CN113929449A - 纳米高熵氧化物陶瓷粉体及其制备方法 - Google Patents
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- 229910052715 tantalum Inorganic materials 0.000 description 1
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Abstract
本发明提供纳米高熵氧化物陶瓷粉体及其制备方法，包括以下步骤：(1)原料准备，原料微米级粉体TiC、ZrC、HfC、NbC、TaC；(2)将上述各种原料粉体按等摩尔分子量进行配比，球磨，得到碳化物陶瓷混合粉体；(3)将上述所制得的球磨粉体进行热压烧结，得到单相高熵碳化物陶瓷；(4)将单相高熵碳化物陶瓷采用机械方式进行破碎；(5)将破碎的单相高熵碳化物陶瓷粉体氧化，获得纳米高熵氧化物陶瓷粉体。本发明为纳米高熵氧化物陶瓷的制备提供一种全新的制备路线，制备的纳米高熵氧化物陶瓷粉体可以在未来能源、环境所需的材料上应用。
Description
技术领域
本发明涉及到纳米材料的制备技术，特别涉及了纳米高熵氧化物陶瓷粉体及其制备方法。
背景技术
高熵材料的世界是多样的，通过添加组元元素，材料出现一些新颖的性质。高熵氧化物作为高熵陶瓷中的一类重要研究对象，具备优异的性能，可以在热和环境保护、热电、催化和能源存储等方面有广泛的应用。
目前，高熵氧化物的合成路线包括固相反应，喷雾热解法，火焰热解法，共沉淀法和改进的溶液燃烧合成法，然而关于纳米高熵陶瓷粉体的制备方法尚无文献报道。
纳米高熵氧化物陶瓷粉体的制备或有利于材料在环境、能源领域的领域。
发明内容
本发明的第一目的在于提供一种纳米高熵氧化物陶瓷粉体的制备方法。
本发明的第二目的在于提供一种单相纳米高熵氧化物陶瓷粉体。
纳米高熵氧化物陶瓷粉体的制备方法，包括以下步骤：
(1)采用的原料为高纯(纯度＞99.5％)微米级粉体TiC、ZrC、HfC、NbC、TaC，粒度为400-800目粉体；
(2)将上述各种原料粉体按等摩尔分子量进行配比，球磨参数：球料比，即球磨介质与物料的质量比为8-10:1，球磨介质为硬质陶瓷球，转速设定为200-300r/min，按照球磨2-4小时冷却一小时的方式进行多次球磨，球磨时间为20-30h，得到碳化物陶瓷混合粉体。
(3)将上述所制得的碳化物陶瓷混合粉体在1800～2200℃条件下进行热压烧结，升温速率控制在10℃/min以下，1500℃开始加压到50-100MPa，得到的晶粒尺寸小于50μm的单相高熵碳化物陶瓷。
(4)将单相高熵碳化物陶瓷采用机械方式进行破碎，破碎至颗粒尺寸小于500μm。
(5)最后，将破碎的单相高熵碳化物陶瓷粉体在900-1200℃马弗炉中氧化3-5h，可制备获得纳米高熵氧化物陶瓷粉体。
优选的，球磨的球料比为10:1，球磨介质为硬质陶瓷球，转速设定为200r/min，球磨两小时冷却一小时，球磨混合均匀的碳化物陶瓷扥莫。
本发明的有益效果如下：
利用高熵碳化物的成功制备，使元素Ti、Zr、Hf、Nb、Ta达到原子级别的均匀混合，再利用高熵碳化物相与其氧化相的晶胞尺寸差异产生的晶格应力，获得尺寸均匀的纳米高熵氧化物陶瓷。
本发明为纳米高熵氧化物陶瓷的制备提供一种全新的制备路线，制备的纳米高熵氧化物陶瓷粉体可以在未来能源、环境所需的材料上应用。
附图说明
图1为实施例1经过热压后得到的单相高熵碳化物的XRD衍射图谱。
图2为实施例1纳米高熵氧化物陶瓷粉体形貌。
图3为实施例1纳米高熵氧化物陶瓷粉体成分分布。
具体实施方式
结合实施例说明本发明的具体技术方案。
纳米高熵氧化物陶瓷粉体的制备方法，包括以下步骤：
(1)准备采用的原料主要有高纯(纯度＞99.5％)微米级粉体TiC、HfC、TaC、NbC、ZrC，粒度为400-800目粉体；
(2)将上述各种原料粉体按等摩尔分子量进行配比，球磨参数：球料比，即球磨介质与物料的质量比为10:1，球磨介质为硬质陶瓷球，转速设定为200-300r/min，按照球磨2小时冷却一小时的方式进行多次球磨，球磨时间为20h，得到碳化物陶瓷混合粉体；
(3)再将所制得的碳化物陶瓷混合粉体在2000℃条件下进行热压烧结，升温速率控制在8℃/min，1500℃开始加压到50-100MPa，得到的晶粒尺寸约50μm的单相高熵碳化物陶瓷；
如图1为经过热压后得到的单相高熵碳化物的XRD衍射图谱。
(4)将单相高熵碳化物陶瓷采用机械方式进行破碎，破碎至颗粒尺寸小于100μm；
