CN112768167A - 一种钕铁硼永磁体的制备方法 - Google Patents
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- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 60
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 43
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 37
- 239000001257 hydrogen Substances 0.000 claims abstract description 26
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 25
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910000640 Fe alloy Inorganic materials 0.000 claims abstract description 18
- 229910000583 Nd alloy Inorganic materials 0.000 claims abstract description 18
- RKLPWYXSIBFAJB-UHFFFAOYSA-N [Nd].[Pr] Chemical compound [Nd].[Pr] RKLPWYXSIBFAJB-UHFFFAOYSA-N 0.000 claims abstract description 18
- RDTHZIGZLQSTAG-UHFFFAOYSA-N dysprosium iron Chemical compound [Fe].[Dy] RDTHZIGZLQSTAG-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000003723 Smelting Methods 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 238000005245 sintering Methods 0.000 claims description 20
- 239000002245 particle Substances 0.000 claims description 18
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 12
- 239000001301 oxygen Substances 0.000 claims description 12
- 229910052760 oxygen Inorganic materials 0.000 claims description 12
- 238000007792 addition Methods 0.000 claims description 8
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- 238000002156 mixing Methods 0.000 claims description 7
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- 229910052779 Neodymium Inorganic materials 0.000 claims description 5
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- 239000007788 liquid Substances 0.000 claims description 5
- 150000002431 hydrogen Chemical class 0.000 claims description 3
- 238000010902 jet-milling Methods 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 239000011812 mixed powder Substances 0.000 claims description 2
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- 238000009776 industrial production Methods 0.000 abstract description 4
- 238000001035 drying Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 238000005266 casting Methods 0.000 description 6
- 239000006247 magnetic powder Substances 0.000 description 6
- 238000010008 shearing Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 4
