Thermogravimetry-evolved gas analysis-mass spectrometry system for materials research
Thermogravimetry-evolved gas analysis-mass spectrometry system for materials research
复制标题
用于材料研究的热重-逸出气体分析-质谱系统
DOI：
10.1007/bf02711191
复制
发表时间：
2003
影响因子：
1.8
通讯作者：
B. Raj
中科院分区：
文献类型：
--
作者：
M. Kamruddin;P. K. Ajikumar;S. Dash;A. K. Tyagi;B. Raj
热分析是一种广泛应用于材料研究的分析技术。而热分析与同步演化气体分析更能准确、完整地描述热事件。在各种气体分析技术中，质谱法具有许多优点。因此，开发了一种基于超高真空（UHV）兼容的质谱分析（EGA-MS）系统。该系统由一个装有质谱仪的测量室、旋转转子计和真空计以及一个高真空、高温反应室组成。它与商用热重分析仪（TGA: TG + DTA）相连。增加了额外的基于质量流量的气体/蒸汽输送系统和校准气体入口，使其成为多功能的TGA-EGA-MS设施。该系统提供了有关重量变化、热量变化、气体性质和含量的完整信息，用于(i)程序化温度分解（TPD）、（ii）纳米晶材料合成、（iii）气固相互作用和（iv）气体混合物分析。对各种无机氧阴离子固体的TPD进行了研究，并对反应中间体/产物进行了离线分析。在许多情况下，动态操作条件可以产生纳米晶产品。本文主要描述了现有EGA-MS系统与TGA耦合的设计特点，相关的流体处理系统，系统校准程序和温度程序分解的结果。此外，还介绍了真空热分解法合成几种纳米晶氧化物、气体分析以及该装置作为可控大气暴露装置用于研究气固相互作用的潜力。
Thermal analysis is a widely used analytical technique for materials research. However, thermal analysis with simultaneous evolved gas analysis describes the thermal event more precisely and completely. Among various gas analytical techniques, mass spectrometry has many advantages. Hence, an ultra high vacuum (UHV) compatible mass spectrometry based evolved gas analysis (EGA-MS) system has been developed. This system consists of a measurement chamber housing a mass spectrometer, spinning rotor gauge and vacuum gauges coupled to a high vacuum, high temperature reaction chamber. A commercial thermogravimetric analyser (TGA: TG + DTA) is interfaced to it. Additional mass flow based gas/vapour delivery system and calibration gas inlets have been added to make it a versatile TGA-EGA-MS facility. This system which gives complete information on weight change, heat change, nature and content of evolved gases is being used for (i) temperature programmed decomposition (TPD), (ii) synthesis of nanocrystalline materials, (iii) gas-solid interactions and (iv) analysis of gas mixtures. The TPD of various inorganic oxyanion solids are studied and reaction intermediates/products are analysed off-line. The dynamic operating conditions are found to yield nanocrystalline products in many cases. This paper essentially describes design features involved in coupling the existing EGA-MS system to TGA, associated fluid handling systems, the system calibration procedures and results on temperature programmed decomposition. In addition, synthesis of a few nanocrystalline oxides by vacuum thermal decomposition, gas analysis and potential use of this facility as controlled atmosphere exposure facility for studying gas-solid interactions are also described.