(5)将破碎的单相高熵碳化物陶瓷粉体在900℃马弗炉中氧化3h，可制备获得纳米高熵氧化物陶瓷粉体。
如图2为纳米高熵氧化物陶瓷粉体形貌。如图3为纳米高熵氧化物陶瓷粉体成分分布。
Claims (8)
1.纳米高熵氧化物陶瓷粉体的制备方法，其特征在于，包括以下步骤：
(1)原料准备，原料微米级粉体TiC、ZrC、HfC、NbC、TaC；
(2)将上述各种原料粉体按等摩尔分子量进行配比，球磨，得到碳化物陶瓷混合粉体；
(3)将上述所制得的球磨粉体进行热压烧结，得到单相高熵碳化物陶瓷；
(4)将单相高熵碳化物陶瓷采用机械方式进行破碎；
(5)将破碎的单相高熵碳化物陶瓷粉体氧化，获得纳米高熵氧化物陶瓷粉体。
2.根据权利要求1所述的纳米高熵氧化物陶瓷粉体的制备方法，其特征在于：步骤(1)中原料采用纯度＞99.5％、粒度为400-800目粉体。
3.根据权利要求1所述的纳米高熵氧化物陶瓷粉体的制备方法，其特征在于：步骤(2)中所述的球磨参数：球料比，即球磨介质与物料的质量比为8-10:1，球磨介质为硬质陶瓷球，转速设定为200-300r/min，按照球磨2-4小时冷却一小时的方式进行多次球磨，球磨时间为20-30h。
4.根据权利要求3所述的纳米高熵氧化物陶瓷粉体的制备方法，其特征在于：步骤(2)所得的碳化物陶瓷混合粉体尺寸小于20μm。
5.根据权利要求1所述的纳米高熵氧化物陶瓷粉体的制备方法，其特征在于：步骤(3)中所述的热压烧结，将所制得的碳化物陶瓷混合粉体在1800～2200℃条件下进行热压烧结，升温速率控制在10℃/min以下，1500℃开始加压到50-100MPa，得到的晶粒尺寸小于50μm的单相高熵碳化物陶瓷。
6.根据权利要求1所述的纳米高熵氧化物陶瓷粉体的制备方法，其特征在于：步骤(4)中所述的破碎，破碎至颗粒尺寸小于500μm。
7.根据权利要求1所述的纳米高熵氧化物陶瓷粉体的制备方法，其特征在于：步骤(4)中所述氧化，为在900-1200℃马弗炉中氧化3-5h。
8.纳米高熵氧化物陶瓷粉体，其特征在于：根据权利要求1到7任一项所述的制备方法所得。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20090074604A1 (en) * | 2007-09-19 | 2009-03-19 | Industrial Technology Research Institute | Ultra-hard composite material and method for manufacturing the same |
| CN108439986A (zh) * | 2018-05-09 | 2018-08-24 | 西北工业大学 | (HfTaZrTiNb)C高熵陶瓷粉体及高熵陶瓷粉体和高熵陶瓷块体的制备方法 |
| CN110204328A (zh) * | 2019-06-05 | 2019-09-06 | 西南交通大学 | 一种高熵氧化物陶瓷的制备方法 |
| CN112723862A (zh) * | 2020-12-29 | 2021-04-30 | 太原理工大学 | 简单低耗制备高熵氧化物陶瓷材料的方法 |
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| US20090074604A1 (en) * | 2007-09-19 | 2009-03-19 | Industrial Technology Research Institute | Ultra-hard composite material and method for manufacturing the same |
| CN108439986A (zh) * | 2018-05-09 | 2018-08-24 | 西北工业大学 | (HfTaZrTiNb)C高熵陶瓷粉体及高熵陶瓷粉体和高熵陶瓷块体的制备方法 |
| CN110204328A (zh) * | 2019-06-05 | 2019-09-06 | 西南交通大学 | 一种高熵氧化物陶瓷的制备方法 |
| CN112723862A (zh) * | 2020-12-29 | 2021-04-30 | 太原理工大学 | 简单低耗制备高熵氧化物陶瓷材料的方法 |
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Application publication date: 20220114 |
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