CN117542641A - 一种耐热钕铁硼磁体的制备方法 - Google Patents
一种耐热钕铁硼磁体的制备方法 Download PDFInfo
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Abstract
本发明涉及钕铁硼磁体技术领域,且公开了一种耐热钕铁硼磁体的制备方法,通过引入Y、Ni等元素,优化了磁体元素的搭配,显著提高了钕铁硼磁体的居里温度和矫顽力、降低了温度系数,从而改善了钕铁硼磁体耐热不良的缺点;采用快淬薄带、氢爆制粉及压延成型工艺,使主相晶粒得到细化,实现了机械取向,使得磁体具备较高的磁性能;通过KH550对钕铁硼磁粉进行表面改性,脱水缩合后形成以Si‑O‑共价键形式与磁粉进行化学吸附,有利于改善磁粉与树脂的粘结性;含有耐热基团的萘基和三嗪基团的聚氨酯弹性体粘结剂,能与改性钕铁硼磁体构成一个非常稳固的体系,使得磁体在高温环境下具有优良的尺寸稳定性。
Description
技术领域
本发明涉及钕铁硼磁体技术领域,具体为一种耐热钕铁硼磁体的制备方法。
背景技术
钕铁硼磁体以其优异的磁性能而占领了永磁材料的巨大市场,在汽车电机、风力发电机及仪表器件等领域的应用越来越广泛,因而钕铁硼磁体制成的部件需要适应较高的环境温度;另外在一些精密仪器仪表及磁性器件,当外界工作环境条件变化时,要求磁体提供的磁场稳定,否则就要影响仪器仪表的精度和可靠性,因而要求磁体温度系数低,但是普通钕铁硼磁体的居里温度低、温度系数高,限制了其在环境温度较高的电机及精密仪表等领域的应用,因此有效的解决钕铁硼的高温稳定性,成为很多钕铁硼磁体研究工作的重点。
磁体的耐热性是指其磁性能不因温度的升高而劣化,在机器发热源处使用钕铁硼磁体,要求随使用温度升高而磁性能不恶化,在现有技术中,低温度系数的钕铁硼磁体,其工作温度较低、矫顽力也较低且成本普遍较高,目前烧结钕铁硼方面为了改善磁体的耐热性采取的方法主要是通过添加Co元素来提高居里温度,但是Co的添加会形成软磁性的晶界相,不起磁去耦作用,导致材料矫顽力的急剧降低;与烧结钕铁硼磁体相比,粘结钕铁硼磁体具有性价比高、成型方便、加工精度高等优势,但现有粘结钕铁硼磁体存在磁粉与专用树脂粘接不牢、树脂在磁粉表面包覆不完整、易团聚等问题,导致磁体的耐高温性能不理想。
本发明通过在钕铁硼磁体成分中引入Y、Ni等元素,使磁体的居里温度升高、温度系数降低;以合成耐热聚氨酯弹性体作为粘结剂,与表面改性后的磁粉进行压延成型,相容性好,使得制备的钕铁硼磁体较高的温度下仍保持较高的磁性能,工艺简单,成本低廉。
发明内容
本发明解决的技术问题为:
针对现有技术的不足,本发明提供了一种耐热钕铁硼磁体的制备方法,解决了现有钕铁硼磁体居里温度低、耐热性能差的问题。
为了实现上述目的,本发明采用如下技术方案:
一种耐热钕铁硼磁体的制备方法,所述制备方法按以下步骤进行:
(1)将按质量份数计的10-15份金属Nd粉、1-6份金属Y粉、1.5-4.5份金属Pr粉、2.5-3.5份金属Nb粉、45-60份金属Fe粉、8-18份金属Ni粉、3-8份ZrO2、0.6-5.4份B-Fe合金、0.2-1.5份金属Cu粉、0.5-3.0份Al2O3的原料放置于真空电弧熔炼炉的水冷铜坩埚中,通入氩气保护,在真空度为0.8×10-3Pa-1.5×10-3Pa、温度为1300-1500℃下熔炼10-30min,冷却成合金铸锭,然后将合金铸锭破碎至8-15mm,置于熔体快淬炉的铜坩埚中融化,融化后的合金液体快速浇注到钼辊上,得到钕铁硼快淬薄带。
