CN106816250B - 一种耐高温抗腐蚀永磁铁及其制备方法 - Google Patents

一种耐高温抗腐蚀永磁铁及其制备方法 Download PDF

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CN106816250B
CN106816250B CN201710134172.1A CN201710134172A CN106816250B CN 106816250 B CN106816250 B CN 106816250B CN 201710134172 A CN201710134172 A CN 201710134172A CN 106816250 B CN106816250 B CN 106816250B
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曹庆波
王遵跃
张展胜
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Anhui Dongfang Magnetic Magnet Manufacturing Co Ltd
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    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
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    • 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
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    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
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    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • 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
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    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
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    • 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
    • H01F41/0266—Moulding; Pressing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/248—Thermal after-treatment

Abstract

本发明提出了一种耐高温抗腐蚀钕铁硼永磁铁及其制备方法，耐高温抗腐蚀钕铁硼永磁铁由如下各组分重量百分比的原料制成：5％‑20％钕铁硼磁性粉末、12％‑20％Fe3O4、3％‑8％SiO2、4％‑8％硬脂酸、3％‑9％单晶氧化镁、1％‑5％碳酸钙粉、2％‑5％碳黑、1％‑4％苯甲酸钠、2％‑7％丙酸钙，余量为硼酸；该发明具体包括如下步骤：熔炼、制粉、压制、回火、磁性检测；本发明制得的钕铁硼磁铁具有磁性强、耐高温和抗腐蚀的优点，具备极大的推广价值。

