CN105931785A - 一种钆钬离子注入的镀镍钕铁硼磁体及其制备方法 - Google Patents

一种钆钬离子注入的镀镍钕铁硼磁体及其制备方法 Download PDF

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CN105931785A
CN105931785A CN201610555168.8A CN201610555168A CN105931785A CN 105931785 A CN105931785 A CN 105931785A CN 201610555168 A CN201610555168 A CN 201610555168A CN 105931785 A CN105931785 A CN 105931785A
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唐睿
沈军
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Anhui One Magnet Electronic Co Ltd
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Abstract

本发明公开了一种钆钬离子注入的镀镍钕铁硼磁体，由下述组分按质量百分比组成：Pr‑Nd：25‑35％、B：0.5‑1.5％、Al：0.1‑1％、Cu：0‑0.2％、Co：1‑2％、Ga：0.1‑1％、Nb：0.02‑0.08％、Zr：0.01‑0.05％、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；本发明生产的烧结钕铁硼磁体晶型结构均匀，靠近磁体核心的区域重稀土含量偏低，保证了磁体的剩磁基本不受影响，靠近磁体表面的区域重稀土含量偏高，显著提高了磁体的矫顽力，钕铁硼烧结磁体的缺点得到全面改善、优点得到大幅提高。

Description

一种钆钬离子注入的镀镍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，尤其涉及一种钆钬离子注入的镀镍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容易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，导致最终磁体晶界中富稀土相缺失或不连续，进行晶界扩散处理时会影响Dy/Tb等重稀土元素沿晶界向磁体内部的扩散效果。
中国发明专利CN105702405A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。
为满足钕铁硼磁体同时具有高磁能积和高矫顽力的要求，最直接方式是大量添加Dy/Tb等重稀土元素，然而在磁体中添加过多Dy会因为Dy与Fe形成反铁磁耦合，致使磁体的剩磁会随着Dy的增加而下降，并且重稀土元素资源稀缺、价格昂贵，以现有工艺生产高矫顽力磁体会提高成本和加剧资源消耗。烧结钕铁硼晶界扩散工艺是在已经烧结成型的钕铁硼毛坯状态下从表面开始向内部渗透，避免了主相中重稀土含量过多的问题，能够在几乎不损害剩磁的同时大幅提高磁体矫顽力，同时重稀土元素的含量显著降低；但是重稀土只能在烧结完成的毛坯表面扩散导致了重稀土在磁体内部的扩散深度有限、重稀土浓度由表及里呈衰减式梯度分布。
中国发明专利CN105742048A采用高能离子的方式将稀土及合金注入钕铁硼预烧坯，解决了现有晶界扩散技术中稀土及合金较多的残留在钕铁硼磁体表面，稀土实际利用率不高的问题，但是其只是提高了稀土合金的扩散效率，轻重稀土金属和常规金属的随意配比不但使得磁体晶界结构复杂、晶界中富Nd相缺失且不连续，最终影响Dy/Tb等重稀土元素沿晶界向磁体内部扩散的效果，实际上并没有大幅度提高钕铁硼磁体的矫顽力。
为此本发明从气流磨磨制后的钕铁硼磁体原料粉末入手，将微米级原料粉末先进行表面镀镍，颗粒表面包覆一层纳米级镍层，再与介孔二氧化硅混合进行取向压坯，预烧坯后以高能离子形式注入重稀土合金，再经烧结致密化并发生晶界扩散，改善磁体边界结构，从而提高烧结钕铁硼磁体的矫顽力。
发明内容
本发明是为了弥补现有技术的不足，提供一种钆钬离子注入的镀镍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：
一种钆钬离子注入的镀镍钕铁硼磁体，由下述组分按质量百分比组成：
Pr-Nd：25-35％、B：0.5-1.5％、Al：0.1-1％、Cu：0-0.2％、Co：1-2％、Ga：0.1-1％、Nb：0.02-0.08％、Zr：0.01-0.05％、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％；
所述的介孔二氧化硅的粒径为100-200nm、孔径为10-20nm。
所述的一种钆钬离子注入的镀镍钕铁硼磁体，由下述组分按质量百分比组成：
Pr-Nd：28-32％、B：0.8-1.2％、Al：0.4-0.6％、Cu：0.05-0.15％、Co：1.4-1.6％、Ga：0.3-0.7％、Nb：0.04-0.06％、Zr：0.02-0.04％、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％；
所述的介孔二氧化硅的粒径为100-200nm、孔径为10-20nm。
