CN106024239A - 一种添加介孔材料的镀锌钕铁硼磁体及其制备方法 - Google Patents

一种添加介孔材料的镀锌钕铁硼磁体及其制备方法 Download PDF

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CN106024239A
CN106024239A CN201610555206.XA CN201610555206A CN106024239A CN 106024239 A CN106024239 A CN 106024239A CN 201610555206 A CN201610555206 A CN 201610555206A CN 106024239 A CN106024239 A CN 106024239A
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沈军
唐睿
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Anhui One Magnet Electronic Co Ltd
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Abstract

本发明公开了一种添加介孔材料的镀锌钕铁硼磁体，由下述组分按质量百分比组成：Pr‑Nd：25‑35％、B：1‑2％、Al：0.1‑1％、Cu：0‑0.2％、Co：1‑2％、Ga：0.1‑0.3％、Nb：0.1‑1％、Zr：0‑0.1％、介孔二氧化硅0.1‑1％，余量为Fe和材料中少量不可避免的杂质；本发明从气流磨磨制后的钕铁硼磁体原料粉末入手，将微米级原料粉末直接包覆镀锌，提高了钕铁硼原料粉末的抗氧化能力，介孔二氧化硅的加入使纳米组分与钕铁硼磁体主相复合成晶界相，在保证剩磁基本不变的同时提高了磁体的矫顽力，生产的钕铁硼磁体晶型结构均匀，耐温性和机械加工性显著提升，具有优良的抗氧化性和高矫顽力。

