CN1199204C - 高耐气候性磁铁粉的制造方法及得到的产品 - Google Patents
高耐气候性磁铁粉的制造方法及得到的产品 Download PDFInfo
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- CN1199204C CN1199204C CN01130728.5A CN01130728A CN1199204C CN 1199204 C CN1199204 C CN 1199204C CN 01130728 A CN01130728 A CN 01130728A CN 1199204 C CN1199204 C CN 1199204C
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- Prior art keywords
- powder
- magnetic iron
- iron powder
- magnet
- resin
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- 230000006641 stabilisation Effects 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000010729 system oil Substances 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 238000001721 transfer moulding Methods 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
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Abstract
一种高耐气候性磁铁粉的制造方法,通过在有机溶剂中粉碎含有稀土类元素的铁系磁铁合金粉制造磁铁粉,在粉碎磁铁合金粉时,在上述有机溶剂中添加磷酸,相对于上述磁铁合金粉,磷酸的添加量是0.1mol/kg以上2mol/kg以下,在粉碎磁铁合金粉后,进而在惰性气体中或真空中,在100℃以上400℃以下的温度范围内进行加热处理,根据此制造方法获得了高耐气候性磁铁粉,并提供含有它的粘结磁铁用树脂组合物及粘结磁铁,特别在实用中重要的湿度环境下,其耐气候性优良且具有高矫顽力。
Description
技术领域
本发明涉及高耐气候性磁铁粉的制造方法及得到的产品,进而详细地是涉及制造耐气候性优良的、含有稀土类元素的铁系磁铁粉的制造方法及由其制造方法得到的高耐气候性磁铁粉,进而含有它的粘结磁铁用树脂组合物及粘结磁铁。
背景技术
以往,铁素体磁铁、铝铁镍钴磁铁、稀土类磁铁等用于以电机为主的各种用途。可是,这些磁铁,由于主要是用烧结法制造的,所以一般有脆、难以得到薄壁的或形状复杂的缺点。此外,烧结时的收缩率可大到15~20%,所以也得不到尺寸精度高的,为了提高精度需要进行研磨等后加工。
另一方面,粘结磁铁,是为解决这些烧结法的缺点同时开拓新的用途,而于近年来开发出来的,但通常是通过将聚酰胺树脂、对聚苯硫树脂等热塑性树脂作为粘结剂,在其中充填磁性粉末而制造的。
可是,即使在这样的粘结磁铁中,特别是使用含有稀土类元素的铁系磁铁粉的粘结磁铁,由于在高温多湿氛围下容易生锈及磁特性降低,为了防止这些,例如在成型体表面形成热固化性树脂等涂层膜抑制生锈,或者,如日本第208321/2000号发明专利申请公开公报公开的那样,在成型体表面施以含有磷酸盐涂料的被膜处理来抑制生锈,但是在难生锈特性和矫顽力等磁特性这一点上不能充分满足要求。
可是,在将含有稀土类元素的铁系磁铁粉与树脂混练作成粘结磁铁使用时,为了得到高磁特性,必须将磁铁合金粉粉碎成数μm。磁铁合金粉的粉碎通常是在惰性气体中或在溶剂中进行的,但由于粉碎后的磁铁粉的活性极高,所以若在成型体上施以被膜处理前接触大气,存在氧化生锈激烈进行而使磁特性劣化的问题。
