CN114736010B - 一种高熵氧化物陶瓷及其制备方法和作为电磁波吸收材料的应用 - Google Patents
一种高熵氧化物陶瓷及其制备方法和作为电磁波吸收材料的应用 Download PDFInfo
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Abstract
本发明属于电磁波吸收材料技术领域，具体涉及一种高熵氧化物陶瓷及其制备方法和作为电磁波吸收材料的应用。分子式为(Fe0.2Co0.2Ni0.2Cu0.2Zn0.2)O/Fe2O4，具有两种晶型：岩盐型和尖晶石型。制备步骤如下：（1）、选取FeO、CoO、NiO、CuO、ZnO作为原料，称取FeO、CoO、NiO、CuO、ZnO粉体的摩尔比为1∶1∶1∶1∶1，混合均匀，获得混合粉体；（2）、将步骤（1）制备好的混合粉体压制成圆片生坯，空气气氛下控温在1200‑1300℃煅烧10‑12h，取出煅烧产物即得高熵氧化物陶瓷。本发明以氧化亚铁、氧化钴、氧化镍、氧化铜、氧化锌为原料，进行煅烧，获得高纯度、强吸波性能、宽吸收频带的高熵氧化物陶瓷，经分析表明制备得到的高熵氧化物陶瓷的最小反射损耗值为‑52.3dB。
Description
技术领域
本发明属于电磁波吸收材料技术领域，具体涉及一种高熵氧化物陶瓷及其制备方法和作为电磁波吸收材料的应用。
背景技术
随着电磁波的应用与发展，电磁波给人们带来了很大的便利。例如，手机通话、网上聊天等。但是，电磁波是一把双刃剑，在使用电磁波的同时，还伴随着电磁波辐射的困扰。长期暴露在电磁辐射中对人体健康有害，会引起恶心、头痛、眼病等症状,以及对婴儿大脑发育有不利的影响。在机场，航班可能因电磁波干扰无法起飞；在医院，移动电话常会干扰各种电子诊疗仪器的正常工作。此外，在军事领域，出于雷达隐身的需要，飞行器需要避开电磁波的作用。因此需要研发吸波材料来对电磁波信号进行吸收。随着技术的发展，吸波材料不仅需要有“薄、轻、宽、强”的特点，还要有环境适应性、耐高温、抗氧化等特点。但是，传统的吸波材料中磁性材料较多，其缺点是质量大，在高温下容易失去磁性，严重影响其高温吸波性能。
高熵陶瓷具有“高熵效应”、“晶格畸变效应”、“迟滞扩散效应”和“鸡尾酒效应”，这四种效应使高熵陶瓷具有耐高温、抗氧化等特点，并且还具有良好的性能调控空间，有利于通过不同金属的加入对其性能进行大范围的控制，但目前关于高熵氧化物成分与电磁吸收性能的文章还比较少。
发明内容
本发明的目的在于提供一种高熵氧化物陶瓷及其制备方法和作为电磁波吸收材料的应用。
为实现上述目的，本发明采取的技术方案如下：
一种高熵氧化物陶瓷，分子式为(Fe0.2Co0.2Ni0.2Cu0.2Zn0.2)O/Fe2O4，具有两种晶型：岩盐型和尖晶石型。
所述高熵陶瓷的制备方法，制备步骤如下：
（1）、选取FeO、CoO、NiO、CuO、ZnO作为原料，称取FeO、CoO、NiO、CuO、ZnO粉体的摩尔比为1∶1∶1∶1∶1，混合均匀，获得混合粉体；
（2）、将步骤（1）制备好的混合粉体压制成圆片生坯，空气气氛下控温在1200-1300℃煅烧10-12h，取出煅烧产物即得高熵氧化物陶瓷。
较好地，步骤（1）中，所述FeO、CoO、NiO、CuO、ZnO粉体原料粒径均为1-2mm。
较好地，步骤（1）中，采用湿法球磨的方式将所有金属氧化物原料混合均匀；球磨后，将浆体干燥，得到混合粉体。
较好地，湿法球磨时，添加的球磨珠与所有金属氧化物原料总量的质量比为（5-10）∶1，研磨助剂是无水乙醇，转速为250-300 r/min。
