CN106098282A - 一种降低镝含量的磁体制备方法 - Google Patents

一种降低镝含量的磁体制备方法 Download PDF

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CN106098282A
CN106098282A CN201610396463.3A CN201610396463A CN106098282A CN 106098282 A CN106098282 A CN 106098282A CN 201610396463 A CN201610396463 A CN 201610396463A CN 106098282 A CN106098282 A CN 106098282A
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肖震
韩珩
钟炳文
解伟
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Longyan Cercis Innovation Research Institute
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    • H01F41/00—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
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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
    • H01F41/0293—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 diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
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    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • 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
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • 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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    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • 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
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • 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
    • H01F1/0575—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 pressed, sintered or bonded together
    • H01F1/0577—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 pressed, sintered or bonded together sintered
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—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
    • H01F41/02—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
    • 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

本发明公开一种降低镝含量的磁体制备方法，先制备钕铁硼铸片，再制备成微米级的钕铁硼粉体；再将获得的粉末压制成型；然后经过压型后，利用热喷涂设备在压坯表面喷涂一层金属镝，镝的用量为2‑3%；调整热喷涂的喷嘴压力、喷涂距离、喷涂行走速度使涂层厚度达到50‑150µm；最后经过热喷涂涂层后的压坯放入管式烧结炉中进行烧结，冷却，温度达到室温时取出烧结磁体。本发明在保证矫顽力的同时降低了Dy元素的添加量，与目前工艺相比，镝含量降低了2%。磁体可应用于微特电机、磁传感器等领域。