为了解决此问题,例如将磁铁合金粉粉碎成数μm后将少许氧导入惰性氛围中将磁铁粉缓慢氧化,或者如日本第251124/1999号发明专利申请公开公报公开的那样,在粉碎后的磁铁粉施以磷酸盐的被膜处理。
可是,存在着粉碎后的磁铁粉由于其磁性而相互凝集,即使用被膜保护凝集粉表面也不能对每个磁铁粉进行充分保护,而这样得到的磁铁粉,虽然可提高在干燥环境下的耐气候性,但问题是实用上重要的湿度环境下的耐气候性未得到圆满改善。
这样的状况下,近年,对于用于小型电机、音响设备、办公自动化(OA)设备等粘结磁铁,从设备小型化的需要,要求磁特性优良的,但对于由以往含有稀土类元素的铁系磁铁粉得到的粘结磁铁的磁特性用于这些用途是不充分的,强烈希望尽早改善含有稀土类元素的铁系磁铁粉的耐气候性,提高粘结磁铁的磁特性。
发明内容
本发明的目的鉴于上述的以往技术的问题,在于提供耐气候性优良的、特别在实用上重要的湿度环境下具有矫顽力的含有稀土类元素的铁系磁铁粉的制造方法及由其制法得到的高耐气候性磁铁粉,进而含有它的粘结磁铁用树脂组合物以及粘结磁铁。
本发明者们,为了达到上述目的研究发现,在有机溶剂中粉碎含有稀土类元素的铁系磁铁合金粉制造磁铁粉的方法中,在粉碎磁铁合金粉时,通过添加磷酸可得到所希望的耐气候性优良、抑制在湿度环境下的矫顽力降低的磁铁粉而完成本发明。
本发明提供一种高耐气候性磁铁粉的制造方法,通过在有机溶剂中粉碎含有稀土类元素的铁系磁铁合金粉制造磁铁粉,在粉碎磁铁合金粉时,在上述有机溶剂中添加磷酸,相对于上述磁铁合金粉,磷酸的添加量是0.1mol/kg以上2mol/kg以下,在粉碎磁铁合金粉后,进而在惰性气体中或真空中,在100℃以上400℃以下的温度范围内进行加热处理。
本发明还提供通过上述制造方法得到的高耐气候性磁铁粉。
本发明提供一种粘结磁铁用树脂组合物,是将上述高耐气候性磁铁粉作为主成份。
本发明提供一种粘结磁铁,是成型上述的粘结磁铁用树脂组合物而得到的。
用本发明的制造方法得到的磁铁粉,在粉碎同时通过磷酸处理可能是用被膜保护每个磁铁粉表面的原因,与以往方法得到的磁铁粉比较,耐气候性显著提高。另外,即使破碎干燥后磁铁粉的凝集体也不放热,在粘结磁铁的制造中与树脂混练时的粉末使用容易的同时,可防止由于放热的磁特性的劣化。通过用本发明的制造方法得到的磁铁粉可制造高耐气候性粘结磁铁,其工业价值极大。
具体实施方式
以下,详细地说明本发明。
1、磁铁合金粉
本发明所用的磁铁合金粉,只要是至少含有稀土类元素的铁系磁铁合金粉,就没有特别限制,例如可举出通常用于粘结磁铁的稀土类-铁-硼系、稀土类-铁-氮系的各种磁性粉。其中,特别优选的是Nd-Fe-B系的液体急冷法的合金粉末、Sm-Fe-N系的合金粉末、在表面化学被覆锌的Sm-Fe-N系的合金粉末、Nd-(Dy,Tb)-Fe-B系的合金粉末、Sm-Fe-Co-N系的合金粉末。
2、高耐气候性磁铁粉的制造方法
在本发明中,在有机溶剂中粉碎含有稀土类元素的铁系磁铁合金粉制造磁铁粉时,添加规定量的磷酸。
作为本发明所使用的磷酸,没有特别限制,可使用市售的通常的磷酸,例如85%浓度的磷酸水溶液。
另外,磷酸的添加方法,没有特别限制,例如在使用介质搅拌磨等粉碎时,在作为溶剂使用的有机溶剂中添加磷酸。磷酸只要是最终达到所希望的磷酸浓度就可以,也可在粉碎开始前一次添加,也可在粉碎中慢慢添加,但通常在溶液中必须存在磷酸,以使立即处理粉碎产生的新生的破断面。另外,作为有机溶剂,没有特别限制,通常可以使用乙醇或异丙醇等醇类、酮类、低级烃类、芳香族类或这些的混合物。