(2)将钕铁硼快淬薄带加入到不锈钢氢爆罐中,在真空度为1.8×10-1Pa-2.8×10-1Pa、温度为450-550℃下活化20-50min,在罐内压力为0.15-0.25MPa下吸氢1-3h,在温度为480-520℃下放氢4-8h,冷却,气流磨制成粒度为1-5μm的细粉,得到钕铁硼磁粉。
(3)将钕铁硼磁粉置于KH550的乙醇溶液中,在20-35℃下,用超声波分散处理20-40min,然后浸泡12-24h,在100-120℃下干燥5-10h,得到改性钕铁硼磁粉。
(4)将耐热聚氨酯弹性体粘结剂、增塑剂、润滑剂和钙锌稳定剂加入捏合机中,在140-170℃下预处理30-60min,然后置于密闭式混炼机中,加入改性钕铁硼磁粉进行混炼,密炼机上顶栓压力为0.4-0.9MPa,将混合均匀的物料在双辊压延机上压延成型,成型后得到耐热钕铁硼磁体。
优选的,所述步骤(1)中钼辊表面线速度为5-20m/s,甩带温度为1200-1350℃。
优选的,所述步骤(3)中KH550的质量为钕铁硼磁粉质量的3-6%。
优选的,所述步骤(4)中各物质按质量份数计,耐热聚氨酯弹性体为2.5-6.5份、增塑剂为0.5-1.5份、润滑剂为2-4份、钙锌稳定剂为0.2-0.6份、改性钕铁硼磁粉为85-95份。
优选的,所述步骤(4)中混炼温度为150-180℃,混炼时间为40-80min,辊温为120-160℃。
优选的,所述耐热聚氨酯弹性体的制备方法按以下步骤进行:将聚四氢呋喃醚二醇在100-130℃下真空脱水1-3h,然后冷却至40-60℃,加入1,5-二异氰酸萘,在70-85℃下保温2-3h,得到聚氨酯预聚体,然后真空脱泡5-10min,加入扩链剂2,4,6-三(4-羟基苯基)-1,3,5-三嗪和1,4-二氧六环,搅拌10-20min,浇注到涂有脱模剂的平板模具中,固化干燥后得到耐热聚氨酯弹性体。
优选的,所述各物质按质量份数计,聚四氢呋喃醚二醇为100份,1,5-二异氰酸萘为42-105份,扩链剂2,4,6-三(4-羟基苯基)-1,3,5-三嗪为20-30份。
优选的,所述固化温度为60-80℃,固化时间为5-10天;所述干燥温度为110-130℃,干燥时间为2-4h。
与现有技术相比,本发明具有如下有益效果:
(1)成分优化:通过引入适量的Y、Ni等元素,优化了磁体元素的搭配,显著提高了钕铁硼磁体的居里温度和矫顽力、降低了温度系数,且保持了磁体本身的磁性能,进一步改善了钕铁硼磁体耐热性能不良的缺点,扩大了钕铁硼磁体的适用范围。
(2)工艺优化:采用快淬薄带工艺,可以使主相晶粒得到细化,富钕相均匀分布,使得对主相晶粒的去耦合作用更加完全,从而提高磁体的矫顽力;采用氢爆制粉工艺可以获得粒径为1-5μm的颗粒,减少磁体表面的氧化,从而获得良好取向的磁体;采用压延成型工艺,使得磁粉在平行和垂直压延方向上,均能呈现片状平铺排列状态,实现了机械取向,从而具备了较高的磁性能。
(3)磁粉表面改性优化:通过KH550对钕铁硼磁粉进行表面改性,脱水缩合后形成以Si-O-共价键形式与磁粉进行化学吸附,这种吸附与磁粉结合紧密,具有良好的防氧化效果且有利于改善磁粉与树脂的粘结性。