Description

一种降低镝含量的磁体制备方法
技术领域
本发明涉及到稀土永磁合金，特别是钕铁硼的烧结磁体，尤指一种降低镝含量的磁体制备方法。
背景技术
被誉为磁王的烧结钕铁硼永磁材料的应用范围和市场前景十分广阔，且逐渐向高技术领域转移，如应用于制造几百kw的电动汽车的发电机和电动机，以及制造MW量级的风力发电永磁电机。近年来我国钕铁硼制造技术进步明显，永磁设备不断发展与改进，新技术得到采用，产品档次迅速提高。国内部分企业已可制造UH、EH、VH和AH的高矫顽力烧结钕铁硼，但提高矫顽力过度依赖Dy和Tb。在钕铁硼永磁材料中加入镝元素，用镝取代部分钕元素，细化了晶粒，能有效地提高该磁体的内禀矫顽力。并且随着镝含量的增加，矫顽力不断增加，磁通不可逆损失减小，热稳定性得到改善。但Dy和Tb元素属于重稀土元素，储量低，价格高，过多的添加Dy元素不利于成本的降低。
尽管通过细化晶粒和改善边界结构都可以提高烧结钕铁硼磁体的矫顽力，但用Dy和Tb等重稀土元素部分置换磁体中的Nd是一种显著有效的方法。
发明内容
本发明的目的在于提供一种降低镝含量的磁体制备方法，降低了Dy元素的使用量，在矫顽力没有降低的同时降低了成本。
为了达成上述目的，本发明的解决方案是：
一种降低镝含量的磁体制备方法，其步骤是：
第一步，制备钕铁硼铸片，再制备成微米级的钕铁硼粉体；
第二步，将获得的粉末压制成型；
第三步，经过压型后，利用热喷涂设备在压坯表面喷涂一层金属镝，镝的用量为2-3%；调整热喷涂的喷嘴压力、喷涂距离、喷涂行走速度使涂层厚度达到50-150µm；
第四步，经过热喷涂涂层后的压坯放入管式烧结炉中进行烧结，烧结工艺为：在真空度达到10-3Pa时开始升温，升至400-800℃保温3-7小时，然后在950-1100℃保温5-10小时，然后随炉冷却，温度达到室温时取出烧结磁体。
所述第一步，通过真空感应熔炼炉制备钕铁硼铸片，原料中成分：Nd30.3%、Pr0.1%、Co4%、Ga0.46%、B0.92%，余量为Fe，熔炼炉内真空度达到10-3Pa时充入氩气到2000Pa，熔炼后浇注在铜辊中进行甩带获得铸片，甩带速度30m/s；再通过气流磨制备成微米级的钕铁硼粉体，气流磨喷嘴空气压力0.5MP，分级轮转速为3000rpm，气流磨后获得钕铁硼粉体粒度20-60µm。
所述第二步，将获得的粉末放入磁场压机模腔中，在磁场中取向压制成型，压坯密度达到4.5g/cm3，将取向压型后的压坯放入等静压机中继续压型，增加压坯密度，达到6.5/cm3。
所述第三步，热喷涂的喷嘴压力1-1.5MP、喷涂距离10cm，喷涂行走速度0.8-1cm/s。
采用上述方案后，本发明通过热喷涂的方式在磁体表面附着一层Dy金属粉末，热处理过程中，Dy随液态富钕相沿晶界分布，而后扩散进入晶粒表层取代Nd元素，在晶粒边界形成富Dy的薄壳层，主相晶粒内部成分不变。因为(Nd，Dy)2Fe14B相的各向异性场比Nd2Fe14B的高很多，所以矫顽力显著提高。被置换出来的Nd进入晶界，弥补富Nd相的不足，形成连续的晶界相，增强去耦合作用。本发明的有益效果是在保证了磁体矫顽力的同时降低了Dy元素的添加量，与目前工艺相比，镝含量降低了2%。
本发明制成的磁体可应用于微特电机、磁传感器等领域。
具体实施方式
实例1
第一步，通过真空感应熔炼炉制备钕铁硼铸片，原料中成分：Nd30.3%、Pr0.1%、Co4%、Ga0.46%、B0.92%，余量为Fe，熔炼炉内真空度达到10-3Pa时充入氩气到2000Pa，熔炼后浇注在铜辊中进行甩带获得铸片，甩带速度30m/s；再通过气流磨制备成微米级的钕铁硼粉体，气流磨喷嘴空气压力0.5MP，分级轮转速为3000rpm，气流磨后获得钕铁硼粉体粒度20-60µm；
第二步，将获得的粉末放入磁场压机模腔中，在磁场中取向压制成型，压坯密度达到4.5g/cm3，将取向压型后的压坯放入等静压机中继续压型，增加压坯密度，达到6.5/cm3；
第三步，经过等静压机压型后，利用热喷涂设备在压坯表面喷涂一层金属镝，镝的用量为2%，调整热喷涂的喷嘴压力1MP、喷涂距离10cm，喷涂行走速度1cm/s。涂层厚度达到100µm；
第四步，经过热喷涂涂层后的压坯放入管式烧结炉中进行烧结，烧结工艺为：在真空度达到10-3Pa时开始升温，升至500℃保温6小时，然后在1000℃保温7小时，然后随炉冷却，温度达到室温时取出烧结磁体。磁体矫顽力10.7KOe。
实例2
第一步，通过真空感应熔炼炉制备钕铁硼铸片，原料中成分：Nd30.3%、Pr0.1%、Co4%、Ga0.46%、B0.92%，余量为Fe，熔炼炉内真空度达到10-3Pa时充入氩气到2000Pa，熔炼后浇注在铜辊中进行甩带获得铸片，甩带速度30m/s；再通过气流磨制备成微米级的钕铁硼粉体，气流磨喷嘴空气压力0.5MP，分级轮转速为3000rpm，气流磨后获得钕铁硼粉体粒度20-60µm；
第二步，将获得的粉末放入磁场压机模腔中，在磁场中取向压制成型，压坯密度达到4.5g/cm3，将取向压型后的压坯放入等静压机中继续压型，增加压坯密度，达到6.5/cm3；
第三步，经过等静压机压型后，利用热喷涂设备在压坯表面喷涂一层金属镝，镝的用量为2.6%，调整热喷涂的喷嘴压力1.5MP、喷涂距离10cm，喷涂行走速度0.8cm/s。涂层厚度达到140µm；
第四步，经过热喷涂涂层后的压坯放入管式烧结炉中进行烧结，烧结工艺为：在真空度达到10-3Pa时开始升温，升至600℃保温6小时，然后在1100℃保温8小时，然后随炉冷却，温度达到室温时取出烧结磁体。磁体矫顽力11.6KOe。