磷酸的添加量,与粉碎后的磁铁粉的粒径、表面积等有关,所以不能一概而论,但通常对于粉碎的磁铁合金粉是0.1mol/kg以上2mol/kg以下、更优选的是0.15~1.5mol/kg、最优选的是0.2~0.4mol/kg。即,若不足0.1mol/kg,由于不能充分进行磁铁粉的表面处理,所以不能改善耐气候性,而且,若在大气中干燥时,进行氧化、放热后磁特性极度降低。若是2mol/kg以上,与磁铁粉的反应激烈溶解磁铁粉。
进而,在本发明中,优选的是将由上述得到的磁铁粉在惰性气体中或真空中、100℃以上400℃以下的温度范围内进行加热处理。若在不足100℃下进行加热处理,磁铁粉的干燥不能充分进行,阻碍稳定的表面被膜的形成,另外,若在400℃以上进行加热处理,有磁铁粉受到热的伤害或矫顽力变得相当低的问题。
可是,在以往的方法中,为了防止磁铁粉的氧化,需要在干燥时,将微量的氧小心地导入到惰性氛围中慢慢进行氧化。为此,必须长时间干燥,这是造成制造成本升高的主要原因。另外,若观察得到的磁铁粉的磁特性的经时变化,虽然在80℃干燥状态下维持比较大的矫顽力,但在80℃相对湿度90%的环境下放置24小时,可降低60%的矫顽力。
另一方面,在本发明的方法中,惊奇地是由于在磁铁合金粉进行粉碎时适量地加入磷酸,可能是在机械化学的作用下在磁铁粉表面形成被膜的原因,在惰性气体中或者真空中进行磁铁粉的干燥的条件以外不需要特别条件,所以可缩短干燥时间。另外,得到的磁铁粉的矫顽力,即使在80℃相对湿度90%的环境下放置24小时也几乎不发生变化,达到大幅度的耐气候性的改善。这样优良的作用效果,至今不清楚其作用机理,完全是意料之外的。
3、粘结磁铁用树脂组合物及粘结磁铁
使用本发明的高耐气候性磁铁粉制造粘结磁铁用树脂组合物及粘结磁铁的方法,没有特别限制,可使用以下公知的热塑性树脂和添加剂来制造。
(热塑性树脂)
热塑性树脂起着磁铁粉粘结剂的作用,没有特别的限制,可使用以往公知的。
作为热塑性树脂的具体例子,可举出尼龙6、尼龙66、尼龙11、尼龙12、尼龙612、芳香族系尼龙、将这些分子一部分改性的改性尼龙等聚酰胺树脂、直链型聚苯硫树脂、交联型聚苯硫树脂、半交联型聚苯硫树脂、低密度聚乙烯、线性低密度聚乙烯树脂、高密度聚乙烯树脂、超高分子量聚乙烯树脂、聚丙烯树脂、乙烯-醋酸乙烯共聚树脂、乙烯-乙基丙烯酸酯共聚树脂、离子型树脂、聚甲基戊烯树脂、聚苯乙烯树脂、丙烯腈-丁二烯-苯乙烯共聚树脂、丙烯腈-苯乙烯共聚树脂、聚氯乙烯树脂、聚偏氯乙烯树脂、聚醋酸乙烯树脂、聚乙烯醇树脂、聚乙烯基丁缩醛树脂、聚乙烯基甲缩醛树脂、甲基丙烯酸树脂、聚偏氟乙烯树脂、聚三氟氯乙烯树脂、四氟乙烯-六氟丙烯共聚树脂、乙烯-四氟乙烯共聚树脂、四氟乙烯-过氟烷基乙烯醚共聚树脂、聚四氟乙烯树脂、聚碳酸酯树脂、聚乙缩醛树脂、聚对苯二甲酸乙二醇酯树脂、聚对苯二甲酸丁二醇酯树脂、聚苯氧树脂、聚烯丙基醚烯丙基砜树脂、聚醚砜树脂、聚醚醚酮树脂、聚芳香族树脂、芳香族聚酯树脂、醋酸纤维素树脂、上述各树脂系弹性体等。这些单聚合物或与其它种单体的无规共聚物、嵌段共聚物、接枝共聚物、用其它物质的末端基改性物等。
这些热塑性树脂的熔融粘度或分子量,最好是对于得到的粘结磁铁在得到所希望的机械强度的范围内是低的。另外,热塑性树脂的形状是粉末状、球状、颗粒状等,没有特别限制,但在与磁铁粉均匀混合这一点上,优选的是粉末状。
热塑性树脂的配合量,对于磁铁粉100重量份,通常是5~100重量份、优选的是5~50重量份。若热塑性树脂的配合量不足5重量份,则组合物的混练阻力(扭矩)变大,流动性降低,成型磁铁困难,另一方面,若超过100重量份,得不到所希望的磁特性。
(其它添加剂)
对于使用本发明的高耐气候性磁铁粉的粘结磁铁用组合物,在不损害本发明目的的范围内,可配合塑料成型用润滑剂或各种稳定剂等其它添加剂。
