CN100411071C - 粘合磁体及制造该粘合磁体的方法 - Google Patents

粘合磁体及制造该粘合磁体的方法 Download PDF

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CN100411071C
CN100411071C CNB2004800018264A CN200480001826A CN100411071C CN 100411071 C CN100411071 C CN 100411071C CN B2004800018264 A CNB2004800018264 A CN B2004800018264A CN 200480001826 A CN200480001826 A CN 200480001826A CN 100411071 C CN100411071 C CN 100411071C
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千田正康
末永真一
片山英纪
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Nippon Bengara Kogyo Co Ltd
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Abstract

一种用于用橡胶基树脂作为粘合剂加以粘合的粘合磁体的铁氧体磁粉,该磁粉是含有碱土金属的铁氧体磁粉,氯含量为0.05wt%或者更少,粉末pH小于6。该磁粉的制造是通过粉碎含有碱土金属的铁氧体成分煅烧产品,对粉碎后的铁氧体成分进行退火以减轻结晶应变,将退火后粉末分散在水基介质中并用无机酸加以中和,向其中添加分散剂,和对分散物进行固液分离,随后进行真空干燥。从而获得氯含量为0.05wt%或者更少,粉末pH小于6的铁氧体磁粉。

Description

粘合磁体及制造该粘合磁体的方法
技术领域
本发明涉及用于用橡胶基树脂粘合剂加以粘合的粘合磁体(bonded magnet)的铁氧体磁粉及制造该磁粉的方法。
背景技术
利用橡胶基树脂作为粘合剂的橡胶基粘合磁体的磁特性不仅受到所用磁粉的特性的强烈影响,还受到橡胶基粘合剂中磁粉的填充速度的强烈影响。尽管橡胶基粘合剂中磁粉的填充速度受到各种因素的影响,包括磁粉的颗粒直径和颗粒尺寸分布、颗粒的形状和表面构型以及橡胶基粘合剂的类型,但是对于磁粉而言最主要的是与橡胶基粘合剂具有高的相容性而不改变其固有性质。在本说明书中,磁粉的这种不降低橡胶基粘合剂固有性质的性质被称作“磁粉非反应性”,其与橡胶基粘合剂的相容性被称作“磁粉亲和性”。
如果磁粉的非反应性和亲和性较差,则在与橡胶基粘合剂揉合(kneading)时或者在形成混合物时,粘度会变得较高而流动性较低。结果,磁颗粒会受到机械应力。由于施加机械应力导致的磁颗粒应变增加,使得磁粉的矫顽力降低。
铁氧体磁粉的非反应性和亲和性能够通过例如测量混合物的粘度和/或切应力加以估计。可以认为,粘度和/或切应力越小,相对于树脂的非反应性和亲和性(相容性)越好。
JP 2001-160506A(‘506)讲授,碳含量为0.010-0.040wt%,pH为6与小于9之间的铁氧体磁粉能够通过如下方法获得:粉碎由铁氧体构成的煅烧产品,对产物进行退火从而获得pH不小于9的铁氧体磁粉,将粉末悬浮在水中并向悬浮物中吹入二氧化碳气体。该产品据称与树脂基粘合剂具有优良的非反应性和亲和性。参考文献‘506进一步讲授,通过添加无机酸(mineral acid)进行中和而不是吹入二氧化碳气体,干燥产品中出现的黏着会使得必须进行相当强的碾碎处理,在这种情况下,完全避免内应力的产生是很困难的。
日本专利No.3294507讲授,碳含量为0.015-0.080wt%,pH为7-10的铁氧体磁粉能够通过如下方法获得:在搅动下,使退火后的铁氧体磁粉与CO2源接触。该产品据称与树脂基粘合剂具有优良的非反应性和亲和性。
发明内容
橡胶基粘合磁体的一个特点是,其韧性(toughness)使得它能够被高度自由地安装在设备上。例如,薄片状(sheet-like)橡胶基粘合磁体能够曲率一致地安装在一个弯曲的部分上。粘合磁体的弹性(韧性)会由于磁粉的性质而恶化。关于磁粉导致橡胶基粘合磁体经历这种模制部件劣化(degradability)的原因,目前还没有报道。