Description

一种耐高温抗腐蚀永磁铁及其制备方法
技术领域
本发明涉及磁铁制备领域，具体涉及一种耐高温抗腐蚀永磁铁及其制备方法。
背景技术
钕铁硼磁铁可分为粘结钕铁硼磁铁和烧结钕铁硼磁铁两种。粘结实际上就是注塑成型，而烧结是抽真空通过高温加热成型。钕铁硼磁铁的优点是性价比高，在磁学界被誉为“磁王”，具良好的机械特性；不足之处在于居里温度点低，温度特性差，且易于粉化腐蚀。
在中国公开的专利申请CN102942357A中针对获得高剩余磁化强度和高内禀矫顽能力的钕铁硼磁铁，称取原料为碳酸钙粉末、碳酸锶粉末、碳酸钡粉末、氧化镧粉末以及三氧化二铁粉末来制备钕铁硼磁铁，在一定程度上提高了钕铁硼的磁性强度和矫顽力。在中国公开申请的CN103794354A中针对制备抗腐蚀和高矫顽力的钕铁硼磁铁，进行表面处理时，将磁铁放入氧化镍颗粒和液体石蜡的振动容器中处理，提高了钕铁硼磁铁的矫顽力和抗腐蚀能力，使得该磁铁更适合在潮湿恶劣的环境中使用。
目前现有技术虽能在一定程度上提高矫顽力和抗腐蚀能力，但碳酸钡是钡盐，有很强的毒性，碳酸钡会蓄积在骨骼上，引起骨髓造白细胞组织增生，从而发生慢性中毒。氧化镍粉末对人体健康有害，有致癌、致敏的风险，对水体环境产生长期影响。
发明内容
针对上述存在的问题，本发明提供了一种耐高温、抗腐蚀的永磁铁。本发明所用原料均无毒无害，对环境无污染。本发明提供的钕铁硼磁铁还具有韧性好、磁场稳定、高矫顽力等优点。
为了实现上述的目的，本发明采用以下的技术方案：
一种耐高温抗腐蚀永磁铁，由如下各组分重量百分比的原料制成：5％-20％钕铁硼磁性粉末、12％-20％Fe3O4、3％-8％SiO2、4％-8％硬脂酸、3％-9％单晶氧化镁、1％-5％碳酸钙粉、2％-5％碳黑、1％-4％苯甲酸钠、2％-7％丙酸钙，余量为铁。
优选地，由如下各组分重量百分比的原料制成：10％-20％钕铁硼磁性粉末、15％-20％Fe3O4、5％-8％SiO2、5％-8％硬脂酸、4％-9％单晶氧化镁、2％-5％碳酸钙粉、3％-5％碳黑、2％-4％苯甲酸钠、3％-7％丙酸钙，余量为铁。
上述的耐高温抗腐蚀永磁铁的制备方法，包括如下几个步骤：
(1)熔炼：按配比称取原料后，将钕铁硼粉末、Fe3O4、碳酸钙粉、苯甲酸钠、硬脂酸和铁放入熔炼炉中，升温至1500℃-1600℃，然后依次加入碳黑、丙酸钙、SiO2和单晶氧化镁，继续升温至所有原料融为液态，再调节温度为2750℃-2860℃，保持3-5h，得到永磁铁粗成品溶液；
(2)制粉：将永磁铁粗成品溶液冷却固化后得到固态粗成品永磁铁，送入管磨机连续研磨3-5h，得到粒径为0.5-1微米的永磁铁粉末；
(3)压制：将所得永磁铁粉末在氩气保护气的作用下放入磁场强度为20000-25000Gs的磁场中取向定型，再通过400MPa压力静压制成毛坯；
(4)回火：将上述毛坯放入800℃-900℃真空环境中一次回火，持续2-3h，再进调节温度为400℃-700℃进行二次回火，保持1-2h，得永磁铁；
(5)磁性检测：将所得永磁铁冷却至室温后放入磁性监测仪中检测其磁性。
优选地，所述步骤(1)中升温至1500℃-1600℃后，保温时间为1-2h。
优选地，步骤(2)中所述的管磨机转速为200-300r/min。
采用上述的技术方案，本发明的有益效果是：本发明添加的碳酸钙粉、碳黑和硬脂酸联合作用，具有一定的耐冲击能力，对酸、碱、油、水等介质具有良好的稳定性，从而增强了永磁铁的综合性能。本发明中添加SiO2，在研磨中使共晶团细化，珠光体数量增多，提高了永磁铁的硬度，增强了机械性能。本发明使用丙酸钙和苯甲酸钠联合作用，能够抑制微生物的繁殖，并且具备一定的耐酸碱腐蚀能力，提高了永磁铁的抗腐蚀性能。另外，添加的单晶氧化镁，具有良好的耐高温性和抗腐蚀性，大大提高了钕铁硼磁铁的耐高温和抗腐蚀性能。本发明采用合理的工艺方法、参数优化和工艺调控制得的永磁铁在机械性能和磁性能上均具有显著地改进。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚，下面将结合本发明，对本发明实施例中的技术方案进行清楚、完整地描述。基于本发明的实施例，本领域普通技术人员在没有作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1：
一种耐高温抗腐蚀永磁铁，由如下各组分重量百分比的原料制成；10％钕铁硼磁性粉末、16％Fe3O4、3％SiO2、4％硬脂酸、3％单晶氧化镁、1％碳酸钙粉、3％碳黑、2％苯甲酸钠、3％丙酸钙，余量为铁。
(1)熔炼：按配比称取原料后，将钕铁硼粉末、Fe3O4、碳酸钙粉、苯甲酸钠、硬脂酸和铁放入熔炼炉中，升温至1500℃，保温1h，然后依次加入碳黑、丙酸钙、SiO2和单晶氧化镁，继续升温至所有原料融为液态，再调节温度为2750℃，保持3h，得到永磁铁粗成品溶液；
(2)制粉：将永磁铁粗成品溶液冷却固化后得到固态粗成品永磁铁，送入管磨机连续研磨3h，得到粒径为0.5微米的永磁铁粉末；
(3)压制：将所得永磁铁粉末在氩气保护气的作用下放入磁场强度为20000Gs的磁场中取向定型，再通过400MPa压力静压制成毛坯；
(4)回火：将上述毛坯放入800℃真空环境中一次回火，持续2h，再调节温度为400℃进行二次回火，保持1.5h，得永磁铁；
(5)磁性检测：将所得永磁铁冷却至室温后放入磁性监测仪中检测其磁性。
实施例2：