作为润滑剂,例如可举出石蜡、液体石蜡、聚乙烯蜡、聚丙烯蜡、酯蜡、巴西棕榈蜡、微晶蜡等蜡类、硬脂酸、1,2-氧基硬脂酸、月桂酸、棕榈酸、油酸等脂肪酸类、硬脂酸钙、硬脂酸钡、硬脂酸镁、硬脂酸锂、硬脂酸锌、硬脂酸铝、月桂酸钙、亚油酸锌、蓖麻醇酸钙、2-乙基己糖酸锌等脂肪酸盐(金属皂类)、硬脂酰胺、油酸酰胺、芥酸酰胺、山嵛酸酰胺、棕榈酰胺、月桂酰胺、羟基硬脂酸酰胺、亚甲基双硬脂酸酰胺、乙烯双硬脂酸酰胺、乙烯双月桂酸酰胺、二硬脂基己二酸酰胺、乙烯双油酸酰胺、二油基己二酸酰胺、N-硬脂酰硬脂酸酰胺等脂肪酸酰胺类、硬脂酸丁酯等脂肪酸酯、乙二醇、硬脂醇等醇类、聚乙二醇、聚丙二醇、聚丁二醇及这些改性物组成的聚醚类、二甲基聚硅氧烷、硅酯膏等聚硅氧烷类、氟系油、氟系膏、含氟树脂粉末的氟化合物、氮化硅、碳化硅、氧化镁、氧化铝、二氧化硅、二硫化钼等无机化合物粉体。这些润滑剂,可以一种单独或二种以上组合使用。该润滑剂的配合量,对于磁铁粉100重量份,通常是0.01~20重量份、优选的是0.1~10重量份。
另外,作为稳定剂,可举出双(2,2,6,6-四甲基-4-哌啶基)癸二酸酯、双(1,2,2,6,6-五甲基-4-哌啶基)癸二酸酯、1-[2-{3-(3,5-二叔丁基-4-羟基苯基)丙基氧}乙基]-4-{3-(3,5-二叔丁基-4-羟基苯基)丙基氧}-2,2,6,6-四甲基哌啶、8-苄基-7,7,9,9-四甲基-3-辛基-1,2,3-三氮杂螺[4,5]十一烷基-2,4-二酮、4-苯甲酰氧-2,2,6,6-四甲基哌啶、琥珀酸二甲基-1-(2-羟基乙基)-4-羟基-2,2,6,6-四甲基哌啶缩聚物、聚[[6-(1,1,3,3-四甲基丁基)亚氨基-1,3,5-三嗪-2,4-二基][(2,2,6,6-四甲基-4-哌啶基)亚氨基]六亚甲基[[2,2,6、6-四甲基-4-哌啶基)亚氨基]]、2-(3,5-二叔丁基-4-羟基苄基)-2-正丁基丙二酸双(1,2,2,6,6-戊基甲基-4-哌啶基)等位阻胺系稳定剂,此外,还有苯酚系、磷酸酯系、硫醚系等抗氧化剂等。这些氧化剂可单独也可二种以上组合使用。稳定剂的配合量,对于磁铁粉100重量份,通常是0.01~5重量份、优选的是0.05~3重量份。
另外,上述的各成份的混合方法,没有特别限制,例如可使用螺旋混合机、辊筒混合机、纳塔混合机、偏壳混合机、超级混合机等混合机、或者班伯里混合机、捏合机、辊筒、捏合混合机、单轴挤出机、双轴挤出机等混练机进行。得到的粘结磁铁用组合物形状是粉末状、球状、颗粒状或这些的混合物状,在容易使用这一点上,优选的是颗粒状。
接着,上述粘结磁铁用组合物,在热塑性树脂的熔融温度下加热熔融后,成型为所希望的磁铁形状。此时,作为成型法,可举出以往塑料成型加工等所使用的注射成型法、挤出成型法、注射压缩成型法、注射压入成型法、传递成型法等各种成型法,但在这些中,特别优选的是注射成型法、挤出成型法、注射压缩成型法及注射压入成型法。
实施例
以下,表示本发明的实施例及比较例,但本发明不受这些实施例的任何限制。另外,用于实施例及比较例的各成份的详细情况及评价方法如以下所示。
(1)成份
磁铁合金粉
Sm-Fe-N系磁铁合金粉(住友金属矿山(株)制)、平均粒径:50μm
磷酸
85%浓度水溶液(商品名:磷酸、关东化学(株)制)
(2)评价方法
①矫顽力评价
在80℃相对湿度95%氛围中放置得到的磁铁粉试样1小时~24小时后,用振动试样磁力计在常温下测定矫顽力。
实施例1~6、比较例1、2、4、5
根据表1的记载,在含有所规定的磷酸的乙醇中用介质搅拌磨将磁铁合金粉粉碎2小时后,在真空或氩气中,在室温或所规定的温度下干燥1小时制造磁铁粉。用上述的评价方法评价得到的磁铁粉,得到如表1所示的结果。
比较例3
在乙醇中粉碎磁铁合金粉后,在真空中室温下慢慢地导入氧气,一边进行缓慢氧化,一边使其干燥,制造磁铁粉。用上述的评价方法评价得到的磁铁粉,得到如表1所示的结果。
比较例6
在乙醇中粉碎磁铁合金粉后,根据表1的记载,添加、搅拌所规定量的磷酸。将其在真空中室温下干燥制造磁铁粉。用上述的评价方法评价得到的磁铁粉,得到如表1所示的结果。
表1 80℃相对湿度90%环境下的矫顽力HCJ