Claims (4)

1.一种降低镝含量的磁体制备方法，其特征在于步骤是：
第一步，制备钕铁硼铸片，再制备成微米级的钕铁硼粉体；
第二步，将获得的粉末压制成型；
第三步，经过压型后，利用热喷涂设备在压坯表面喷涂一层金属镝，镝的用量为2-3%；调整热喷涂的喷嘴压力、喷涂距离、喷涂行走速度使涂层厚度达到50-150µm；
第四步，经过热喷涂涂层后的压坯放入管式烧结炉中进行烧结，烧结工艺为：在真空度达到10-3Pa时开始升温，升至400-800℃保温3-7小时，然后在950-1100℃保温5-10小时，然后随炉冷却，温度达到室温时取出烧结磁体。
2.根据权利要求1所述的一种降低镝含量的磁体制备方法，其特征在于：所述第一步，通过真空感应熔炼炉制备钕铁硼铸片，原料中成分：Nd30.3%、Pr0.1%、Co4%、Ga0.46%、B0.92%，余量为Fe，熔炼炉内真空度达到10-3Pa时充入氩气到2000Pa，熔炼后浇注在铜辊中进行甩带获得铸片，甩带速度30m/s；再通过气流磨制备成微米级的钕铁硼粉体，气流磨喷嘴空气压力0.5MP，分级轮转速为3000rpm，气流磨后获得钕铁硼粉体粒度20-60µm。
3.根据权利要求1所述的一种降低镝含量的磁体制备方法，其特征在于：所述第二步，将获得的粉末放入磁场压机模腔中，在磁场中取向压制成型，压坯密度达到4.5g/cm3，将取向压型后的压坯放入等静压机中继续压型，增加压坯密度，达到6.5/cm3。
4.根据权利要求1所述的一种降低镝含量的磁体制备方法，其特征在于：所述第三步，热喷涂的喷嘴压力1-1.5MP、喷涂距离10cm，喷涂行走速度0.8-1cm/s。
CN201610396463.3A 2016-06-07 2016-06-07 一种降低镝含量的磁体制备方法 Expired - Fee Related CN106098282B (zh)

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CN108922768A (zh) * 2018-07-18 2018-11-30 浙江中科磁业有限公司 一种高压热处理晶界扩散增强钕铁硼磁体矫顽力的方法
CN111554502A (zh) * 2020-04-29 2020-08-18 南京理工大学 增压扩散热处理制备高矫顽力烧结钕铁硼的方法

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CN103258633A (zh) * 2013-05-30 2013-08-21 烟台正海磁性材料股份有限公司 一种R-Fe-B系烧结磁体的制备方法
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JPH05105904A (ja) * 1992-03-13 1993-04-27 Sumitomo Special Metals Co Ltd ボンド磁石用合金粉末の製造方法
CN103903823A (zh) * 2012-12-26 2014-07-02 宁波金鸡强磁股份有限公司 一种稀土永磁材料及其制备方法
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108922768A (zh) * 2018-07-18 2018-11-30 浙江中科磁业有限公司 一种高压热处理晶界扩散增强钕铁硼磁体矫顽力的方法
CN108922768B (zh) * 2018-07-18 2020-10-09 浙江中科磁业股份有限公司 一种高压热处理晶界扩散增强钕铁硼磁体矫顽力的方法
CN111554502A (zh) * 2020-04-29 2020-08-18 南京理工大学 增压扩散热处理制备高矫顽力烧结钕铁硼的方法

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