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- 241001062472 Stokellia anisodon Species 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
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- 229910052802 copper Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 229910052733 gallium Inorganic materials 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 229910052758 niobium Inorganic materials 0.000 description 3
- 239000000047 product Substances 0.000 description 3
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- 239000007858 starting material Substances 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 229910052726 zirconium Inorganic materials 0.000 description 3
- 229910052692 Dysprosium Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
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- 239000002002 slurry Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
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Abstract
本发明属于稀土永磁体技术领域，涉及一种钕铁硼永磁体的制备方法。本发明通过在钕铁硼氢破粉中添加氢破的镨钕合金、镝铁合金稀土合金粉的制备工艺，大大提高了成品的矫顽力；通过氢破稀土的添加方式，不仅可以根据钕铁硼原料中各成分含量的需求进行后续添加的调整，而且解决了熔炼过程中稀土元素含量过高的现象，从而降低了工业生产的成本。
Description
技术领域
本发明属于稀土永磁体技术领域，涉及一种钕铁硼永磁体的制备方法。
背景技术
钕铁硼磁体的制备工艺一般为通过在钕铁硼中添加重稀土，再经过熔炼、制粉、成型、烧结制的最终成品。为了提高钕铁硼的矫顽力，现有技术中一般采用两种方法：
一、在熔炼时添加一定比例的重稀土元素，但是熔炼后配方即已确定，重稀土元素会一部分分布到组合晶粒，往往使得重稀土元素含量过高，而且在后续工艺中不能控制，使得最终在工业生产中成品钕铁硼成本提高。
二、在母合金制成粉末后，通过添加稀土氧化物的方式。如中国专利申请文件(公开号：CN101812606A)公开了一种铸锭改铸片添加重稀土氧化物制备低成本钕铁硼的方法，其通过浆制备好的铸片氢破后，添加重稀土氧化物，将两种粉体搅拌经气流磨制粉，最后经压制成型、烧结等工艺制得成品，虽然在一定程度上降低了制造成本，但是最终产品的性能还需要得到更好地提升。
发明内容
本发明的目的是针对现有技术存在的上述问题，提出了一种节约成本、提高钕铁硼磁体性能的制备方法。
本发明的目的可通过下列技术方案来实现：一种钕铁硼永磁体的制备方法，所述方法包括如下步骤：先将钕铁硼原料熔炼为金属液，通过速凝工艺制成甩带片，再将甩带片氢破成粗粉，在粗粉中添加氢破稀土粉均匀混合，经气流磨制粉后再压制成型制成生坯，将生坯进行烧结，即得到钕铁硼永磁体。
在上述的一种钕铁硼永磁体的制备方法，所述均匀混合后氢破稀土粉的含量占粉料总重量的0.5-2.5％。氢破稀土粉的添加如果过多，会降低稀土粉增强钕铁永磁体的效能，而且生产成本会大幅上升。
作为优选，所述均匀混合后氢破稀土粉的含量占粉料总重量的0.5-1％。
在上述的一种钕铁硼永磁体的制备方法，所述氢破稀土粉为镨钕合金或镝铁合金中的一种或两种经氢破工艺制成。将镨钕合金、镝铁合金以氢破粉的形式添加，不仅可以根据原料中成分含量进行调整，而且可以解决在熔炼过程中添加导致含量过高的现象，这种通过将原料中一部分稀土合金通过氢破稀土粉的添加形式提高矫顽力的能力远远高于在熔炼阶段直接添加的方式，因为氢破稀土粉中的镨元素和镝会沿着晶界向主相钕铁硼扩散，并在晶粒表面形成硬磁化层，提升了磁体内禀矫顽力，优化了磁体的微观结构，使最终钕铁硼永磁体的物理性能大幅提高。
在上述的一种钕铁硼永磁体的制备方法，所述所述镨钕合金成分质量百分比为Pr：20％-25.0％、Nd：75-80％；镝铁合金的成分为Dy：79-81.0％、Fe：19-21％。
在上述的一种钕铁硼永磁体的制备方法，所述所述甩带片氢破后粒径为1-3mm；氧含量为＜800ppm。