一种所述的钆钬离子注入的镀镍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1300-1400℃条件下熔炼成合金液，合金液用真空速凝炉在1300-1400℃、氩气保护下速凝甩带成平均厚度为0.2-0.4mm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200-250g/LNiSO4·6H2O、25-35g/LNiCl2·6H2O、30-40g/LH3BO3、0.5-1g/L糖精钠、1-2g/L十二烷基硫酸钠的镀镍溶液浸泡进行表面电镀镍层，在温度为40-60℃、pH为4.5-5.5、电流密度为1-2A/dm2的条件下电镀20-30分钟至表面镍层厚度为40-60nm时停止；
(4)将上述镀了镍层的钕铁硼原料细粉用去离子水清洗、过滤4-6次，过滤好的细粉在90-110℃下恒温干燥4-5小时，冷却至室温，在氮气保护下细粉与介孔二氧化硅以及总重量0.1-0.3wt％的润滑剂在三维混料机中混料3-4小时，形成均匀的混合磁粉；
(5)将上述混合磁粉用全自动成型压机自动定量称取，取向成型压制成坯，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，得到孔隙率10-20％预烧坯，送入离子注入装置内，以高能离子形式将重稀土合金Gd100-aHoa注入预烧坯表面，注入能量100-300keV、注入计量2-8×1017cm-2，再送入真空烧结炉中进一步烧结致密化；
(6)在温度1000-1100℃、真空度0.004-0.006Pa的条件下烧结3-5小时，冷却后得到烧结磁体，再经二级真空回火处理，真空度为0.003-0.005Pa条件下一级回火温度850-950℃、保温2-3小时，二级回火温度450-550℃、保温3-4小时，最终得到烧结钕铁硼磁体。
一种所述的钆钬离子注入的镀镍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镍溶液体积比为70-90g：1L。
一种所述的钆钬离子注入的镀镍钕铁硼磁体制备方法，所述步骤(5)中a为Ho在重稀土合金Gd100-aHoa中的原子分数，30at％≤a≤50at％。
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镍，粉末颗粒表面包覆一层纳米级镍层，提高了钕铁硼原料粉末的耐腐蚀性，并且阻止后续过程中粉末团聚成颗粒基团，有利于粉末的取向成型，在后续晶界扩散处理时保证了磁体晶界中富稀土相足够且连续，大幅度提高重稀土元素沿晶界向磁体内部的扩散效率，在克服了晶界扩散对产品尺寸要求的同时得到了更高性能的钕铁硼磁体；介孔二氧化硅的加入使纳米组分与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；采用离子注入工艺将重稀土元素Gd、Ho以高能离子形式注入预烧坯表面，再进行晶界扩散处理，改善边界结构，提高矫顽力，通过控制注入能量和计量来减少重稀土元素的使用量、提高其实际利用率，避免多余稀土富集在磁体表面，增加离子注入深度来缩短扩散路径、提高扩散效率；生产的烧结钕铁硼磁体晶型结构均匀，靠近磁体核心的区域重稀土含量偏低，保证了磁体的剩磁基本不受影响，靠近磁体表面的区域重稀土含量偏高，显著提高了磁体的矫顽力，钕铁硼烧结磁体的缺点得到全面改善、优点得到大幅提高。
具体实施方式
一种钆钬离子注入的镀镍钕铁硼磁体，由下述组分按质量百分比组成：
Pr-Nd：28％、B：0.8％、Al：0.4％、Cu：0.05％、Co：1.4％、Ga：0.3％、Nb：0.04％、Zr：0.02％、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％；
所述的介孔二氧化硅的粒径为100nm、孔径为10nm。
一种所述的钆钬离子注入的镀镍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1300℃条件下熔炼成合金液，合金液用真空速凝炉在1300℃、氩气保护下速凝甩带成平均厚度为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200g/LNiSO4·6H2O、25g/LNiCl2·6H2O、30g/LH3BO3、0.5g/L糖精钠、1g/L十二烷基硫酸钠的镀镍溶液浸泡进行表面电镀镍层，在温度为40℃、pH为4.5、电流密度为1A/dm2的条件下电镀20分钟至表面镍层厚度为40nm时停止；
(4)将上述镀了镍层的钕铁硼原料细粉用去离子水清洗、过滤4次，过滤好的细粉在90℃下恒温干燥4小时，冷却至室温，在氮气保护下细粉与介孔二氧化硅以及总重量0.1wt％的润滑剂在三维混料机中混料3小时，形成均匀的混合磁粉；
(5)将上述混合磁粉用全自动成型压机自动定量称取，取向成型压制成坯，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，得到孔隙率10％预烧坯，送入离子注入装置内，以高能离子形式将重稀土合金Gd100-aHoa注入预烧坯表面，注入能量100keV、注入计量2×1017cm-2，再送入真空烧结炉中进一步烧结致密化；
(6)在温度1000℃、真空度0.004Pa的条件下烧结3小时，冷却后得到烧结磁体，再经二级真空回火处理，真空度为0.003Pa条件下一级回火温度850℃、保温2小时，二级回火温度450℃、保温3小时，最终得到烧结钕铁硼磁体。
一种所述的钆钬离子注入的镀镍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镍溶液体积比为70g：1L。
一种所述的钆钬离子注入的镀镍钕铁硼磁体制备方法，所述步骤(5)中a为Ho在重稀土合金Gd100-aHoa中的原子分数，30at％≤a≤50at％。

