水热合成法在制备纳米粉体材料方面具有许多独特的优势,但是由于反应在密闭容器中进行,很难研究清楚反应机理和动力学过程。利用原位检测技术,我们能够实时在线地监测反应过程,获得反应前驱体、相转变以及短寿命中间相的信息,更好地理解成核、结晶生长等动力学过程,进而为材料的可控制备提供依据。根据近年来国内外研究进展,本文全面介绍了基于同步辐射光源的能量色散分辨X射线衍射(EDXRD)、角度分辨X射线衍射(ADXRD)、X射线吸收精细结构谱(XAFS)、小角X射线散射(SAXS)、中子粉末衍射及小角散射(NPD和SANS)以及基于各种光谱(UV—Vis、Raman、FTIR)的原位检测技术和检测装置,以及纳米粉体水热制备机理的原位研究最新进展。
Hydrothermal synthesis has many unique advantages in the preparation of nanopowders. But the reaction mechanisms and kinetics have not been clearly understood because the reaction was generally occurred in a sealed vessel. In-situ techniques can be used to collect information about the precursors, phase evolution, the fate of the transient intermediates and better understand the nucleation, crystallization and growth by monitoring the whole reaction process in real time. Thus the controlled synthesis of materials can be achieved. This review summarizes the in-situ techniques, in-situ reactors and their applications in understanding the hydrothermal formation mechanisms of nanopowders. These in-situ techniques include synchrotron energy dispersive X-ray diffraction (EDXRD), angular dispersive X-ray diffraction (ADXRD), X-ray absorption fine structure (XAFS), small-angle X-ray scattering (SAXS), neutron powder diffraction (NPD), small-angle neutron scattering (SANS) and several selected spectroscopic methods (UV-Vis, Raman, FTIR).