(4)耐热性聚氨酯弹性体粘结剂优化:通过合成含有耐热基团的萘基和三嗪基团的聚氨酯弹性体,与改性钕铁硼磁体构成一个非常稳固、刚硬的体系,使得磁体在高温环境下具有优良的尺寸稳定性。
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作出创造性劳动前提下所获得的所有其他实施例,都涉及本发明保护的范围。
耐热钕铁硼磁体的制备:
(1)将按质量份数计的10-15份金属Nd粉、1-6份金属Y粉、1.5-4.5份金属Pr粉、2.5-3.5份金属Nb粉、45-60份金属Fe粉、8-18份金属Ni粉、3-8份ZrO2、0.6-5.4份B-Fe合金(含B为20-30wt%)、0.2-1.5份金属Cu粉、0.5-3.0份Al2O3的原料放置于真空电弧熔炼炉的水冷铜坩埚中,通入氩气保护,在真空度为0.8×10-3Pa-1.5×10-3Pa、温度为1300-1500℃下熔炼10-30min,冷却成合金铸锭,然后将合金铸锭破碎至8-15mm,置于熔体快淬炉的铜坩埚中融化,融化后的合金液体快速浇注到钼辊上,钼辊表面线速度为5-20m/s,甩带温度为1200-1350℃,得到钕铁硼快淬薄带。
(2)将钕铁硼快淬薄带加入到不锈钢氢爆罐中,在真空度为1.8×10-1Pa-2.8×10-1Pa、温度为450-550℃下活化20-50min,在罐内压力为0.15-0.25MPa下吸氢1-3h,在温度为480-520℃下放氢4-8h,冷却,气流磨制成粒度为1-5μm的细粉,得到钕铁硼磁粉。
(3)将钕铁硼磁粉置于质量分数为3-6%的KH550的乙醇溶液中,在20-35℃下,用超声波分散处理20-40min,然后浸泡12-24h,在100-120℃下干燥5-10h,得到改性钕铁硼磁粉。
(4)将按质量份数计的100份聚四氢呋喃醚二醇在100-130℃下真空脱水1-3h,然后冷却至40-60℃,加入42-105份1,5-二异氰酸萘,在70-85℃下保温2-3h,得到聚氨酯预聚体,然后真空脱泡5-10min,加入20-30份扩链剂2,4,6-三(4-羟基苯基)-1,3,5-三嗪和1,4-二氧六环,搅拌10-20min,浇注到涂有脱模剂的平板模具中,在60-80℃固化5-10天,在110-130℃干燥时间2-4h,得到耐热聚氨酯弹性体粘结剂。
(5)将按质量份数计的2.5-6.5份耐热聚氨酯弹性体粘结剂、0.5-1.5份增塑剂、2-4份润滑剂和0.2-0.6份钙锌稳定剂加入捏合机中,在140-170℃下预处理30-60min,然后置于密闭式混炼机中,加入85-95份改性钕铁硼磁粉进行混炼,混炼温度为150-180℃,混炼时间为40-80min,辊温为120-160℃,密炼机上顶栓压力为0.4-0.9MPa,将混合均匀的物料在双辊压延机上压延成型,成型后得到耐热钕铁硼磁体。
实施例1
(1)将按质量份数计的12份金属Nd粉、1份金属Y粉、3.5份金属Pr粉、3份金属Nb粉、56份金属Fe粉、8份金属Ni粉、4.5份ZrO2、0.6份B-Fe合金(含B为25wt%)、0.6份金属Cu粉、2.6份Al2O3的原料放置于真空电弧熔炼炉的水冷铜坩埚中,通入氩气保护,在真空度为1.2×10-3Pa、温度为1350℃下熔炼20min,冷却成合金铸锭,然后将合金铸锭破碎至10mm,置于熔体快淬炉的铜坩埚中融化,融化后的合金液体快速浇注到钼辊上,钼辊表面线速度为15m/s,甩带温度为1300℃,得到钕铁硼快淬薄带。