在橡胶基粘合磁体实例中,当通过加工成预定构型获得的模制部件经历韧性退变或者形状改变时,通常会发生磁性能劣化。在下列情况下,例如利用橡胶基粘合磁体的性质沿着一个弯曲表面弯曲地安装薄片状模制部件时,如果发生破裂,则粘合磁体本身的性能会降低。对于用磁粉进行粘合磁体塑模(molding)之后能够延续多长的寿命,还没有过测量。
因此,本发明致力于阐明在模制粘合磁体之后磁粉导致产品磁性能降低的原因,并且为橡胶基粘合磁体提供一种除去了该原因的铁氧体磁粉。
已经发现,这个目标能够通过一种含有碱土金属的铁氧体磁粉加以实现,该铁氧体磁粉的氯含量为0.05wt%或更少,粉末的pH小于6。这种磁粉能够通过如下方法获得:粉碎含有碱土金属的铁氧体成分煅烧产品,将粉碎的铁氧体成分退火从而减轻结晶应变,将退火后的粉末分散在水中并用无机酸加以中和,向其中添加分散剂,并对分散物进行固液分离随后进行真空干燥。已经发现,在真空干燥期间,添加分散剂比不添加分散剂的黏着预防效应更高。
本发明提供一种粘合磁体,通过将铁氧体磁粉粘合于橡胶基树脂获得,该铁氧体磁粉含有碱土金属,氯含量为0.05wt%或者更少,粉末pH小于6。
根据本发明的上述粘合磁体,其中橡胶基树脂至少是丁晴橡胶和三元乙丙橡胶中的一种。
根据本发明的上述粘合磁体,其中橡胶基树脂是氯化聚乙烯。
本发明还提供一种制造上述粘合磁体的方法,包括:粉碎含有碱土金属的铁氧体成分的煅烧产品;对粉碎后的铁氧体成分进行退火以减轻晶体应变;将退火后的粉末分散在水基介质中并用无机酸加以中和;向其中添加分散剂;对分散物进行固液分离,随后进行真空干燥;将获得的铁氧体磁粉末与橡胶基粘合剂揉合以获得一种混合物;以及将该混合物成形为指定的构型。
附图说明
在图1中,比较了不同混合物中粘度和切应力随剪切速率的变化,即把通过混合根据本发明的铁氧体磁粉与橡胶基粘合剂获得的混合物与参考实例和比较实例进行比较。
具体实施方式
铁氧体磁粉的组成和颗粒形状有相当大的不同。其干法制造过程一般包括如下步骤:混合起始材料——制粒——煅烧——碾碎——冲洗和脱水——干燥——碾碎——退火——产品。最终的“退火”步骤用于减轻在煅烧后的粉碎期间(以及干燥后的碾碎期间)产生的结晶应力。在碾碎和/或粉碎期间产生的结晶应力需要被减轻,因为它会降低产品的磁性质,特别是其矫顽力。通过该退火步骤之后,铁氧体磁粉的pH为10-12,也就是显强碱性。这种pH值的上升在含有碱土金属的铁氧体磁粉实例中特别明显。
当铁氧体磁粉显示出这种强碱性时,会劣化橡胶基粘合剂,并对混合物的粘度和流动性产生显著的副作用。此外,在经过退火步骤之后的铁氧体磁粉中发现了来自于添加剂和起始材料的残余杂质成分及类似物。这些残余成分可能是导致橡胶基粘合磁体在揉合/成型之后劣化的原因。在这些成分中,发现氯具有特别坏的效应。
在本发明中,退火后的铁氧体磁粉首先被悬浮在水中,优选地加以充分搅拌,并添加无机酸。该处理将通过磁粉带来的氯降低到了一个基本上无害的水平。而且,已经发现通过将粉末pH降低到6之下,防止了模制橡胶基粘合磁体部件的质量降低。
尽管用无机酸中和退火后的粉末悬浮物在固液分离之后的干燥过程中会趋向于黏着,但是已经发现,干燥期间的黏着能够通过执行适当的黏着预防处理加以避免。通常使用的预防黏着的处理可以包括添加几乎没有吸附的水(adsorbed water)的无机物质,添加脂肪酸酰胺(fatty acid amide)、氟化脂肪酸或者其他的这类抗粘着剂,以及用硅石型表面处理剂(silica type surface treatment agent)或表面活性剂进行表面处理。然而,根据本发明的黏着预防处理是通过在干燥步骤之前添加分散剂(表面活性剂)并在固液分离之后在降低的压力下进行干燥步骤。
这样,在将退火后的铁氧体磁粉进行湿处理之后获得的干燥产品的氯含量变成0.05%wt或者更少,优选地为0.02%wt或者更少,粉末的pH变得小于6。结果与橡胶基粘合剂的非反应性和亲和性优异,并能够提高模制部件的弯曲强度。结果,橡胶基粘合磁体的特性能够长时间保持。
这里参考的铁氧体磁粉pH值的测量与JIS K 5101的测量方法一致。尽管能够应用本发明的铁氧体磁粉的成分并没有特别的限制,但是将本发明应用于含有碱土金属的铁氧体磁粉是特别有利的。用于粘合铁氧体磁粉的粘合剂也没有特别地限制在橡胶基粘合剂范围内。有可能使用,例如,可硫化的橡胶如NBR(丁晴橡胶)(acrylonitrilebutadiene copolymer rubber)或者EPDM(三元乙丙橡胶)(ethylenepropylene diene monomer rubber),或者具有橡胶弹性的热塑性树脂如CPE(氯化聚乙烯)(chlorinated polyethylene)、塑化PVC(聚氯乙烯)(plasticized poly vinyl chloride)或EVA(乙烯醋酸乙烯共聚物)(ethylene vinyl acetate copolymer)。还可能使用氯磺化聚乙烯、硅氧橡胶或类似物。
