CN115594496B - 一种具有尖晶石结构的中熵陶瓷及其制备方法 - Google Patents

一种具有尖晶石结构的中熵陶瓷及其制备方法 Download PDF

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CN115594496B
CN115594496B CN202211352421.1A CN202211352421A CN115594496B CN 115594496 B CN115594496 B CN 115594496B CN 202211352421 A CN202211352421 A CN 202211352421A CN 115594496 B CN115594496 B CN 115594496B
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entropy ceramic
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CN115594496A (zh
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杨玉杰
陈丛亮
陈冬阳
张英明
孟雨亭
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Anhui University
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Abstract

本发明提供一种具有尖晶石结构的中熵陶瓷及其制备方法，涉及陶瓷材料技术领域。所述具有尖晶石结构的中熵陶瓷的化学式为(Me)3O4，化学式中的Me为四种摩尔比相等的金属元素，其制备方法为将原料球磨后经过两次无压烧结制备最终的目标材料，本发明克服了现有技术的不足，制备工艺具有成本低、操作简单、制备周期短等特点，且获得的中熵陶瓷材料在磁学领域有良好的应用前景。

Description

一种具有尖晶石结构的中熵陶瓷及其制备方法
技术领域
本发明涉及陶瓷材料技术领域，具体涉及一种具有尖晶石结构的中熵陶瓷及其制备方法。
背景技术
最初熵稳定材料在高熵合金中得到广泛的应用，高熵陶瓷的概念也继承自该领域。高熵氧化物的概念在2015年被提出。因为熵稳定材料的晶体结构具有高度无序的特征，所以其结构更加稳定。而高熵氧化物属高熵陶瓷的一种，高熵陶瓷指的是一个或多个威考夫位点被5个或5个以上相同或相似比例的元素占据的陶瓷材料。
高熵陶瓷独特的结构使其在许多领域都表现出优异的的性能，如：力学性能、导热性能、储能性能、磁性能等。然而，当材料形成的摩尔焓很小时，即使占据一个或多个威考夫位点的元素数量小于5个，也可以形成熵稳定的材料。
随着熵稳定材料研究的不断深入，当一个或多个威考夫位点被三种或四种离子占据时，也能形成稳定的氧化物，这类陶瓷被称为中熵陶瓷。
中熵陶瓷有着和高熵陶瓷类似的特性，目前中熵陶瓷的研究主要集中在电化学、光学、导热、电学等方向上，然而关于中熵陶瓷磁性的研究较少。
发明内容
针对现有技术不足，本发明提供一种具有尖晶石结构的中熵陶瓷及其制备方法，设计开发中熵陶瓷，使其能够有效应用在磁学领域，提升材料的应用价值，同时提升材料加工的便捷性，降低应用成本。
为实现以上目的，本发明的技术方案通过以下技术方案予以实现：
一种具有尖晶石结构的中熵陶瓷，所述具有尖晶石结构的中熵陶瓷的化学通式为(Me)3O4。
优选的，所述Me为四种等摩尔比的金属元素。
一种具有尖晶石结构的中熵陶瓷的制备方法包括以下步骤：
(1)原料预处理：按照金属离子摩尔比称取四种金属氧化物，并将金属氧化物的粉末置于球磨仪中充分球磨混合得浆料，后将浆料烘干，得球磨原料备用；
(2)初次烧结：将上述球磨原料置于马弗炉，加热至700℃-1450℃进行保温烧结，后取出研磨粉碎，得预制粉料备用；
(3)二次烧结：将上述预制粉料置入马弗炉在800℃-1450℃下进行第二次烧结，得到具有尖晶石材料的中熵陶瓷粉末。
优选的，所述步骤(1)中球磨仪混合的方式为将金属氧化物粉末置入盛有蒸馏水的球磨仪中，以150-250r/min的转速充分混合5-10小时。
优选的，所述步骤(2)中加热至700℃-1450℃的升温速度为3.5-4℃/min。
优选的，所述步骤(2)中研磨粉碎的粉末需过80目筛。
优选的，所述步骤(3)中第二次烧结保温的时间为10h。
优选的，所述步骤(3)获得的具有尖晶石材料的中熵陶瓷粉末后期将粉末压型后烧结，并应用于吸波或软磁方向。
本发明提供一种具有尖晶石结构的中熵陶瓷及其制备方法，与现有技术相比优点在于：设置处一种能够在磁学领域进行有效应用的中熵陶瓷材料，其能够具有优良的磁学性能，同时在整个材料的加工生产过程操作简单、制备成本低、周期短，能够有效提升生产的经济效益和生产价值。
附图说明：
图1(a)为本发明实施例1中熵陶瓷粉体的XRD图；图1(b)为本发明实施例2中熵陶瓷粉体的XRD图；图1(c)为本发明实施例3中熵陶瓷粉体的XRD图；图(d)为本发明实施例4中熵陶瓷粉体的XRD图；
图2为本发明实施例1的中熵陶瓷的SEM图；
图3为本发明实施例1的中熵陶瓷粉体的M-H图；
图4为本发明实施例2的中熵陶瓷的SEM图；
图5为本发明实施例2的中熵陶瓷粉体的M-H图；
图6为本发明实施例3的中熵陶瓷的SEM图；
图7为本发明实施例3的中熵陶瓷粉体的M-H图；
图8为本发明实施例4的中熵陶瓷的SEM图；
图9为本发明实施例4的中熵陶瓷粉体的M-H图。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚，下面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，都属于本发明保护的范围。