在上述的一种钕铁硼永磁体的制备方法，所述氢破稀土粉的粒径为1-2mm；氧含量为＜600ppm。
在上述的一种钕铁硼永磁体的制备方法，所述气流磨后的混合粉料粒径为2.9-3.3μm；氧含量为＜1000ppm。
钕铁硼的颗粒越细，越有助于磁体内禀矫顽力的提升，但是粉料越细，越容易被氧化，当粒径为2.9-3.3μm时，永磁体的内禀矫顽力得到大幅提升，而且这时氢破稀土粉能在后续工艺中充分融入晶界，因为稀土合金粉的熔点低，烧结过程中先融化，沿着晶粒间的空隙流动，分布在晶界位置，在一定程度上抑制了钕铁硼晶粒的长大，磁体的密度增加，使得制备的钕铁硼永磁体达到最佳物理性能。
与现有技术相比，本发明具有以下有益效果：本发明通过在钕铁硼氢破粉中添加氢破的镨钕合金、镝铁合金稀土合金粉的制备工艺，大大提高了成品的矫顽力；通过氢破稀土的添加方式，不仅可以根据钕铁硼原料中各成分含量的需求进行后续添加的调整，而且解决了熔炼过程中稀土元素含量过高的现象，从而降低了工业生产的成本。
具体实施方式
以下是本发明的具体实施例，对本发明的技术方案作进一步的描述，但本发明并不限于这些实施例。
实施例1：
配比原料28.0wt％PrNd、2.0wt％DyFe、0.97wt％B、0.75wt％Al、0.2wt％Cu、1.2wt％Co、0.2wt％Nb、0.2wt％Ga、0.06wt％Zr、余量为Fe和不可避免的杂质，将上述原料装入速凝炉坩埚中熔炼，将速凝炉抽真空至5Pa以下，开始烘料，烘料功率设为130KW；烘料达25分钟左右，当真空度低于1Pa时，充氩气至-0.065Mpa，然后将功率升高至510KW，开始熔炼；铁棒完全沉没后，调整熔炼功率为420KW，对钢液进行精炼，精炼时间约为15分钟；待合金液面一旦转为银白色，开始测温，当温度达到规定浇铸温度1485℃时，开始浇铸，得到甩带片。
将甩带片放入氢碎炉中吸氢至饱和，然后加热至550℃脱氢至20Pa以下，得到粒径为1-3mm的粗粉、氧含量为＜800ppm。
在粗粉中添加1％的粒径为1.0-2.0mm、氧含量为＜600ppm的氢破稀土粉；氢破稀土粉为镨钕合金、镝铁合金经剪切机剪切成1.0-6.0cm的粉末，通过氢破工艺制得；其中镨钕合金、镝铁合金两者质量比为1:1，镨钕合金成分质量百分比为Pr：23.0％、Nd：77.0％；镝铁合金的成分为DY：80.0％、Fe：20.0％。将两种粉料均匀混合，经气流磨制得粒径为2.9μm的磁粉，再压制成型制成生坯，放入真空烧结炉内烧结，在1050℃的烧结温度下烧结4h后，从烧结炉中取出，即制成钕铁硼磁体，即得到钕铁硼永磁体。
实施例2
按照配比将原料(28.5wt％PrNd、2.1wt％DyFe、0.97wt％B、0.75wt％Al、0.2wt％Cu、1.2wt％Co、0.2wt％Nb、0.2wt％Ga、0.06wt％Zr、余量为Fe和不可避免的杂质)装入速凝炉坩埚中熔炼，将速凝炉抽真空至5Pa以下，开始烘料，烘料功率设为130KW；烘料达25分钟左右，当真空度低于1Pa时，充氩气至-0.065Mpa，然后将功率升高至510KW，开始熔炼；铁棒完全沉没后，调整熔炼功率为420KW，对钢液进行精炼，精炼时间约为15分钟；待合金液面一旦转为银白色，开始测温，当温度达到规定浇铸温度1485℃时，开始浇铸，得到甩带片。
将甩带片放入氢碎炉中吸氢至饱和，然后加热至550℃脱氢至20Pa以下，得到粒径为1-3mm的粗粉，氧含量为＜800ppm。
在粗粉中添加0.5％的粒径为1.0-3mm、氧含量为＜600ppm的氢破稀土粉；氢破稀土粉为镨钕合金、镝铁合金经剪切机剪切成1.0-6.0cm的粉末，再通过氢破工艺制得；其中镨钕合金、镝铁合金两者质量比为1:1，镨钕合金成分质量百分比为Pr：20％、Nd：80％；镝铁合金的成分为DY：79％、Fe：21％。将两种粉料均匀混合，经气流磨制得粒径为3.3μm的磁粉，再压制成型制成生坯，放入真空烧结炉内烧结，在1050℃的烧结温度下烧结4h后，从烧结炉中取出，即制成钕铁硼磁体，即得到钕铁硼永磁体。
实施例3：
配比原料27.5wt％PrNd、1.8wt％DyFe、0.97wt％B、0.75wt％Al、0.2wt％Cu、1.2wt％Co、0.2wt％Nb、0.2wt％Ga、0.06wt％Zr、余量为Fe和不可避免的杂质，将上述原料装入速凝炉坩埚中熔炼，将速凝炉抽真空至5Pa以下，开始烘料，烘料功率设为130KW；烘料达25分钟左右，当真空度低于1Pa时，充氩气至-0.065Mpa，然后将功率升高至510KW，开始熔炼；铁棒完全沉没后，调整熔炼功率为420KW，对钢液进行精炼，精炼时间约为15分钟；待合金液面一旦转为银白色，开始测温，当温度达到规定浇铸温度1485℃时，开始浇铸，得到甩带片。
将甩带片放入氢碎炉中吸氢至饱和，然后加热至550℃脱氢至20Pa以下，得到粒径为1-3mm的粗粉、氧含量为＜800ppm。
在粗粉中添加2.5％的粒径为1.0-2.0mm、氧含量为＜600ppm的氢破稀土粉；氢破稀土粉为镨钕合金、镝铁合金经剪切机剪切成1.0-6.0cm的粉末，通过氢破工艺制得；其中镨钕合金、镝铁合金两者质量比为1:1，镨钕合金成分质量百分比为Pr：23.0％、Nd：77.0％；镝铁合金的成分为DY：80.0％、Fe：20.0％。将两种粉料均匀混合，经气流磨制得粒径为2.9μm的磁粉，再压制成型制成生坯，放入真空烧结炉内烧结，在1050℃的烧结温度下烧结4h后，从烧结炉中取出，即制成钕铁硼磁体，即得到钕铁硼永磁体。