Claims (5)

1.一种钆钬离子注入的镀镍钕铁硼磁体，其特征在于由下述组分按质量百分比组成：
Pr-Nd：25-35％、B：0.5-1.5％、Al：0.1-1％、Cu：0-0.2％、Co：1-2％、Ga：0.1-1％、Nb：0.02-0.08％、Zr：0.01-0.05％、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％；
所述的介孔二氧化硅的粒径为100-200nm、孔径为10-20nm。
2.根据权利要求1所述的一种钆钬离子注入的镀镍钕铁硼磁体，其特征在于由下述组分按质量百分比组成：
Pr-Nd：28-32％、B：0.8-1.2％、Al：0.4-0.6％、Cu：0.05-0.15％、Co：1.4-1.6％、Ga：0.3-0.7％、Nb：0.04-0.06％、Zr：0.02-0.04％、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％；
所述的介孔二氧化硅的粒径为100-200nm、孔径为10-20nm。
3.一种如权利要求1所述的钆钬离子注入的镀镍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1300-1400℃条件下熔炼成合金液，合金液用真空速凝炉在1300-1400℃、氩气保护下速凝甩带成平均厚度为0.2-0.4mm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200-250g/LNiSO4·6H2O、25-35g/LNiCl2·6H2O、30-40g/LH3BO3、0.5-1g/L糖精钠、1-2g/L十二烷基硫酸钠的镀镍溶液浸泡进行表面电镀镍层，在温度为40-60℃、pH为4.5-5.5、电流密度为1-2A/dm2的条件下电镀20-30分钟至表面镍层厚度为40-60nm时停止；
(4)将上述镀了镍层的钕铁硼原料细粉用去离子水清洗、过滤4-6次，过滤好的细粉在90-110℃下恒温干燥4-5小时，冷却至室温，在氮气保护下细粉与介孔二氧化硅以及总重量0.1-0.3wt％的润滑剂在三维混料机中混料3-4小时，形成均匀的混合磁粉；
(5)将上述混合磁粉用全自动成型压机自动定量称取，取向成型压制成坯，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，得到孔隙率10-20％预烧坯，送入离子注入装置内，以高能离子形式将重稀土合金Gd100-aHoa注入预烧坯表面，注入能量100-300keV、注入计量2-8×1017cm-2，再送入真空烧结炉中进一步烧结致密化；
(6)在温度1000-1100℃、真空度0.004-0.006Pa的条件下烧结3-5小时，冷却后得到烧结磁体，再经二级真空回火处理，真空度为0.003-0.005Pa条件下一级回火温度850-950℃、保温2-3小时，二级回火温度450-550℃、保温3-4小时，最终得到烧结钕铁硼磁体。
4.一种如权利要求3所述的钆钬离子注入的镀镍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镍溶液体积比为70-90g：1L。
5.一种如权利要求3所述的钆钬离子注入的镀镍钕铁硼磁体制备方法，其特征在于所述步骤(5)中a为Ho在重稀土合金Gd100-aHoa中的原子分数，30at％≤a≤50at％。
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