Description

一种添加介孔材料的镀锌钕铁硼磁体及其制备方法
技术领域
本发明涉及稀土永磁材料技术领域，尤其涉及一种添加介孔材料的镀锌钕铁硼磁体及其制备方法。
背景技术
钕铁硼永磁材料，作为稀土永磁材料发展的最新结果，由于其优异的磁性能而被称为磁王，是目前具有最强磁力的永久磁体，其最大磁能积高过铁氧体10倍以上，具有体积小重量轻、极高的磁能积和矫顽力、能量密度高等优点，使得钕铁硼永磁材料在现代工业和电子技术中获得了广泛应用。
近年来随着钕铁硼磁体在多领域的高速发展，烧结钕铁硼磁体以优越的性能广泛应用于各方面，从而使得计算机硬件、仪器仪表、电声电机、传感器、磁选磁化等设备的小型化、轻量化、薄型化成为可能。由于微米级钕铁硼磁体原料粉末之间的范德华力、伦敦力和磁力的相互作用使粉末团聚成二次粉末颗粒，形成了小颗粒基团，造成粉末的流动性差、取向困难，最终导致钕铁硼永磁材料具有居里温度点低、温度特性差、易被氧化腐蚀等缺点。
中国发明专利CN 105702405A首创采用纳米级介孔材料添加到钕铁硼磁体材料中来改善其微结构及结构缺陷，从而提高其矫顽力和工作温度，其优点在于加工工艺简单、晶型结构均一、磁体材料矫顽力强、耐温性好，但其并没有改善钕铁硼磁体易被氧化腐蚀的缺点，为此本发明从气流磨磨制后的钕铁硼磁体原料粉末入手，将微米级的原料粉末先进行表面镀锌，颗粒表面包覆一层纳米级锌层，再与介孔二氧化硅混合进行后续工艺，从而全面改善钕铁硼磁体的缺点。
发明内容
本发明是为了弥补现有技术的不足，提供一种添加介孔材料的镀锌钕铁硼磁体及其制备方法。
本发明是通过以下技术方案实现的：
一种添加介孔材料的镀锌钕铁硼磁体，由下述组分按质量百分比组成：
Pr-Nd：25-35％、B：1-2％、Al：0.1-1％、Cu：0-0.2％、Co：1-2％、Ga：0.1-0.3％、Nb：0.1-1％、Zr：0-0.1％、介孔二氧化硅0.1-1％，余量为Fe和材料中少量不可避免的杂质；
所述的Pr-Nd合金中Nd含量为20-40wt％。
所述的一种添加介孔材料的镀锌钕铁硼磁体，由下述组分按质量百分比组成：
Pr-Nd：28-32％、B：1.3-1.7％、Al：0.4-0.6％、Cu：0.05-0.15％、Co：1.4-1.6％、Ga：0.15-0.25％、Nb：0.3-0.7％、Zr：0.04-0.08％、介孔二氧化硅0.2-0.5％，余量为Fe和材料中少量不可避免的杂质；
所述的Pr-Nd合金中Nd含量为20-40wt％。
一种所述的添加介孔材料的镀锌钕铁硼磁体制备方法，包括以下步骤：
(1)按比例称取制备钕铁硼磁体的原料Pr-Nd、B、Al、Cu、Co、Ga、Nb、Zr、Fe，经无油、无潮和无锈处理后送入真空感应炉中，在真空度10.2-10.6Pa、温度1200-1300℃的条件下熔炼成合金液，合金液以2-4m/s的速度浇铸到铜辊表面速凝甩带成厚度为0.2-0.5mm的合金薄片；
(2)将上述合金薄片送入氢碎炉，在0.6-1.2Mpa的氢压下吸氢2-4小时，再在500-650℃的温度下脱氢6-8小时破碎成平均粒度为100-200μm的粗粉，将粗粉用气流粉碎机在0.12-0.18Mpa的压力下磨至平均粒度为3-4μm的细粉；
(3)将上述钕铁硼原料细粉用含有浓度为20-30g/L硫酸锌、25-35g/L次磷酸钠、0.002-0.005g/L甘氨乙酸、20-30g/L乳酸钠、25-35g/L柠檬酸钠的镀锌溶液浸泡进行表面镀锌，在温度70-90℃、pH4.5-5.5条件下镀锌20-30分钟至锌层厚度为40-60nm时停止；
(4)将上述镀了锌层的钕铁硼原料细粉用去离子水清洗、过滤4-6次，再将过滤好的细粉在90-110℃下恒温干燥4-5小时，冷却至室温，在氮气保护下与介孔二氧化硅在三维混料机中搅拌混合，混料时添加总重量0.1-0.3wt％润滑剂后混料3-4小时，形成均匀的混合磁粉；
(5)将上述混合磁粉在全自动成型压机中自动定量称取，取向成型压制成坯块，经真空封装、冷等静压、剥油后送入真空烧结炉中，在300-400℃下保温0.5-1小时，在800-900℃下保温2-3小时，在温度1050-1100℃、真空度0.004-0.006Pa的条件下烧结4-6小时，冷却后得到烧结磁体；
(6)将上述烧结磁体进行二级回火处理，一级回火温度850-950℃、保温3-4小时，二级回火温度450-550℃、保温4-5小时，最终得到烧结永磁体。
一种所述的添加介孔材料的镀锌钕铁硼磁体制备方法，所述步骤(3)中钕铁硼原料细粉质量与镀锌溶液体积比为35-45g：1L。
一种所述的添加介孔材料的镀锌钕铁硼磁体制备方法，所述步骤(4)中介孔二氧化硅的粒径为100-200nm、孔径为10-20nm。
与现有技术相比，本发明的优点是：
本发明从气流磨磨制后的钕铁硼磁体原料粉末入手，将微米级原料粉末直接包覆镀锌，粉末颗粒表面包覆一层纳米级锌层，提高了钕铁硼原料粉末的抗氧化能力，防止了后续过程中粉末团聚成颗粒基团，有利于粉末的取向成型；介孔二氧化硅的加入使纳米组分与钕铁硼磁体主相复合成晶界相，既可以起到异相成核作用，还可以改善钕铁硼磁体微结构，在保证剩磁基本不变的同时提高了磁体的矫顽力，生产出的烧结钕铁硼磁体晶型结构均匀，耐温性和机械加工性能都得到显著提升，更具有优良的抗氧化性和高矫顽力的优点。
具体实施方式
一种添加介孔材料的镀锌钕铁硼磁体，由下述组分按质量百分比组成：
Pr-Nd：28％、B：1.3％、Al：0.4％、Cu：0.05％、Co：1.4％、Ga：0.15％、Nb：0.3％、Zr：0.04％、介孔二氧化硅0.2％，余量为Fe和材料中少量不可避免的杂质；
所述的Pr-Nd合金中Nd含量为20wt％。
一种所述的添加介孔材料的镀锌钕铁硼磁体制备方法，包括以下步骤：
(1)按比例称取制备钕铁硼磁体的原料Pr-Nd、B、Al、Cu、Co、Ga、Nb、Zr、Fe，经无油、无潮和无锈处理后送入真空感应炉中，在真空度10.2Pa、温度1200℃的条件下熔炼成合金液，合金液以2m/s的速度浇铸到铜辊表面速凝甩带成厚度为0.2mm的合金薄片；
(2)将上述合金薄片送入氢碎炉，在0.6Mpa的氢压下吸氢2小时，再在500℃的温度下脱氢6小时破碎成平均粒度为100μm的粗粉，将粗粉用气流粉碎机在0.12Mpa的压力下磨至平均粒度为3μm的细粉；
(3)将上述钕铁硼原料细粉用含有浓度为20g/L硫酸锌、25g/L次磷酸钠、0.002g/L甘氨乙酸、20g/L乳酸钠、25g/L柠檬酸钠的镀锌溶液浸泡进行表面镀锌，在温度70℃、pH5条件下镀锌20分钟至锌层厚度为40nm时停止；
(4)将上述镀了锌层的钕铁硼原料细粉用去离子水清洗、过滤4次，再将过滤好的细粉在90℃下恒温干燥4小时，冷却至室温，在氮气保护下与介孔二氧化硅在三维混料机中搅拌混合，混料时添加总重量0.1wt％润滑剂后混料3小时，形成均匀的混合磁粉；
(5)将上述混合磁粉在全自动成型压机中自动定量称取，取向成型压制成坯块，经真空封装、冷等静压、剥油后送入真空烧结炉中，在300℃下保温0.5小时，在800℃下保温2小时，在温度1050℃、真空度0.004Pa的条件下烧结4小时，冷却后得到烧结磁体；
(6)将上述烧结磁体进行二级回火处理，一级回火温度850℃、保温3小时，二级回火温度450℃、保温4小时，最终得到烧结永磁体。
一种所述的添加介孔材料的镀锌钕铁硼磁体制备方法，所述步骤(3)中钕铁硼原料细粉质量与镀锌溶液体积比为35g：1L。
一种所述的添加介孔材料的镀锌钕铁硼磁体制备方法，所述步骤(4)中介孔二氧化硅的粒径为100nm、孔径为10nm。