实施例1：
制备化学式为(Mn0.25Fe0.25Mg0.25Zn0.25)3O4的中熵陶瓷：
(1)选取Mn3O4、Fe2O3、MgO、ZnO为原料，按照所述化学式称取等金属摩尔比的原料粉末，并将称取的原料粉末放入盛有100ml蒸馏水的球磨罐中，加入钢球进行球磨；设置球磨罐转速为250r/min，球磨7小时后取出，将充分混合后的浆料置入烘箱内烘干获得球磨原料；
(2)将上述球磨原料置入马弗炉，设置每分钟升温速度为3.5℃-4℃，将球磨原料加热至890℃并保温1.5小时进行第一次烧结，后取出第一次烧结得到的粉末置入研钵破碎，将破碎后的粉末过80目筛，筛出颗粒较小的粉末为预制粉料；
(3)将上述预制粉料置入马弗炉在1200℃下进行第二次烧结，保温10小时，获得具有尖晶石材料的中熵陶瓷粉末。
实施例2：
制备化学式为(Mn0.25Fe0.25Mg0.25Co0.25)3O4的中熵陶瓷：
(1)选取Mn3O4、Fe2O3、MgO、Co3O4为原料，按照所述化学式称取等金属摩尔比的原料粉末，并将称取的原料粉末放入盛有100ml蒸馏水的球磨罐中，加入钢球进行球磨；设置球磨罐转速为250r/min，球磨7小时后取出，将充分混合后的浆料置入烘箱内烘干获得球磨原料；
(2)将上述球磨原料置入马弗炉，设置每分钟升温速度为3.5℃-4℃，将球磨原料加热至890℃并保温1.5小时进行第一次烧结，后取出第一次烧结得到的粉末置入研钵破碎，将破碎后的粉末过80目筛，筛出颗粒较小的粉末为预制粉料；
(3)将上述预制粉料置入马弗炉在1200℃下进行第二次烧结，保温10小时，获得具有尖晶石材料的中熵陶瓷粉末。
实施例3：
制备化学式为(Mn0.25Fe0.25Mg0.25Ni0.25)3O4的中熵陶瓷：
(1)选取Mn3O4、Fe2O3、MgO、NiO为原料，按照所述化学式称取等金属摩尔比的原料粉末，并将称取的原料粉末放入盛有100ml蒸馏水的球磨罐中，加入钢球进行球磨；设置球磨罐转速为250r/min，球磨7小时后取出，将充分混合后的浆料置入烘箱内烘干获得球磨原料；
(2)将上述球磨原料置入马弗炉，设置每分钟升温速度为3.5℃-4℃，将球磨原料加热至890℃并保温1.5小时进行第一次烧结，后取出第一次烧结得到的粉末置入研钵破碎，将破碎后的粉末过80目筛，筛出颗粒较小的粉末为预制粉料；
(3)将上述预制粉料置入马弗炉在1200℃下进行第二次烧结，保温10小时，获得具有尖晶石材料的中熵陶瓷粉末。
实施例4：
制备化学式为(Mn0.25Fe0.25Ni0.25Co0.25)3O4的中熵陶瓷：
(1)选取Mn3O4、Fe2O3、NiO、Co3O4为原料，按照所述化学式称取等金属摩尔比的原料粉末，并将称取的原料粉末放入盛有100ml蒸馏水的球磨罐中，加入钢球进行球磨；设置球磨罐转速为250r/min，球磨7小时后取出，将充分混合后的浆料置入烘箱内烘干获得球磨原料；
(2)将上述球磨原料置入马弗炉，设置每分钟升温速度为3.5℃-4℃，将球磨原料加热至890℃并保温1.5小时进行第一次烧结，后取出第一次烧结得到的粉末置入研钵破碎，将破碎后的粉末过80目筛，筛出颗粒较小的粉末为预制粉料；
(3)将上述预制粉料置入马弗炉在1200℃下进行第二次烧结，保温10小时，获得具有尖晶石材料的中熵陶瓷粉末。
检测：
对上述实施例1-4所制得的中熵陶瓷进行检测：
1、通过XRD确定实施例1-4中制备的中熵陶瓷具有尖晶石结构(Fd-3m)，即将实施例1-4制得的中熵陶瓷X射线衍射图谱图与MgFe2O4(PDF#88-1937)的衍射峰对比发现该陶瓷样品具有单一的尖晶石结构，具体如图1所示，且图1中(a)为实施例1中熵陶瓷样品的X射线衍射图谱图，(b)为实施例2中熵陶瓷样品的X射线衍射图谱图，(c)为实施例3中熵陶瓷样品的X射线衍射图谱图，(d)为实施例4中熵陶瓷样品的X射线衍射图谱图。
2、对上述实施例1-4所制得的中熵陶瓷采用SEM观察样品颗粒的形貌，具体实施例1的中熵陶瓷样品的SEM图为图2，实施例2的中熵陶瓷样品的SEM图为图4，实施例3的中熵陶瓷样品的SEM图为图6，实施例4的中熵陶瓷样品的SEM图为图8，且各实施例中样品粉末多为多面体。
3、对上述实施例1-4采用振动样品磁强计测量样品的磁性能：其中图3、图5、图7、图9分别为实施例1、实施例2、实施例3、实施例4中熵陶瓷样品的M-H图，且各组的样品磁性弱，具体磁学性能测量性能如下表所示：
组别 实施例1 实施例2 实施例3 实施例4
矫顽力 17Oe 18.1Oe 15.7Oe 0.2Oe
剩余磁化强度 0.0018emu/g 1.6067emu/g 1.0674emu/g 0.0112emu/g
饱和磁化强度 - 31.3800emu/g 30.3474emu/g 37.9482emu/g
需要说明的是，在本文中，诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来，而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且，术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含，从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素，而且还包括没有明确列出的其他要素，或者是还包括为这种过程、方法、物品或者设备所固有的要素。在没有更多限制的情况下，由语句“包括一个……”限定的要素，并不排除在包括所述要素的过程、方法、物品或者设备中还存在另外的相同要素。
以上实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。