(2)将钕铁硼快淬薄带加入到不锈钢氢爆罐中,在真空度为2.2×10-1Pa、温度为500℃下活化40min,在罐内压力为0.2MPa下吸氢2h,在温度为510℃下放氢5h,冷却,气流磨制成粒度为2μm的细粉,得到钕铁硼磁粉。
(3)将钕铁硼磁粉置于质量分数为5%的KH550的乙醇溶液中,在30℃下,用超声波分散处理35min,然后浸泡16h,在110℃下干燥8h,得到改性钕铁硼磁粉。
(4)将按质量份数计的100份聚四氢呋喃醚二醇在120℃下真空脱水3h,然后冷却至45℃,加入78份1,5-二异氰酸萘,在80℃下保温2h,得到聚氨酯预聚体,然后真空脱泡10min,加入25份扩链剂2,4,6-三(4-羟基苯基)-1,3,5-三嗪和1,4-二氧六环,搅拌15min,浇注到涂有脱模剂的平板模具中,在70℃固化9天,在130℃干燥时间3h,得到耐热聚氨酯弹性体粘结剂。
(5)将按质量份数计的2.5份耐热聚氨酯弹性体粘结剂、1.2份增塑剂邻苯二甲酸醋、3份润滑剂脂肪酰胺和0.5份钙锌稳定剂加入捏合机中,在160℃下预处理50min,然后置于密闭式混炼机中,加入90份改性钕铁硼磁粉进行混炼,混炼温度为170℃,混炼时间为60min,辊温为150℃,密炼机上顶栓压力为0.6MPa,将混合均匀的物料在双辊压延机上压延成型,成型后得到耐热钕铁硼磁体。
实施例2
本实施例与实施例1的区别在于,步骤(1)中金属Y粉的用量为2份,其他条件不变。
实施例3
本实施例与实施例1的区别在于,步骤(1)中金属Y粉的用量为3份,其他条件不变。
实施例4
本实施例与实施例1的区别在于,步骤(1)中金属Y粉的用量为4份,其他条件不变。
实施例5
本实施例与实施例1的区别在于,步骤(1)中金属Y粉的用量为5份,其他条件不变。
实施例6
本实施例与实施例1的区别在于,步骤(1)中金属Y粉的用量为6份,其他条件不变。
对比例1
本对比例与实施例1的区别在于,步骤(1)中不加入金属Y粉,其他条件不变。
居里温度测试:
采用振动样品磁强计(VSM)测试磁体的居里温度和矫顽力温度系数。
居里温度(℃) | 矫顽力温度系数(%/℃) | |
实施例1 | 310 | -0.2924 |
实施例2 | 321 | -0.2410 |
实施例3 | 339 | -0.2119 |
实施例4 | 348 | -0.1945 |
实施例5 | 355 | -0.1834 |
实施例6 | 364 | -0.1675 |
对比例1 | 289 | -0.3598 |
强铁磁性体从铁磁性或亚铁磁性转变为顺磁性的临界温度称为居里温度,居里温度高材料的工作温度就高,而且有利于提高磁性材料的温度稳定性。从上表测试结果可知,随着钕铁硼合金中Y元素含量的增加,磁体的居里温度从289℃上升至364℃,提高了75℃,说明Y元素的添加提高了钕铁硼磁体的高温工作的稳定性,显著拓宽了钕铁硼磁体的应用范围;矫顽力温度系数指其矫顽力随温度变化的比率,该系数的绝对值愈小,该磁体的磁性能越好;上表数据表明,随着Y元素含量的增加,矫顽力温度系数由对比例1的-0.3598%/℃变化为实施例6的-0.1675%/℃,这说明Y元素的加入有效改善了钕铁硼磁体的耐热性,因此可以被运用到更宽的温度范围。