磷酸添加量(mol/kg) | pH | 加热温度(℃) | 加热氛围 | 矫顽力HCJ(kOe) | ||
放置1小时 | 放置24小时 | |||||
实施例1 | 0.3 | 3.5 | 室温 | 真空 | 10.5 | 9.2 |
实施例2 | 0.3 | 3.5 | 150 | 氩气 | 10.1 | 10.7 |
实施例3 | 0.3 | 3.5 | 150 | 真空 | 11.4 | 11.3 |
实施例4 | 0.3 | 3.5 | 200 | 真空 | 10.4 | 10.9 |
实施例5 | 0.4 | 2.8 | 150 | 氩气 | 10.0 | 10.1 |
实施例6 | 0.2 | 4.2 | 150 | 氩气 | 10.2 | 10.2 |
对比例1 | 0 | 7 | 室温 | 真空 | 氧化发热,非磁性化 | |
对比例2 | 0.1 | 5.8 | 室温 | 真空 | 氧化发热,非磁性化 | |
对比例3 | 0 | 7 | 室温 | 真空(缓慢氧化) | 10.1 | 2.6 |
对比例4 | 2 | 2.5 | 因磁铁粉溶解而中止粉碎 | |||
对比例5 | 0.3 | 3.5 | 400 | 真空 | 4.0 | 4.0 |
对比例6 | 0.3 | 2.8 | 室温 | 真空 | 10.1 | 6.3 |
从表1表明,用本发明的制造方法得到的磁铁粉,可能是通过与磷酸的反应形成的被膜完全保护了表面的原因,显著地抑制矫顽力的降低,即使取出到大气中也不会氧化、放热。另外,通过加热处理使表面被膜稳定化,进一步抑制矫顽力的降低。
Claims (4)
1.一种高耐气候性磁铁粉的制造方法,通过在有机溶剂中粉碎含有稀土类元素的铁系磁铁合金粉制造磁铁粉,其特正是,在粉碎磁铁合金粉时,在上述有机溶剂中添加磷酸,相对于上述磁铁合金粉,磷酸的添加量是0.1mol/kg以上2mol/kg以下,在粉碎磁铁合金粉后,进而在惰性气体中或真空中,在100℃以上400℃以下的温度范围内进行加热处理。
2.通过权利要求1所述的制造方法得到的高耐气候性磁铁粉。
3.粘结磁铁用树脂组合物,其特征是含有权利要求2所述的高耐气候性磁铁粉作为主成份。
4.粘结磁铁,其特征是成型权利要求3所述的粘结磁铁用树脂组合物而得到的。
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JP3882545B2 (ja) * | 2000-11-13 | 2007-02-21 | 住友金属鉱山株式会社 | 高耐候性磁石粉及びこれを用いた磁石 |
JP4135447B2 (ja) * | 2002-09-17 | 2008-08-20 | 住友金属鉱山株式会社 | 高耐候性磁石粉、ボンド磁石用樹脂組成物及びそれを用いて得られるボンド磁石 |
US7416578B2 (en) | 2004-09-17 | 2008-08-26 | Höganäs Ab | Powder metal composition |
WO2006031193A1 (en) * | 2004-09-17 | 2006-03-23 | Höganäs Ab | Powder metal composition comprising secondary amides as lubricant and/or binder |
CN100487830C (zh) * | 2005-01-18 | 2009-05-13 | 横店集团东磁有限公司 | 注塑铁氧体永磁材料配方 |
US20060234085A1 (en) * | 2005-03-29 | 2006-10-19 | Tdk Corporation | Bonded magnet and process for its manufacture |
CN1808648B (zh) * | 2006-01-19 | 2010-11-10 | 北京科技大学 | 一种稀土粘结磁体的制备方法 |