Claims (7)

1.一种具有尖晶石结构的中熵陶瓷，其特征在于，所述具有尖晶石结构的中熵陶瓷的化学通式为(Me)3O4，所述Me为四种等摩尔比的金属元素，且这四种金属元素的选择为以下四种中的任意一种：
①Mn、Fe、Ni、Co；②Mn、Fe、Mg、Zn；③Mn、Fe、Mg、Co；④Mn、Fe、Mg、Ni。
2.一种如权利1所述的具有尖晶石结构的中熵陶瓷的制备方法，其特征在于，所述中熵陶瓷的制备方法包括以下步骤：
(1)原料预处理：按照金属离子摩尔比称取四种金属氧化物，并将金属氧化物的粉末置于球磨仪中充分球磨混合得浆料，后将浆料烘干，得球磨原料备用；
(2)初次烧结：将上述球磨原料置于马弗炉，加热至700℃-1450℃进行保温烧结，后取出研磨粉碎，得预制粉料备用；
(3)二次烧结：将上述预制粉料置入马弗炉在800℃-1450℃下进行第二次烧结，得到具有尖晶石材料的中熵陶瓷粉末。
3.根据权利要求2所述的一种具有尖晶石结构的中熵陶瓷的制备方法，其特征在于：所述步骤(1)中球磨仪混合的方式为将金属氧化物粉末置入盛有蒸馏水的球磨仪中，以150-250r/min的转速充分混合5-10小时。
4.根据权利要求2所述的一种具有尖晶石结构的中熵陶瓷的制备方法，其特征在于：所述步骤(2)中加热至700℃-1450℃的升温速度为3.5-4℃/min。
5.根据权利要求2所述的一种具有尖晶石结构的中熵陶瓷的制备方法，其特征在于：所述步骤(2)中研磨粉碎的粉末需过80目筛。
6.根据权利要求2所述的一种具有尖晶石结构的中熵陶瓷的制备方法，其特征在于：所述步骤(3)中第二次烧结保温的时间为10h。
7.根据权利要求2所述的一种具有尖晶石结构的中熵陶瓷的制备方法，其特征在于：所述步骤(3)获得的具有尖晶石材料的中熵陶瓷粉末后期将粉末压型后烧结，并应用于吸波或软磁方向。
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