实施例4：
与实施例1的区别，仅在于，氢破稀土粉仅为1％的粒径1.0-3mm的镨钕合金。
实施例5：
与实施例1的区别，仅在于，氢破稀土粉仅为1％的粒径小于3mm的镝铁合金。
对比例1：
与实施例1的区别，仅在于，甩带片氢破后不添加氢破稀土粉。
对比例2：
与实施例1的区别，仅在于，甩带片氢破后添加重稀土氧化物，重稀土氧化物为2.75wt％的Dy203和2wt％的Ho2O3。
将本发明实施例1-3、对比例1-4中制得的的性能进行比较，比较结果如表1所示。
表1：实施例1-5、对比例1制得的钕铁硼永磁体性能的比较
综上所述，本发明通过在钕铁硼氢破粉中添加氢破的镨钕合金、镝铁合金稀土合金粉的制备工艺，大大提高了钕铁硼永磁体的性能，因为是通过氢破稀土的添加方式，不仅可以根据磁体稀土含量和矫顽力的需求调整，而且解决了稀土元素含量过高的现象，从而降低了工业生产的成本。
本处实施例对本发明要求保护的技术范围中点值未穷尽之处以及在实施例技术方案中对单个或者多个技术特征的同等替换所形成的新的技术方案，同样都在本发明要求保护的范围内；同时本发明方案所有列举或者未列举的实施例中，在同一实施例中的各个参数仅仅表示其技术方案的一个实例(即一种可行性方案)，而各个参数之间并不存在严格的配合与限定关系，其中各参数在不违背公理以及本发明述求时可以相互替换，特别声明的除外。
本发明方案所公开的技术手段不仅限于上述技术手段所公开的技术手段，还包括由以上技术特征任意组合所组成的技术方案。以上所述是本发明的具体实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也视为本发明的保护范围。
本文中所描述的具体实施例仅仅是对本发明精神作举例说明。本发明所属技术领域的技术人员可以对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代，但并不会偏离本发明的精神或者超越所附权利要求书所定义的范围。
Claims (7)
1.一种钕铁硼永磁体的制备方法，其特征在于，所述方法包括如下步骤：先将钕铁硼原料熔炼为金属液，通过速凝工艺制成甩带片，再将甩带片氢破成粗粉，在粗粉中添加氢破稀土粉均匀混合，经气流磨制粉后再压制成型制成生坯，将生坯进行烧结，即得到钕铁硼永磁体。
2.根据权利要求1所述的一种钕铁硼永磁体的制备方法，其特征在于，所述氢破稀土粉的添加量为粗粉的0.5-2.5％。
3.根据权利要求1所述的一种钕铁硼永磁体的制备方法，其特征在于，所述氢破稀土粉为镨钕合金或镝铁合金中的一种或两种经氢破工艺制成。
4.根据权利要求3所述的一种钕铁硼永磁体的制备方法，其特征在于，所述镨钕合金成分质量百分比为Pr：20％-25.0％、Nd：75-80％；镝铁合金的成分为Dy：79-81.0％、Fe：19-21％。
5.根据权利要求1所述的一种钕铁硼永磁体的制备方法，其特征在于，所述甩带片氢破后粒径为1-3mm；氧含量为＜800ppm。
6.根据权利要求1所述的一种钕铁硼永磁体的制备方法，其特征在于，所述氢破稀土粉的粒径为1-2mm；氧含量为＜600ppm。
7.根据权利要求1所述的一种钕铁硼永磁体的制备方法，其特征在于，所述气流磨后的混合粉料粒径为2.9-3.3μm；氧含量为＜1000ppm。
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| CN103065787A (zh) * | 2012-12-26 | 2013-04-24 | 宁波韵升股份有限公司 | 一种制备烧结钕铁硼磁体的方法 |
| CN103824668A (zh) * | 2014-01-17 | 2014-05-28 | 浙江东阳东磁有限公司 | 一种低重稀土高矫顽力烧结钕铁硼磁体及其制备方法 |
| CN104064346A (zh) * | 2014-05-30 | 2014-09-24 | 宁波同创强磁材料有限公司 | 一种钕铁硼磁体及其制备方法 |
| CN108074693A (zh) * | 2016-11-16 | 2018-05-25 | 中国科学院宁波材料技术与工程研究所 | 一种钕铁硼永磁材料及其制备方法 |
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| CN103065787A (zh) * | 2012-12-26 | 2013-04-24 | 宁波韵升股份有限公司 | 一种制备烧结钕铁硼磁体的方法 |
| CN103824668A (zh) * | 2014-01-17 | 2014-05-28 | 浙江东阳东磁有限公司 | 一种低重稀土高矫顽力烧结钕铁硼磁体及其制备方法 |
| CN104064346A (zh) * | 2014-05-30 | 2014-09-24 | 宁波同创强磁材料有限公司 | 一种钕铁硼磁体及其制备方法 |
| CN108074693A (zh) * | 2016-11-16 | 2018-05-25 | 中国科学院宁波材料技术与工程研究所 | 一种钕铁硼永磁材料及其制备方法 |
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