较好地，干燥温度为60-80℃、干燥时间为2-4 h。
较好地，球磨后，所述混合粉体的粒径为0.1-0.5mm。
较好地，步骤（2）中，压制的压力为50-100MPa，持续时间为60-90s。
较好地，步骤（2）中，以5-10℃/min的速率升温至煅烧温度。
较好地，所述高熵氧化物陶瓷作为电磁波吸收材料的应用。
本发明中，煅烧温度和时间主要影响陶瓷材料的纯度，烧结温度过低且低于上述范围的最小值，则无法得到高纯度的高熵氧化物陶瓷，时间过短且短于上述范围的最小值时，也无法得到高纯度的高熵氧化物陶瓷。
有益效果：
（1）、本发明以氧化亚铁、氧化钴、氧化镍、氧化铜、氧化锌为原料，进行煅烧，获得高纯度、强吸波性能、宽吸收频带的高熵氧化物陶瓷，经分析表明制备得到的高熵氧化物陶瓷的最小反射损耗值为-52.3dB；
（2）、本发明提供的一种高熵氧化物陶瓷的制备方法，工艺简单、快速、实用性强，制备得到的高熵氧化物陶瓷具有耐高温、纯度高、吸波性能强、吸收频带宽等优点。
附图说明
图1：实施例1制得的高熵氧化物陶瓷的XRD图。
图2：实施例1制得的高熵氧化物陶瓷的SEM图。
图3：对照例样品的XRD图。
图4：对照例样品的SEM图。
图5：实施例1制得的高熵氧化物陶瓷的吸波性能曲线。
图6：对照例样品的吸波性能曲线。
具体实施方式
为使本发明更加清楚、明确，以下对本发明进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。
实施例1
一种高熵氧化物陶瓷的制备方法，步骤如下：
（1）、按照摩尔比为1∶1∶1∶1∶1分别称取0.18mol FeO（12.933g）、0.18mol CoO（13.4874g）、0.18mol NiO（13.444g）、0.18mol CuO（14.319g）、0.18mol ZnO（14.6538g），共68.8372g，一起置于球磨机中，加入400g球磨珠和适量的无水乙醇，250 r/min转速下搅拌成糊状，用球磨机室温下球磨8h，放入干燥箱中升温至70℃，保温干燥3h，得混合粉体，其中混合粉体的粒径为0.2mm；
（2）、称取步骤（1）制备好的混合粉末8g，放入直径为30mm的圆形模具中，用压片机施以70MPa的压力，持续时间为90s，得到圆片生坯；
（3）、将步骤（2）所得圆片生坯放入马弗炉中，空气气氛下以10℃/min的速率升温至煅烧温度1200℃，煅烧12h，取出煅烧产物即得高熵氧化物陶瓷。
制得的高熵氧化物陶瓷的XRD图和SEM图分别如图1和2所示，所得的高熵氧化物陶瓷具有两种晶型：岩盐型和尖晶石型，所得的高熵氧化物陶瓷的平均粒径为25mm。
实施例2
与实施例1的区别在于：步骤（1）中，按照摩尔比为1∶1∶1∶1∶1分别称取0.025molFeO（1.79625g）、0.025mol CoO（1.87325g）、0.025mol NiO（1.86725g）、0.025mol CuO（1.98875g）、0.025mol ZnO（2.03525g），共9.56075g，加入50g球磨珠和适量的无水乙醇；其它均同实施例1。
实施例3
与实施例1的区别在于：步骤（3）中，煅烧温度为1250℃；其它均同实施例1。
实施例4
与实施例1的区别在于：步骤（3）中，煅烧温度为1300℃；其它均同实施例1。
对照例
与实施例1的区别在于：步骤（3）中，煅烧温度为1100℃；其它均同实施例1。