DE102006019614B4 (de) * | 2006-04-25 | 2010-06-17 | Vacuumschmelze Gmbh & Co. Kg | Alterungsbeständiger Dauermagnet aus einem Legierungspulver und Verfahren zu seiner Herstellung |
CN105742049A (zh) * | 2016-04-29 | 2016-07-06 | 成都锦粼科技有限公司 | 一种铁芯及其制作方法 |
JP6572171B2 (ja) * | 2016-05-26 | 2019-09-04 | 国立大学法人東北大学 | 磁石合金粉の製造方法 |
JP6471724B2 (ja) * | 2016-05-26 | 2019-02-20 | 住友金属鉱山株式会社 | ボンド磁石用磁石合金粉の製造方法 |
CN109655521A (zh) * | 2019-01-28 | 2019-04-19 | 中国地质科学院水文地质环境地质研究所 | 基于加速器质谱技术的14c的快速测量方法 |
JP7460904B2 (ja) * | 2020-06-22 | 2024-04-03 | 愛知製鋼株式会社 | 希土類磁石粉末の製造方法 |
WO2023119612A1 (ja) * | 2021-12-24 | 2023-06-29 | 愛知製鋼株式会社 | 希土類磁石粉末およびその製造方法 |
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US4668283A (en) * | 1984-06-25 | 1987-05-26 | Mitsui Toatsu Chemicals, Incorporated | Magnetic powder and production process thereof |
JPS61263208A (ja) * | 1985-05-17 | 1986-11-21 | Mitsui Toatsu Chem Inc | 磁性成形体の製造方法 |
US5067990A (en) * | 1988-12-22 | 1991-11-26 | Hitachi Metals International, Ltd. | Method of applying phosphate conversion coatings to Fe-R-B substrates, and Fe-R-B articles having a phosphate conversion coating thereon |
US5087302A (en) * | 1989-05-15 | 1992-02-11 | Industrial Technology Research Institute | Process for producing rare earth magnet |
US4933025A (en) * | 1989-10-02 | 1990-06-12 | General Motors Corporation | Method for enhancing magnetic properties of rare earth permanent magnets |
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JPH11251124A (ja) | 1998-03-03 | 1999-09-17 | Sumitomo Metal Mining Co Ltd | 樹脂結合型磁石用組成物 |
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