CN105009229A - 软磁性陶瓷的制造方法及其用途 - Google Patents

软磁性陶瓷的制造方法及其用途 Download PDF

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CN105009229A
CN105009229A CN201480006632.7A CN201480006632A CN105009229A CN 105009229 A CN105009229 A CN 105009229A CN 201480006632 A CN201480006632 A CN 201480006632A CN 105009229 A CN105009229 A CN 105009229A
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卡伦·欧戈尼西安
维斯瓦夫·史崔克
安杰伊·沃基
保罗·格卢霍夫斯基
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INSTYTUT NISKICH TEMPERATUR I BADAN STRUKTURALNYCH
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Abstract

本发明提供一种制造磁性陶瓷的方法，其包括以下步骤：对包含软磁性铁或铁基粉末混合物的粉末组合物进行模具压制，所述粉末的芯颗粒由量占所述组合物的1重量％至35重量％的电绝缘无机涂层包围；在温度和压力低于所述磁性铁或铁基粉末分解温度/压力的气氛中对压制体进行加热和挤压。

Description

软磁性陶瓷的制造方法及其用途
技术领域
本发明涉及一种新的软磁性复合材料——软磁性陶瓷。具体而言，本发明涉及一种制造具有改善的软磁性质的新的软磁性陶瓷的方法及其用途。
背景技术
本发明的软磁性陶瓷属于一类基于软磁性颗粒的(通常是基于铁的)软磁性复合(SMC)材料，其中每个颗粒上具有电绝缘涂层。按照传统的粉末冶金方法，通过将绝缘颗粒与润滑剂和/或粘结剂一起压制来获得SMC。与通常使用钢层板相比，以此方式获得的SMC材料具有较高的自由度。在压制过程中，可获得三维形状的SMC材料，其具有三维磁通。因此，在过去的数十年里对SMC材料的兴趣增加，对SMC材料的软磁特性的改善成为深入研究的课题，以便扩展这些材料的应用。为了实现这种改善，正在不断地开发新的粉末和方法。此外，磁感应的饱和值和电阻率是SMC材料的非常重要的参数。但由于用于改善SMC材料电阻率和硬度的润滑剂和/或粘结剂的高含量，磁感应值在降低。熟知的SMC材料具有的磁感应饱和值为1.2-1.6T，而纯铁的饱和值为约2.2T。本发明的制造方法允许获得同时具有高磁感应饱和值和高电阻率特征的磁性陶瓷。
发明内容
本发明涉及一种用于制造磁性陶瓷的方法，其包括以下步骤：
对包含由软磁性铁或铁基粉末构成的混合物的粉末组合物进行模具压制并挤压成粒料，所述粉末的芯颗粒由量占所述组合物的1重量％至35重量％的电绝缘无机涂层包围；将压制体从模具中弹出；将所述压制体在非还原性气氛中挤压并加热至低于(但接近)所述铁或铁基粉末的分解条件的压力和温度，以及任选地使所述获得的压制体在还原气氛中于介于300℃和600℃之间的温度下经受热处理。
根据本发明，可获得具有优异磁性、电性和机械性质的软磁性陶瓷。这些陶瓷以优异的性质而突出，例如，高磁通饱和值为至少1.6T，磁导率为至少7，非频率依赖性电阻率为至少0.01Ohm-m至高达10MHz，饱和值为2.01T，硬度为至少1GPa(维氏硬度单位)。
发明详述
根据本发明，软磁性粉末由铁构成。优选地，软磁性粉末包含纳米尺寸的羰基铁或基本上纯的铁。根据本发明可使用的优选的电绝缘层为六方氮化硼(BN)的细粉末。
用于铁或铁基粉末中的润滑剂/粘结剂的类型为重要的类型，并且选择BN和TiO2，因为它们能够通过显著改善所得材料的耐腐蚀性和电阻率的薄层来对铁或铁基粉末的颗粒进行充分涂布。使用BN作为润滑剂使得可完全排除导致铁或铁基粉末含量降低的任何粘结剂。
压制可在2GPa-8GPa的压力以及1000℃-2000℃的温度下进行。可在与接近(略低于)铁或铁基粉末分解的条件对应的条件下获得最佳组合物。如果压制在低于2GPa的压力和/或低于1200℃的温度下进行，则所得陶瓷可具有较低的强度。如果压制在与高于分解条件对应的条件下进行，则绝缘层可能被损坏。
此工序降低了所含铁或铁基颗粒中导致磁导率增加的应变。如果退火在低于300℃的温度下进行，则处理时间会长，令人无法接受。另一方面，如果退火在高于600℃的温度下进行，则绝缘层可能被损坏。处理将优选地在惰性气氛(例如氮气、氩气或氦气)中进行。
能够添加另一种润滑剂，例如二氧化钛、石墨、石墨烯、碳化硅、稀土金属和d区元素。添加所提及的材料以允许对所得陶瓷的硬度、电阻率和磁性进行控制。
从以下实施例可看出，可通过根据本发明的方法获得在电阻率、磁感应和磁导率方面具有显著性质的软磁性陶瓷部件。
附图说明
图1示出用于制备软磁性陶瓷的液压机的示意图。“生坯体”意指压制体。
实施例
实施例1
将获自五羰基铁Fe(CO)5的铁与商业六方氮化硼(BN)以不同重量比在玛瑙研钵中进行研磨(1h)。将所得粉末在0.2GPa的压力下冷压。将冷压的粒料“压制体”置于带有石墨加热器的碳酸钙容器(CaCO3)中，然后在1分钟内进行处理。
表1
从表1可看出，在略低于分解条件的条件下获得最佳样品(2/1450,8/1600和8/450)。而施加高温会损坏绝缘层，这导致电阻率降低高达8级(2/1750)。
实施例2
将获自五羰基铁Fe(CO)5的铁与二氧化钛(TiO2)和BN以79:16:5的重量百分比在玛瑙研钵中进行研磨(1h)。将所得粉末在0.2GPa的压力下冷压。将冷压的粒料“压制体”置于带有石墨加热器的碳酸钙容器(CaCO3)中，然后进行处理。
将样品在高压液压机中在4GPa和1450℃下处理1分钟。
表2