该对照例所得产品的XRD图、SEM图分别见图3和图4。XRD图显示：在1100℃下合成的高熵氧化物陶瓷，也具有岩盐型与尖晶石型结构，且与PDF卡片都对应上，但是相比于实施例1的样品，它的尖晶石相的峰强并不高；同时，SEM图显示样品的晶粒尺寸较小，且有大量气孔，与实施例1的样品相比，它的致密度不高。
电磁波吸收性能的研究：
取实施例1和对照例制得的高熵氧化物陶瓷作为样品，利用矢量网络分析仪(VNA，Agilent N5234A，8.2-12.4GHz) 对材料进行介电性能和电磁性能的分析。具体做法是：先将圆形块体切割为长22.86mm、宽10.16mm的长方体陶瓷，用自动磨抛机打磨精确。利用矢量网络分析仪模拟测试不同厚度样品的吸波性能。
实施例1和对照例制得的高熵氧化物陶瓷的吸波性能曲线，分别如图5和图6所示，图例中的数字代表网络矢量分析仪所模拟的样品厚度。由图5可知：高熵氧化物陶瓷展示出优异的电磁吸波性能，其中最大反射损耗在吸波涂层厚度仅为2.2mm时，达到-52.3 dB，反射率在-10dB以下时最大吸收频带宽为3.2GHz。由图6可知：在8.2-12.4GHz内，样品的吸波性能较差，不同厚度下的反射损耗值均在-10 dB以上。
Claims (9)
1.一种高熵氧化物陶瓷，其特征在于：分子式为(Fe0.2Co0.2Ni0.2Cu0.2Zn0.2)O/Fe2O4，具有两种晶型：岩盐型和尖晶石型；所述高熵氧化物陶瓷按照下述制备步骤获得：
（1）、选取FeO、CoO、NiO、CuO、ZnO作为原料，称取FeO、CoO、NiO、CuO、ZnO粉体的摩尔比为1∶1∶1∶1∶1，混合均匀，获得混合粉体；
（2）、将步骤（1）制备好的混合粉体压制成圆片生坯，空气气氛下控温在1200℃煅烧10-12h，取出煅烧产物即得高熵氧化物陶瓷；压制的压力为50-100MPa，持续时间为60-90s。
2.一种如权利要求1所述的高熵氧化物陶瓷的制备方法，其特征在于，制备步骤如下：
（1）、选取FeO、CoO、NiO、CuO、ZnO作为原料，称取FeO、CoO、NiO、CuO、ZnO粉体的摩尔比为1∶1∶1∶1∶1，混合均匀，获得混合粉体；
（2）、将步骤（1）制备好的混合粉体压制成圆片生坯，空气气氛下控温在1200℃煅烧10-12h，取出煅烧产物即得高熵氧化物陶瓷；压制的压力为50-100MPa，持续时间为60-90s。
3.如权利要求2所述的高熵氧化物陶瓷的制备方法，其特征在于：步骤（1）中，所述FeO、CoO、NiO、CuO、ZnO粉体原料粒径均为1-2mm。
4.如权利要求2所述的高熵氧化物陶瓷的制备方法，其特征在于：步骤（1）中，采用湿法球磨的方式将所有金属氧化物原料混合均匀；球磨后，将浆体干燥，得到混合粉体。
5. 如权利要求4所述的高熵氧化物陶瓷的制备方法，其特征在于：湿法球磨时，添加的球磨珠与所有金属氧化物原料总量的质量比为（5-10）∶1，研磨助剂是无水乙醇，转速为250-300 r/min。
6. 如权利要求4所述的高熵氧化物陶瓷的制备方法，其特征在于：干燥温度为60-80℃、干燥时间为2-4 h。
7.如权利要求4所述的高熵氧化物陶瓷的制备方法，其特征在于：球磨后，所述混合粉体的粒径为0.1-0.5mm。
8.如权利要求2所述的高熵氧化物陶瓷的制备方法，其特征在于：步骤（2）中，以5-10℃/min的速率升温至煅烧温度。
9.一种如权利要求1所述的高熵氧化物陶瓷作为电磁波吸收材料的应用。
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