实施例7
本实施例与实施例1的区别在于,步骤(1)中金属Ni粉的用量为11份,其他条件不变。
实施例8
本实施例与实施例1的区别在于,步骤(1)中金属Ni粉的用量为14份,其他条件不变。
实施例9
本实施例与实施例1的区别在于,步骤(1)中金属Ni粉的用量为16份,其他条件不变。
实施例10
本实施例与实施例1的区别在于,步骤(1)中金属Ni粉的用量为18份,其他条件不变。
对比例2
本对比例与实施例1的区别在于,步骤(1)中不加入金属Ni粉,其他条件不变。
磁性能测试:
采用振动样品磁强计(VSM)测试样品的磁性能,获得矫顽力、剩磁等磁性参数。
矫顽力(KA/m) | 剩磁(T) | |
实施例1 | 680 | 1.237 |
实施例7 | 765 | 1.252 |
实施例8 | 834 | 1.304 |
实施例9 | 898 | 1.325 |
实施例10 | 956 | 1.357 |
对比例2 | 550 | 1.121 |
矫顽力代表磁性材料抵抗退磁的能力,在磁体使用中,磁体矫顽力越高,温度稳定性越好。由上表测试结果可知,钕铁硼合金中Ni元素含量的增加,磁体的矫顽力逐渐增大,说明磁体的耐热性能得到一定程度的提升;钕铁硼磁体的剩磁随着Ni元素含量的增加有小幅度的增长,说明Ni元素的添加不影响磁体的磁性能。
实施例11
本实施例与实施例1的区别在于,步骤(5)中耐热聚氨酯弹性体粘结剂的用量为3.5份,其他条件不变。
实施例12
本实施例与实施例1的区别在于,步骤(5)中耐热聚氨酯弹性体粘结剂的用量为4.5份,其他条件不变。
实施例13
本实施例与实施例1的区别在于,步骤(5)中耐热聚氨酯弹性体粘结剂的用量为5.5份,其他条件不变。
实施例14
本实施例与实施例1的区别在于,步骤(5)中耐热聚氨酯弹性体粘结剂的用量为6.5份,其他条件不变。
对比例3
本对比例与实施例1的区别在于,步骤(5)中不加入耐热聚氨酯弹性体粘结剂,其他条件不变。
耐温尺寸稳定性测试:
采用烘箱进行磁体的耐温尺寸稳定性测试,将待测磁体在120℃的烘箱中放置72h,计算磁体的体积变化率。
耐高温性是磁体能否在高温环境中长期工作的一个重要指标,如果耐高温性差,磁体会出现老化、膨胀、分解,导致磁体尺寸发生明显变化、磁场强度衰减而使器件无法工作。由上表测试结果可知,随着磁体中耐热聚氨酯弹性体粘结剂含量的增加,磁体在120℃烘箱中干燥72h后,其体积变化率逐渐减小,有更优的耐高温稳定特性,这是因为聚氨酯弹性体既具有橡胶的高弹性和塑料的高强度,还有优异的耐温耐磨特性,引入的耐热性好的萘基和三嗪基团,使得制备的粘结剂耐高温性能优异,钕铁硼磁体经KH550改性后,能与聚氨酯形成较强的结合力,从而进一步提高了磁体的耐热特性。
以上所述,仅为本申请的具体实施方式,但本申请的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本申请揭露的技术范围内,可轻易想到变化或替换,都应涵盖在本申请的保护范围之内。
Claims (8)
1.一种耐热钕铁硼磁体的制备方法,其特征在于,所述制备方法按以下步骤进行:
(1)将按质量份数计的10-15份金属Nd粉、1-6份金属Y粉、1.5-4.5份金属Pr粉、2.5-3.5份金属Nb粉、45-60份金属Fe粉、8-18份金属Ni粉、3-8份ZrO2、0.6-5.4份B-Fe合金、0.2-1.5份金属Cu粉、0.5-3.0份Al2O3的原料放置于真空电弧熔炼炉的水冷铜坩埚中,通入氩气保护,在真空度为0.8×10-3Pa-1.5×10-3Pa、温度为1300-1500℃下熔炼10-30min,冷却成合金铸锭,然后将合金铸锭破碎至8-15mm,置于熔体快淬炉的铜坩埚中融化,融化后的合金液体快速浇注到钼辊上,得到钕铁硼快淬薄带;
(2)将钕铁硼快淬薄带加入到不锈钢氢爆罐中,在真空度为1.8×10-1Pa-2.8×10-1Pa、温度为450-550℃下活化20-50min,在罐内压力为0.15-0.25MPa下吸氢1-3h,在温度为480-520℃下放氢4-8h,冷却,气流磨制成粒度为1-5μm的细粉,得到钕铁硼磁粉;
(3)将钕铁硼磁粉置于KH550的乙醇溶液中,在20-35℃下,用超声波分散处理20-40min,然后浸泡12-24h,在100-120℃下干燥5-10h,得到改性钕铁硼磁粉;
(4)将耐热聚氨酯弹性体粘结剂、增塑剂、润滑剂和钙锌稳定剂加入捏合机中,在140-170℃下预处理30-60min,然后置于密闭式混炼机中,加入改性钕铁硼磁粉进行混炼,密炼机上顶栓压力为0.4-0.9MPa,将混合均匀的物料在双辊压延机上压延成型,成型后得到耐热钕铁硼磁体。
2.根据权利要求1所述的耐热钕铁硼磁体的制备方法,其特征在于,所述步骤(1)中钼辊表面线速度为5-20m/s,甩带温度为1200-1350℃。
3.根据权利要求1所述的耐热钕铁硼磁体的制备方法,其特征在于,所述步骤(3)中KH550的质量为钕铁硼磁粉质量的3-6%。
4.根据权利要求1所述的耐热钕铁硼磁体的制备方法,其特征在于,所述步骤(4)中各物质按质量份数计,耐热聚氨酯弹性体为2.5-6.5份、增塑剂为0.5-1.5份、润滑剂为2-4份、钙锌稳定剂为0.2-0.6份、改性钕铁硼磁粉为85-95份。
5.根据权利要求1所述的耐热钕铁硼磁体的制备方法,其特征在于,所述步骤(4)中混炼温度为150-180℃,混炼时间为40-80min,辊温为120-160℃。
6.根据权利要求1所述的耐热钕铁硼磁体的制备方法,其特征在于,所述耐热聚氨酯弹性体的制备方法按以下步骤进行:将聚四氢呋喃醚二醇在100-130℃下真空脱水1-3h,然后冷却至40-60℃,加入1,5-二异氰酸萘,在70-85℃下保温2-3h,得到聚氨酯预聚体,然后真空脱泡5-10min,加入扩链剂2,4,6-三(4-羟基苯基)-1,3,5-三嗪和1,4-二氧六环,搅拌10-20min,浇注到涂有脱模剂的平板模具中,固化干燥后得到耐热聚氨酯弹性体。
7.根据权利要求6所述的耐热钕铁硼磁体的制备方法,其特征在于,所述各物质按质量份数计,聚四氢呋喃醚二醇为100份,1,5-二异氰酸萘为42-105份,扩链剂2,4,6-三(4-羟基苯基)-1,3,5-三嗪为20-30份。
8.根据权利要求6所述的耐热钕铁硼磁体的制备方法,其特征在于,所述固化温度为60-80℃,固化时间为5-10天;所述干燥温度为110-130℃,干燥时间为2-4h。
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