Claims (15)

1.一种用于制造软磁性陶瓷部件的方法，其包括以下步骤：
对粉末组合物进行模具压制，所述粉末组合物包含获自五羰基铁Fe(CO)5的铁和BN的混合物；
从模具中弹出压制体；
置于带有石墨加热器的碳酸钙容器(CaCO3)中；
在2-8GPa和1000℃-2000℃下进行烧结处理。
2.根据权利要求1所述的方法，其中所述铁和BN之间的重量百分比关系为至少1:1。
3.根据权利要求1所述的方法，其中分散在BN介质内部的所述铁或铁基粉末颗粒形成陶瓷多晶结构。
4.根据权利要求1所述的方法，其中所述铁或铁基粉末和BN研磨时间至少1小时。
5.根据权利要求1所述的方法，其中所述压制在室温下进行。
6.根据权利要求1所述的方法，其中所述压制在介于0.1GPa和0.2GPa之间的压力下进行。
7.根据权利要求1所述的方法，其中烧结在介于1000℃和2000℃的温度下进行。
8.根据权利要求1所述的方法，其中所述烧结在介于2GPa和8GPa的压力下进行。
9.根据权利要求1所述的方法，其中所述BN绝缘层可以减轻所得陶瓷的腐蚀。
10.根据权利要求1所述的方法，其中所述BN绝缘层可以提高所得陶瓷的电阻率。
11.根据权利要求1所述的方法，其中所得陶瓷的电阻率为至少0.01Ohm-m。
12.根据权利要求1所述的方法，其中可添加二氧化钛、石墨、石墨烯、碳化硅、稀土金属和d区元素。
13.根据权利要求1所述的方法，其中所述铁和BN相对于其他润滑剂的重量百分比关系为至少1:1。
14.根据权利要求1或12所述的方法，其中所述陶瓷具有磁导电阻特性以及至少1.8T的磁感应饱和值。
15.一种磁性陶瓷，其可在高频应用中用作感应器，电磁吸收器和滤波器部件。
CN201480006632.7A 2013-01-29 2014-01-27 软磁性陶瓷的制造方法及其用途 Pending CN105009229A (zh)

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