一种耐高温抗腐蚀永磁铁，由如下各组分重量百分比的原料制成；12％钕铁硼磁性粉末、15％Fe3O4、4％SiO2、6％硬脂酸、4％单晶氧化镁、3％碳酸钙粉、4％碳黑、1％苯甲酸钠、2％丙酸钙，余量为铁。
(1)熔炼：按配比称取原料后，将钕铁硼粉末、Fe3O4、碳酸钙粉、苯甲酸钠、硬脂酸和铁放入熔炼炉中，升温至1510℃，保温1.5h，然后依次加入碳黑、丙酸钙、SiO2和单晶氧化镁，继续升温至所有原料融为液态，再调节温度为2760℃，保持3h，得到永磁铁粗成品溶液；
(2)制粉：将永磁铁粗成品溶液冷却固化后得到固态粗成品永磁铁，送入管磨机连续研磨3h，得到粒径为1微米的永磁铁粉末；
(3)压制：将所得永磁铁粉末在氩气保护气的作用下放入磁场强度为21000Gs的磁场中取向定型，再通过400MPa压力静压制成毛坯；
(4)回火：将上述毛坯放入820℃真空环境中一次回火，持续2.5h，再调节温度为450℃进行二次回火，保持1h，得永磁铁；
(5)磁性检测：将所得永磁铁冷却至室温后放入磁性监测仪中检测其磁性。
实施例3：
一种耐高温抗腐蚀永磁铁，由如下各组分重量百分比的原料制成；20％钕铁硼磁性粉末、20％Fe3O4、6％SiO2、8％硬脂酸、6％单晶氧化镁、4％碳酸钙粉、4％碳黑、3％苯甲酸钠、5％丙酸钙，余量为铁。
(1)熔炼：按配比称取原料后，将钕铁硼粉末、Fe3O4、碳酸钙粉、苯甲酸钠、硬脂酸和铁放入熔炼炉中，升温至1530℃，保温1.5h，然后依次加入碳黑、丙酸钙、SiO2和单晶氧化镁，继续升温至所有原料融为液态，再调节温度为2770℃，保持3.5h，得到永磁铁粗成品溶液；
(2)制粉：将永磁铁粗成品溶液冷却固化后得到固态粗成品永磁铁，送入管磨机连续研磨3.5h，得到粒径为0.7微米的永磁铁粉末；
(3)压制：将所得永磁铁粉末在氩气保护气的作用下放入磁场强度为22000Gs的磁场中取向定型，再通过400MPa压力静压制成毛坯；
(4)回火：将上述毛坯放入830℃真空环境中一次回火，持续3h，再调节温度为500℃进行二次回火，保持1h，得永磁铁；
(5)磁性检测：将所得永磁铁冷却至室温后放入磁性监测仪中检测其磁性。
实施例4：
一种耐高温抗腐蚀永磁铁，由如下各组分重量百分比的原料制成；18％钕铁硼磁性粉末、18％Fe3O4、7％SiO2、7％硬脂酸、9％单晶氧化镁、5％碳酸钙粉、5％碳黑、4％苯甲酸钠、7％丙酸钙，余量为铁。
(1)熔炼：按配比称取原料后，将钕铁硼粉末、Fe3O4、碳酸钙粉、苯甲酸钠、硬脂酸和铁放入熔炼炉中，升温至1600℃，保温2h，然后依次加入碳黑、丙酸钙、SiO2和单晶氧化镁，继续升温至所有原料融为液态，再调节温度为2860℃，保持5h，得到永磁铁粗成品溶液；
(2)制粉：将永磁铁粗成品溶液冷却固化后得到固态粗成品永磁铁，送入管磨机连续研磨4h，得到粒径为0.6微米的永磁铁粉末；
(3)压制：将所得永磁铁粉末在氩气保护气的作用下放入磁场强度为25000Gs的磁场中取向定型，再通过400MPa压力静压制成毛坯；
(4)回火：将上述毛坯放入890℃真空环境中一次回火，持续2h，再调节温度为650℃进行二次回火，保持2h，得永磁铁；
(5)磁性检测：将所得永磁铁铁冷却至室温后放入磁性监测仪中检测其磁性。
实施例5：
一种耐高温抗腐蚀永磁铁，由如下各组分重量百分比的原料制成；5％钕铁硼磁性粉末、12％Fe3O4、8％SiO2、5％硬脂酸、8％单晶氧化镁、2％碳酸钙粉、3％碳黑、3％苯甲酸钠、7％丙酸钙，余量为铁。
(1)熔炼：按配比称取原料后，将钕铁硼粉末、Fe3O4、碳酸钙粉、苯甲酸钠、硬脂酸和铁放入熔炼炉中，升温至1590℃，保温2h，然后依次加入碳黑、丙酸钙、SiO2和单晶氧化镁，继续升温至所有原料融为液态，再调节温度为2850℃，保持4h，得到永磁铁粗成品溶液；
(2)制粉：将永磁铁粗成品溶液冷却固化后得到固态粗成品永磁铁，送入管磨机连续研磨5h，得到粒径为0.5微米的永磁铁粉末；
(3)压制：将所得永磁铁粉末在氩气保护气的作用下放入磁场强度为24000Gs的磁场中取向定型，再通过400MPa压力静压制成毛坯；
(4)回火：将上述毛坯放入900℃真空环境中一次回火，持续3h，再调节温度为700℃进行二次回火，保持2h，得永磁铁；
(5)磁性检测：将所得永磁铁冷却至室温后放入磁性监测仪中检测其磁性。
将本发明实施例所得产品与市场中常见的钕铁硼磁铁进行性能测试，数据结果如下表：
耐腐蚀％ 耐高温℃ 磁能积 剩磁 硬度
实施例1 16 271 15.0 8.3 277
实施例2 14 277 14.9 8.3 281
实施例3 11 289 15.2 8.2 282
实施例4 7 302 15.1 8.3 282
实施例5 9 299 14.7 8.1 279
对照例1 30 196 14.7 8 267
对照例2 25 198 14.9 8.1 266
对照例3 21 197 14.8 8.1 269
其中耐高温性能测试采用科标检测；磁能积和剩磁检测来自磁性监测仪；耐腐蚀性能测试为将试验品置于浓硫酸酸雾中相同时间造成的腐蚀率；硬度性能测试为采用硬质合金压头以相同的试验力压入试样表面，保持8s。其中，磁能积单位是kj/m3，剩磁单位是T，硬度单位是HBW。
以上实施例仅用以说明本发明型的技术方案，而非对其限制；尽管参照前述实施例对本发明型进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明型各实施例技术方案的精神和范围。