实例
实例1
称量氧化铁与碳酸锶并以5.75的摩尔比进行混合,产物用水制粒,并且在干燥之后于炉中在1290℃下煅烧4小时。粗略碾碎煅烧后的产品,然后用湿磨(wet mill)进行湿粉碎从而获得平均颗粒直径为1.4μm的锶铁氧体磁粉。该磁粉于炉中在980℃下退火1小时。所得的退火后产品含氯0.055wt%,通过JIS K5101的方法测得其pH为10.22。12,000g粉末用水混合从而获得浆浓度为25wt%的悬浮物。在搅拌下向悬浮物添加硫酸,从而使悬浮物中硫酸的浓度为0.10%,之后继续搅拌15分钟。通过移注(decantation)进行水冲洗,添加surfynolCT151(Nissin有限公司产品)作为分散剂,其添加量相对于铁氧体磁粉的浓度为0.25%。再搅拌10分钟。对产物进行脱水,并且在降低的压力下干燥所得的块状物,然后用高速搅拌型破碎机加以碾碎从而获得平均颗粒直径为1.4μm的锶铁氧体磁粉。化学地分析所得的磁粉。检测到不超过0.01wt%的氯。测量pH发现为4.9。
136.1g所得磁粉与13.5g的NBR注入到LaboPlast磨(Toyoseiki公司)中,在80℃下造粒10分钟,卸载一次,然后在相同条件下再次造粒。将所得的造粒产物用6英寸轧辊滚压成薄片,并切割薄片从而获得多个厚3mm、宽2mm、长50mm的样品(用于亲和性评估),和一个厚3mm、宽20mm、长50mm的样品(用于模制成分劣化评估)。
通过用capillograph(Toyoseike公司)测量剪切速度(SR)、粘度和切应力估计亲和性。测量结果如图1所示。图1横轴的刻度是剪切速度(sec-1),纵轴是粘度(PaS)和切应力(Pa),显示出粘度和切应力随着剪切速度变化而变化。作为对比,图1还显示了对磁粉在退火阶段的亲和性的类似估计(如前所述,其氯含量为0.055wt%,pH为10.22;该磁粉称作参考实例)。
从图1所示的结果能够看出,与参考实例相比,实例1的磁粉在制粒橡胶混合物产品中显示具有低粘度和切应力值,以及与橡胶基粘合剂的良好的亲和性。
通过将薄片在100℃下保持5天,将它们冷却到室温,然后对它们施加弯曲力,其中每个薄片围绕一个22mm直径的圆柱体卷曲,来估计模制成分的劣化性。薄片表面的破裂程度被归为3个等级。用本实例磁粉的薄片的劣化性等级为A,而用退火阶段磁粉(参考实例)的等级为C。
A:任何地方均观察不到裂纹;
B:观察到的裂纹长度小于3mm;
C:观察到的裂纹长度大于等于3mm,宽度大于等于0.1mm。
比较实例
与实例1是重复的,只是在添加硫酸时,硫酸的浓度从0.10%改变到0.05%。所得的磁粉加以化学地分析。检测到的氯含量不超过0.01wt%,粉末pH为6.6。
该比较实例的粉末进行如实例1的亲和性估计。结果如图1所示。粉末也进行如实例1的模制成分劣化试验。其等级为B。
如前面解释的,本发明提供了一种在非反应性和与橡胶基粘合剂的亲和性方面优异的铁氧体磁粉。利用该磁粉的橡胶基粘合磁体的模制部件韧性优异,不出现裂纹或类似的处于弯曲变形状态的情况。这样,本发明提供了一种突出的效应,防止了作为橡胶基粘合磁体特征的可塑性的损失。

Claims (4)

1. 一种粘合磁体,通过将铁氧体磁粉粘合于橡胶基树脂或具有橡胶弹性的热塑性树脂获得,该铁氧体磁粉含有碱土金属,氯含量为0.05wt%或者更少,粉末pH小于6。
2. 根据权利要求1的粘合磁体,其中橡胶基树脂是丁晴橡胶和三元乙丙橡胶中的至少一种。
3. 根据权利要求1的粘合磁体,其中具有橡胶弹性的热塑性树脂是氯化聚乙烯。
4. 一种制造权利要求1-3中任一项的粘合磁体的方法,包括:
粉碎含有碱土金属的铁氧体成分的煅烧产品;
对粉碎后的铁氧体成分进行退火以减轻晶体应变;
将退火后的粉末分散在水基介质中并用无机酸加以中和;
向其中添加分散剂;
对分散物进行固液分离,随后进行真空干燥;
将获得的铁氧体磁粉末与橡胶基粘合剂揉合以获得一种混合物;以及
将该混合物成形为指定的构型。
CNB2004800018264A 2003-02-14 2004-02-13 粘合磁体及制造该粘合磁体的方法 Expired - Fee Related CN100411071C (zh)

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