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XRD测定氧在碳化锆和硼化锆中存在形态的研究
倪寿亮
学位类型硕士
导师袁方利 ; 白柳杨
2016-07
学位授予单位中国科学院研究生院
学位授予地点北京
学位专业化学工程
关键词Zrc Zrb2 X射线衍射 含氧量 存在形态
摘要

ZrC和ZrB2陶瓷具有耐高温的特点,广泛应用于航空航天等领域。但是,ZrC和ZrB2陶瓷中相应的氧化物会对陶瓷的性能会产生不良影响,因此,严格控制ZrC和ZrB2陶瓷粉体的氧含量是获得高性能陶瓷的核心。解析ZrC和ZrB2陶瓷粉体中氧的赋存状态,有助于了解粉体中氧化物的演变过程,对于控制ZrC和ZrB2陶瓷粉体的氧含量具有重要意义。本文从氧元素在纳米ZrC和ZrB2陶瓷粉体中存在的形态的研究出发,通过脉冲红外热导氧氮分析仪测量ZrC和ZrB2陶瓷粉体的全氧含量,借助X射线衍射法确定氧在ZrC和ZrB2陶瓷粉体中的赋存状态,解析氧在ZrC和ZrB2陶瓷粉体合成过程中的演变过程。研究了氧氮分析仪测得的氧的总含量、X射线衍射法测得的含氧化合物中氧的含量以及利用X射线衍射法分析测定纳米ZrC和ZrB2陶瓷粉体的晶粒大小及晶胞参数的变化。系统分析了氧氮分析仪测得的氧的总含量、X射线衍射法测得的含氧化合物中氧的含量以及两者之差与被测纳米ZrC和ZrB2陶瓷粉体的晶粒大小及晶胞参数之间的关系,研究表明氧氮分析仪测得的氧的总含量、X射线衍射法测得的含氧化合物中氧的含量与被测纳米ZrC和ZrB2陶瓷粉体的晶粒大小及晶胞参数之间没有直接相关性,而两种方法测试的氧含量之差与被测纳米ZrC和ZrB2陶瓷粉体的晶粒大小及晶胞参数之间存在一定的直接相关性。说明纳米ZrC和ZrB2陶瓷粉体中的部分氧进入到被测样品的晶格中,以固溶氧的形态存在,对其晶格造成了影响和变化。因此,在纳米ZrC和ZrB2陶瓷粉体中氧主要以氧化物形态存在,部分氧还以固溶氧的形态存在。纳米ZrC和ZrB2陶瓷粉体的结果表明,对于非氧化物陶瓷,氧除了以氧化物的形式存在外,部分氧还会以固溶氧的形态存在,抑制固溶氧的形成是获得低氧含量陶瓷粉体的关键。 

其他摘要

ZrC and ZrB2 ceramics, as high temperature materials, are widely used in aerospace and other fields. But oxygen element in ZrC and ZrB2 ceramics always have adverse effects on the performance of the ceramics. Therefore, more and more attention has been attracted on how to control the oxygen content in ZrC and ZrB2 ceramic powders and obtain high performance ceramics. The analysis of oxygen state in ZrC and ZrB2 ceramic powders can help to understand the evolution process of oxygen element in powders, which is of great significance to synthesize ZrC and ZrB2 ceramic powders with low oxygen content and high performance ceramics.In this paper, the oxygen existing forms and the total oxygen content in ZrC and ZrB2 ceramic powders were measured by oxygen-nitrogen analyzer and X-ray diffraction, respectively. The evolution process of the oxygen element in the synthesis of ZrC and ZrB2 ceramic powders was analyzed based on the oxygen state in ZrC and ZrB2 ceramic powders. The total oxygen content was studied by oxygen-nitrogen analyzer, and the oxygen content in zirconium oxides was studied by X-ray diffraction. The grain size and the crystal cell parameters of ZrC and ZrB2 were determined by X-ray diffraction. Then, the total oxygen content measured by oxygen-nitrogen analyzer, the oxygen content measured by X ray diffraction, and the difference between these two oxygen content values, were compared with the grain size of ZrC and ZrB2 powders and the crystal cell parameters of nanometer ZrC and ZrB2 respectively. Results showed that the total oxygen content and the oxygen content in oxides have no significance in relation to the grain size and crystal cell parameters. However, the difference between the two oxygen content value and the grain size and the crystal cell parameters showed linear correlation between each other. It indicated that part of oxygen element in ZrC and ZrB2 powders entered the crystal lattice of the sample and existed in the form of solid-solution-oxygen, which have affected the crystal lattices and made the change. So oxygen element in ZrC and ZrB2 powders existed in forms as not only oxides but also solid-solution.In short, some oxygen element contained in non-oxide ceramics such as ZrC and ZrB2 ceramic powders can enter the crystal lattice and existed in forms of solid-solution, which in forms that it would help to reduce the oxygen content and get high purity powders by inhibiting the formation of solid solution. 

语种中文
文献类型学位论文
条目标识符http://ir.ipe.ac.cn/handle/122111/22926
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倪寿亮. XRD测定氧在碳化锆和硼化锆中存在形态的研究[D]. 北京. 中国科学院研究生院,2016.
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