Claims (5)

1.一种耐高温抗腐蚀永磁铁，其特征在于，由如下各组分重量百分比的原料制成：5％-20％钕铁硼磁性粉末、12％-20％Fe3O4、3％-8％SiO2、4％-8％硬脂酸、3％-9％单晶氧化镁、1％-5％碳酸钙粉、2％-5％碳黑、1％-4％苯甲酸钠、2％-7％丙酸钙，余量为铁。
2.根据权利要求1所述的耐高温抗腐蚀永磁铁，其特征在于，由如下各组分重量百分比的原料制成：10％-20％钕铁硼磁性粉末、15％-20％Fe3O4、5％-8％SiO2、5％-8％硬脂酸、4％-9％单晶氧化镁、2％-5％碳酸钙粉、3％-5％碳黑、2％-4％苯甲酸钠、3％-7％丙酸钙，余量为铁。
3.根据权利要求1或2所述的耐高温抗腐蚀永磁铁的制备方法，其特征在于，包括如下几个步骤：
(1)熔炼：按配比称取原料后，将钕铁硼粉末、Fe3O4、碳酸钙粉、苯甲酸钠、硬脂酸和铁放入熔炼炉中，升温至1500℃-1600℃，然后依次加入碳黑、丙酸钙、SiO2和单晶氧化镁，继续升温至所有原料融为液态，再调节温度为2750℃-2860℃，保持3-5h，得到永磁铁粗成品溶液；
(2)制粉：将永磁铁粗成品溶液冷却固化后得到固态粗成品永磁铁，送入管磨机连续研磨3-5h，得到粒径为0.5-1微米的永磁铁粉末；
(3)压制：将所得永磁铁粉末在氩气保护气的作用下放入磁场强度为20000-25000Gs的磁场中取向定型，再通过400MPa压力静压制成毛坯；
(4)回火：将上述毛坯放入800℃-900℃真空环境中一次回火，持续2-3h，再进调节温度为400℃-700℃进行二次回火，保持1-2h，得永磁铁；
(5)磁性检测：将所得永磁铁冷却至室温后放入磁性监测仪中检测其磁性。
4.根据权利要求3所述的耐高温抗腐蚀永磁铁的制备方法，其特征在于：所述步骤(1)中升温至1500℃-1600℃后，保温时间为1-2h。
5.根据权利要求3所述的耐高温抗腐蚀永磁铁的制备方法，其特征在于：步骤(2)中所述的管磨机转速为200-300r/min。
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