质量百分比的金属组合物（例如，可选用0.2%、0.5%、0.8%、1.0%、1.5%、2%），金属组合物是Al、Cu、Ga、Zr、Nb的一种或多种任意比例的组合；用Co替代1%-10%的Fe；
2）对母合金进行HD处理，并在这个过程中渗入RTM合金；其中RT是Nd、Pr、Dy、Tb、Gd、Ho、Y、Sc的一种或任几种以任意比例的组合，M是Cu、Al、Ga的一种或任几种以任意比例的组合；
3）将步骤2）的产物进行气流粉碎；
4）在常温下进行磁场成型；
5）真空预热；
6）热压，进一步提高密度；
7）时效，得到磁体。
步骤2）中RTM合金渗入量是RFeB合金质量的0.5-4.5%（例如，可选用0.5%、1%、2%、3%、3.5%、4%、4.5%）。
步骤2）中RTM合金， RT占65--100%，M占0--35%（例如，可选用RT占65%，M占35%；RT占100%，M占0%；RT占75%，M占25%；RT占85%，M占15%；RT占95%，M占5%）。
RTM合金可以用RTFeB合金替代，RT是Nd、Pr、Dy、Tb、Gd、Ho、Y、Sc的一种或任几种以任意比例的组合；RT含有量超过RTFeB合金的50%的质量比。
步骤1）所述RFeB合金为熔炼稀土R含量在27.5--30.5%质量百分比的RFeB合金速凝薄片。
步骤2）所述的HD处理过程包括如下步骤：
a）将1-100微米的RTM合金粉末和速凝片合金混合并装入HD处理炉；
b）真空达到0.1Pa后，充入氢气，保持压力0.05-0.2MPa（例如，可选用0.05 MPa、0.1MPa、0.15 MPa、0.2 MPa）；进行饱和吸氢；
c）在750-950℃进行渗透和脱氢（例如，可选用750℃、800℃、850℃、900℃、950℃）；60min-240min（例如，可选用60 min、120 min、180 min、240min）；
d）然后停止加热，冷却到200℃，二次吸氢；吸氢量500-1000ppm（例如，可选用500 ppm、600 ppm、700 ppm、800 ppm、900 ppm、1000 ppm）；
e）充Ar，通水冷却，冷却到室温后密封出炉。
步骤3）气流粉碎，压缩N2做动力，磨至平均粒度1-6微米（例如，可选用1微米、2微米、3微米、4微米、5微米、6微米）。
步骤4）在常温下进行磁场成型；在取向磁场大于1.2T下压制，密度在3.6-4.2g/cm2，所暴露空间的氧气浓度小于500PPM。为了进一步提高密度，还可进行二次成型，即等静压，等静压压力在150MPa-300MPa（例如，可选用150 MPa、210 MPa、250 MPa、300 MPa）。
步骤5）预热：在10-1--10-4Pa真空下，进行650℃--950℃（例如，可选用650℃、700℃、800℃、900℃、950℃）预热1-10小时（例如，可选用1小时、2小时、3小时、4小时、5小时、6小时、7小时、8小时、9小时、10小时）；
步骤6）预热后立即放入和预热温度接近的模腔内，施加25-120MPa的压力（例如，可选用25MPa、40MPa、50MPa、60MPa、90MPa、120MPa），保压0.3-10分钟（例如，可选用0.3分钟、0.5分钟、0.8分钟、1分钟、3分钟、5分钟、6分钟、8分钟、9分钟、10分钟），热压在氧含量小于200PPM的惰性气体保护中进行，压力为0MPa，即和外部没有压力差；自然冷却或强制冷却到室温。
热压膜具的断面尺寸，要根据预热后生坯收缩后的尺寸加0.05-0.2mm，以便于入模。
步骤7）热压成型后的产品，可选择进行时效处理，时效温度450-950℃（例如，可选用450℃、500℃、600℃、700℃、800℃、900℃、950℃）。
实施例1
RFeB合金的材料配比如下：
Figure DEST_PATH_IMAGE001
按上述配方真空熔炼，速凝甩带得到0.20～0.45mm厚的RFeB合金——速凝薄片。
按照本申请所述方法对速凝薄片进行加工，其中，在HD过程中渗入的RTM合金为DyCu合金粉末，其中Nd90%，Cu10%。
为了保证性能，要求速凝薄片的表明没有氧化层，要求速凝炉出料在密封桶内。在加入氢碎炉时，也要严格保护，不能接触空气。
将速凝薄片和占速凝薄片总质量1%的DyCu合金粉末，装入HD处理炉。真空达到0.1Pa后，进行饱和吸氢，氢气压力0.05MPa-0.2MPa。随后进行900℃脱氢，120min。然后停止加热，保持真空状态。冷却到200℃后，二次吸氢；吸氢量800ppm；冷却后密封出炉。用气流磨磨至平均粒度2-4微米。