Claims (5)

1.一种添加介孔材料的镀锌钕铁硼磁体，其特征在于由下述组分按质量百分比组成：
Pr-Nd：25-35％、B：1-2％、Al：0.1-1％、Cu：0-0.2％、Co：1-2％、Ga：0.1-0.3％、Nb：0.1-1％、Zr：0-0.1％、介孔二氧化硅0.1-1％，余量为Fe和材料中少量不可避免的杂质；
所述的Pr-Nd合金中Nd含量为20-40wt％。
2.根据权利要求1所述的一种添加介孔材料的镀锌钕铁硼磁体，其特征在于由下述组分按质量百分比组成：
Pr-Nd：28-32％、B：1.3-1.7％、Al：0.4-0.6％、Cu：0.05-0.15％、Co：1.4-1.6％、Ga：0.15-0.25％、Nb：0.3-0.7％、Zr：0.04-0.08％、介孔二氧化硅0.2-0.5％，余量为Fe和材料中少量不可避免的杂质；
所述的Pr-Nd合金中Nd含量为20-40wt％。
3.一种如权利要求1所述的添加介孔材料的镀锌钕铁硼磁体制备方法，其特征在于包括以下步骤：
(1)按比例称取制备钕铁硼磁体的原料Pr-Nd、B、Al、Cu、Co、Ga、Nb、Zr、Fe，经无油、无潮和无锈处理后送入真空感应炉中，在真空度10.2-10.6Pa、温度1200-1300℃的条件下熔炼成合金液，合金液以2-4m/s的速度浇铸到铜辊表面速凝甩带成厚度为0.2-0.5mm的合金薄片；
(2)将上述合金薄片送入氢碎炉，在0.6-1.2Mpa的氢压下吸氢2-4小时，再在500-650℃的温度下脱氢6-8小时破碎成平均粒度为100-200μm的粗粉，将粗粉用气流粉碎机在0.12-0.18Mpa的压力下磨至平均粒度为3-4μm的细粉；
(3)将上述钕铁硼原料细粉用含有浓度为20-30g/L硫酸锌、25-35g/L次磷酸钠、0.002-0.005g/L甘氨乙酸、20-30g/L乳酸钠、25-35g/L柠檬酸钠的镀锌溶液浸泡进行表面镀锌，在温度70-90℃、pH4.5-5.5条件下镀锌20-30分钟至锌层厚度为40-60nm时停止；
(4)将上述镀了锌层的钕铁硼原料细粉用去离子水清洗、过滤4-6次，再将过滤好的细粉在90-110℃下恒温干燥4-5小时，冷却至室温，在氮气保护下与介孔二氧化硅在三维混料机中搅拌混合，混料时添加总重量0.1-0.3wt％润滑剂后混料3-4小时，形成均匀的混合磁粉；
(5)将上述混合磁粉在全自动成型压机中自动定量称取，取向成型压制成坯块，经真空封装、冷等静压、剥油后送入真空烧结炉中，在300-400℃下保温0.5-1小时，在800-900℃下保温2-3小时，在温度1050-1100℃、真空度0.004-0.006Pa的条件下烧结4-6小时，冷却后得到烧结磁体；
(6)将上述烧结磁体进行二级回火处理，一级回火温度850-950℃、保温3-4小时，二级回火温度450-550℃、保温4-5小时，最终得到烧结永磁体。
4.一种如权利要求3所述的添加介孔材料的镀锌钕铁硼磁体制备方法，其特征在于所述步骤(3)中钕铁硼原料细粉质量与镀锌溶液体积比为35-45g：1L。
5.一种如权利要求3所述的添加介孔材料的镀锌钕铁硼磁体制备方法，其特征在于所述步骤(4)中介孔二氧化硅的粒径为100-200nm、孔径为10-20nm。
CN201610555206.XA 2016-07-14 2016-07-14 一种添加介孔材料的镀锌钕铁硼磁体及其制备方法 Pending CN106024239A (zh)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105551707A (zh) * 2016-02-25 2016-05-04 廊坊京磁精密材料有限公司 一种钕铁硼磁体原料粉末及其处理工艺
CN105702405A (zh) * 2016-04-29 2016-06-22 湖北工程学院 一种纳米复合钕铁硼磁性材料及制备方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105551707A (zh) * 2016-02-25 2016-05-04 廊坊京磁精密材料有限公司 一种钕铁硼磁体原料粉末及其处理工艺
CN105702405A (zh) * 2016-04-29 2016-06-22 湖北工程学院 一种纳米复合钕铁硼磁性材料及制备方法

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