CN112802679A - 一种无重稀土烧结钕铁硼磁体的制备方法 - Google Patents

一种无重稀土烧结钕铁硼磁体的制备方法 Download PDF

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CN112802679A
CN112802679A CN202011641802.2A CN202011641802A CN112802679A CN 112802679 A CN112802679 A CN 112802679A CN 202011641802 A CN202011641802 A CN 202011641802A CN 112802679 A CN112802679 A CN 112802679A
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neodymium
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张洪伟
郭一方
胡小杰
吴小洁
倪浩瀚
曲喜嘉
陈伟
杨荣
倪朝盛
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Ningbo Songke Magnetic Material Co ltd
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    • 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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    • 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
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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
    • H01F1/0576—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 pressed, e.g. hot working
    • H—ELECTRICITY
    • 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

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Abstract

本申请公开了本发明公开了一种无重稀土烧结钕铁硼磁体的制备方法。属于烧结钕铁硼磁体制备技术领域，该方法能够在不添加任何重稀土元素的条件下，稳定生产出无重稀土超高性能的烧结钕铁硼磁体。所述方法包括如下步骤：一：配制钕铁硼合金，其中镨钕比例低于29.2％；二：通过熔炼炉制备速凝片；三：熔炼氢破后，粗粉先球磨，再粗粉加剂搅拌，后研磨成细粉，然后细粉加剂搅拌；四：在磁场取向条件下进行成型压制，随后再通过等静压进一步使磁体密实；五：使用烧结炉低温烧结，烧结后保温；六：待冷却后，进行一级时效回火处理和二级时效回火处理。

Description

一种无重稀土烧结钕铁硼磁体的制备方法
技术领域
本发明涉及烧结钕铁硼磁体制备技术领域，尤其是一种无重稀土烧结钕铁硼磁体的制备方法。
背景技术
随着新能源汽车、风力发电等新兴产业的快速发展，大幅度拉升了对耐高温烧结钕铁硼的市场需求，为了提高钕铁硼材料的使用温度，市场上目前基本上采用晶界扩散的方式来添加重稀土元素，以制备出超高剩磁超高矫顽力钕铁硼磁钢，那对基材(无重稀土、超高剩磁)的要求就会越来越严格。
现有技术一般采用常规的熔炼、制粉、成型、烧结等生产工艺，熔炼过程稀土含量(主要是镨钕)挥发严重；晶粒细化后，高温烧结出来的坯料晶界分布不均匀，造成产品性能一致性不好，方形度差。
发明内容
本发明是为了解决现有无重稀土烧结钕铁硼磁体存在上述不足，提供一种能够在不添加任何重稀土元素的条件下，稳定生产出无重稀土超高性能的烧结钕铁硼磁体的一种无重稀土烧结钕铁硼磁体的制备方法。
以上技术问题是通过下列技术方案解决的：
一种无重稀土烧结钕铁硼磁体的制备方法，所述方法包括如下步骤：
一：配制钕铁硼合金，其中镨钕比例需要低于29.2％；
二：通过熔炼炉制备速凝片，首先在熔炼装炉先铺一层铁棒在坩埚底部，其次加小料，然后将所有剩余铁棒放入，之后将镨钕放入待加料区；通过抽真空熔炼，当坩埚内材料全部融化后，进行二次加料，将待加料区的镨钕放入坩埚内，待镨钕快速融化后先一次控温，达到熔炼温度后保温，之后进行二次控温，最后开始浇注、冷却、出炉；
三：熔炼氢破后，粗粉先球磨，再粗粉加剂搅拌，后研磨成细粉，然后细粉加剂搅拌；
四：在磁场取向条件下进行成型压制，随后再通过等静压进一步使磁体密实；
五：使用烧结炉低温烧结，烧结后保温；
六：待冷却后，进行一级时效回火处理和二级时效回火处理。
作为本发明进一步的方案：步骤二中一次控温的熔炼温度为1455±10℃。
作为本发明进一步的方案：步骤二中二次控温的熔炼温度为1400±10℃。
作为本发明进一步的方案：步骤三中球磨时间为15±5min，细粉的粒径为2.5±0.5μm。
作为本发明进一步的方案：步骤四中取向磁场为2.0-3.0T。
作为本发明进一步的方案：步骤五中烧结保温的时间为15±5h。
本发明能够达到如下效果：
本发明提供了一种无重稀土烧结钕铁硼磁体的制备方法，与现有技术相比，本发明的有益效果是：能够在不添加任何重稀土元素的条件下，稳定生产出无重稀土超高性能的烧结钕铁硼磁体。
具体实施方式
下面将结合本发明实施例，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例，一种无重稀土烧结钕铁硼磁体的制备方法，所述方法包括如下步骤：一：配制钕铁硼合金，其中镨钕比例28.8％，硼比例0.88％，微量元素1.1％，余Fe；二：通过熔炼炉制备速凝片，首先在熔炼装炉先铺一层铁棒在坩埚底部，其次加小料，然后将所有剩余铁棒放入，之后将镨钕放入待加料区；通过抽真空熔炼，当坩埚内材料全部融化后，进行二次加料，将待加料区的镨钕放入坩埚内，待镨钕快速融化后先一次控温，达到熔炼温度后保温，之后进行二次控温，最后开始浇注、冷却、出炉；三：粗粉加剂搅拌，后研磨成细粉，然后细粉加剂搅拌；四：在磁场取向条件下进行成型压制，随后再通过等静压进一步使磁体密实；五：使用烧结炉低温烧结，烧结后保温；六：待冷却后，进行一级时效回火处理和二级时效回火处理。
本实施例中步骤二中一次控温的熔炼温度为1455±10℃。步骤二中二次控温的熔炼温度为1400±10℃。步骤三中球磨时间为15±5min，细粉的粒径为2.5±0.5μm。步骤四中取向磁场为2.0-3.0T。步骤五中烧结保温的时间为15±5h。
本实施例的优点：1、熔炼进行二次加料，减少稀土镨钕的熔炼时间，稀土元素快速融化，减少稀土在熔炼过程中的损耗；2、熔炼温度达到后，迅速将加热功率调制零，保温一定时间进行精练，确保合金钢液混合均匀，同时精练过程中将氧化层析出后浇注，进一步保证铸片纯度；3、氢破后粗粉采用球磨后制粉的工艺，先球磨可以保证粗粉颗粒更加圆润，棱角更少，使制粉后颗粒更接近类球形，更能保证粉料的一致性和稳定性；4、低温烧结，烧结保温时间一般15±3h，在磁体密度达到的情况下抑制晶粒长大，使磁体晶粒分布更均匀，将晶粒细化做到极致。
对比例：使用相同配方按照常规的熔炼、制粉、成型、烧结的生产制造工艺来制备坯料。
实施例及对比例中可获得的钕铁硼工件性能如下：
序号 类型 Br Hcb Hcj (BH)<sub>max</sub> Hk Hk/Hcj
1 对比例 15.00 9.505 9.702 53.63 9.207 0.949
2 实施例 15.04 12.84 13.11 56.06 12.79 0.975
本发明提供了一种无重稀土烧结钕铁硼磁体的制备方法，能够在不添加任何重稀土元素的条件下，稳定生产出无重稀土超高性能的烧结钕铁硼磁体。
以上所述仅为本发明的优选实施例，并非因此即限制本发明的专利保护范围，凡是运用本发明说明书内容所作的等效结构变换，直接或间接运用在其他相关的技术领域，均同理包括在本发明的保护范围内。对于本领域技术人员而言，显然本发明不限于上述示范性实施例的细节，而且在不背离本发明的精神或基本特征的情况下，能够以其他的具体形式实现本发明。因此，无论从哪一点来看，均应将实施例看作是示范性的，而且是非限制性的，本发明的范围由所附权利要求而不是上述说明限定，因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。
此外，应当理解，虽然本说明书按照实施方式加以描述，但并非每个实施方式仅包含一个独立的技术方案，说明书的这种叙述方式仅仅是为清楚起见，本领域技术人员应当将说明书作为一个整体，各实施例中的技术方案也可以经适当组合，形成本领域技术人员可以理解的其他实施方式。