实验膜具尺寸25*50mm，模腔深度150mm。在低于500ppm的低氧环境下磁场成型，加入525g磁粉，施加15吨的压力，得到25*50*50生坯。在真空度0.01Pa，900℃真空预热，然后再放入模腔，进行40MPa的保压60S，得到密度7.6g/cm2 ，冷却后进行900℃时效处理，得到磁性能55H的性能。剩磁14.5KGs，HcJ 1350KA/m。
实施例2
RFeB合金的材料配比如下：
Figure 28118DEST_PATH_IMAGE001
按上述配方真空熔炼，速凝甩带得到0.20～0.45mm厚的RFeB合金——速凝薄片。
制备TbCuAl合金及其粉末，Tb80%、Cu10%、Al10%（质量百分比）。
与实施例1相同的实施方法，在这个过程中TbCuAl一部分粘在氢碎后的粗颗粒表面，一部分扩散进入粗粉末中。
用和实施例1相同的方法进行气流粉碎、磁场成型、真空预热、热压、回火处理。得到磁性能50EH的性能。剩磁14.0KGs，HcJ 2388KA/m。

Claims (10)

1.一种热压成型制备稀土永磁体的方法，其特征在于，包括如下步骤：
1）熔炼RFeB合金，R是Nd、Pr、Dy、Tb、Ce、La、Gd、Ho、Y的一种或多种的组合，RFeB合金中稀土R含量在27.5--30.5%质量百分比； RFeB合金中还包含0.2-2%质量百分比的金属组合物，金属组合物是Al、Cu、Ga、Zr、Nb的一种或多种任意比例的组合；用Co替代1%-10%的Fe；
2）对母合金进行HD处理，并在这个过程中渗入RTM合金；其中RT是Nd、Pr、Dy、Tb、Gd、Ho、Y、Sc的一种或任几种以任意比例的组合，M是Cu、Al、Ga的一种或任几种以任意比例的组合；
3）将步骤2）的产物进行气流粉碎；
4）在常温下进行磁场成型；
5）真空预热；
6）热压，进一步提高密度；
7）时效，得到磁体。
2.根据权利要求1所述的一种热压成型制备稀土永磁体的方法，其特征在于，步骤2）中的RTM合金， RT占65--100%，M占0--35%。
3.根据权利要求1或2所述的一种热压成型制备稀土永磁体的方法，其特征在于，步骤2）中RTM合金渗入量是RFeB合金质量的0.5-4.5%。
4.根据权利要求1所述的一种热压成型制备稀土永磁体的方法，其特征在于，步骤2）所述的HD处理过程包括如下步骤：
a）将1-100微米的RTM合金粉末和速凝片合金混合并装入HD处理炉；
b）真空达到0.1Pa后，充入氢气，保持压力0.05-0.2MPa，进行饱和吸氢；
c）在750-950℃进行渗透和脱氢，60min-240min；
d）然后停止加热，冷却到200℃，二次吸氢；吸氢量500-1000ppm；
e）充Ar，通水冷却，冷却到室温后密封出炉。
5.根据权利要求1所述的一种热压成型制备稀土永磁体的方法，其特征在于，步骤3）气流粉碎，压缩N2做动力，磨至平均粒度1-6微米。
6.根据权利要求1一种热压成型制备稀土永磁体的方法，其特征在于，步骤4）在取向磁场大于1.2T下压制，压制密度在3.6-4.2g/cm2，所暴露空间的氧气浓度小于500PPM。
7.根据权利要求1一种热压成型制备稀土永磁体的方法，其特征在于，RTM合金用RTFeB合金替代，RT是Nd、Pr、Dy、Tb、Gd、Ho、Y、Sc的一种或任几种以任意比例的组合；RT含有量超过RTFeB合金的50%的质量比。
8.根据权利要求1所述的一种热压成型制备稀土永磁体的方法，其特征在于，步骤5）、6）热压成型包括如下步骤：在10-1--10-4Pa真空下，进行650℃--950℃预热1-10小时；预热后立即放入和预热温度接近的模腔内，施加25-120MPa的压力，保压0.3-10分钟，热压在氧含量小于200PPM的惰性气体保护中进行；自然冷却或强制冷却到室温。
9.根据权利要求1所述的一种热压成型制备稀土永磁体的方法，其特征在于，步骤6）中热压膜具的断面尺寸，根据预热后生坯收缩后的尺寸加0.05-0.2mm，以便于入模。
10.根据权利要求1所述的一种热压成型制备稀土永磁体的方法，其特征在于，热压成型后的产品，进行时效处理，时效温度450-950℃。
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