Claims (6)

1.一种无重稀土烧结钕铁硼磁体的制备方法，其特征在于，所述方法包括如下步骤：
一：配制钕铁硼合金，其中镨钕比例低于29.2％；
二：通过熔炼炉制备速凝片，首先在熔炼装炉先铺一层铁棒在坩埚底部，其次加小料，然后将所有剩余铁棒放入，之后将镨钕放入待加料区；通过抽真空熔炼，当坩埚内材料全部融化后，进行二次加料，将待加料区的镨钕放入坩埚内，待镨钕快速融化后先一次测温，达到熔炼温度后保温，之后进行二次测温，最后开始浇注、冷却、出炉；
三：熔炼氢破后，粗粉先球磨，再粗粉加剂搅拌，后研磨成细粉，然后细粉加剂搅拌；
四：在磁场取向条件下进行成型压制，随后再通过等静压进一步使磁体密实；
五：使用烧结炉低温烧结，烧结后保温；
六：待冷却后，进行一级时效回火处理和二级时效回火处理。
2.根据权利要求1所述的一种无重稀土烧结钕铁硼磁体的制备方法，其特征在于，步骤二中一次控温的熔炼温度为1455±10℃。
3.根据权利要求1所述的一种无重稀土烧结钕铁硼磁体的制备方法，其特征在于，步骤二中二次控温的熔炼温度为1400±10℃。
4.根据权利要求1所述的一种无重稀土烧结钕铁硼磁体的制备方法，其特征在于，步骤三中球磨时间为15±5min，细粉的粒径为2.5±0.5μm。
5.根据权利要求1所述的一种无重稀土烧结钕铁硼磁体的制备方法，其特征在于，步骤四中取向磁场为2.0-3.0T。
6.根据权利要求1所述的一种无重稀土烧结钕铁硼磁体的制备方法，其特征在于，步骤五中烧结保温的时间为15±5h。
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