Center for Materials Crystallography, Department of Chemistry and iNANO, Aarhus University, Langelandsgade 140, 8000 Aarhus C (Denmark) www.cmc.chem.au.dk.
ChemSusChem. 2014 Jun;7(6):1594-611. doi: 10.1002/cssc.201301042. Epub 2014 Mar 5.
Solvothermal and hydrothermal synthesis, that is, synthesis taking place in a solvent at elevated temperature and pressure, is a powerful technique for the production of advanced energy materials as it is versatile, cheap, and environmentally friendly. However, the fundamental reaction mechanisms dictating particle formation and growth under solvothermal conditions are not well understood. In order to produce tailor-made materials with specific properties for advanced energy technologies, it is essential to obtain an improved understanding of these processes and, in this context, in situ studies are an important tool as they provide real time information on the reactions taking place. Here, we present a review of the use of powder diffraction and total scattering methods for in situ studies of synthesis taking place under solvothermal and hydrothermal conditions. The experimental setups used for in situ X-ray and neutron studies are presented, and methods of data analysis are described. Special attention is given to the methods used to extract structural information from the data, for example, Rietveld refinement, whole powder pattern modelling and pair distribution function analysis. Examples of in situ studies are presented to illustrate the types of chemical insight that can be obtained.
溶剂热和水热合成，即在高温高压下在溶剂中进行的合成，是一种生产先进能源材料的有力技术，因为它具有多功能性、廉价和环保的特点。然而，决定溶剂热条件下颗粒形成和生长的基本反应机制还没有得到很好的理解。为了生产具有特定性能的定制材料，用于先进能源技术，必须提高对这些过程的理解，在这方面，原位研究是一种重要的工具，因为它提供了有关正在发生的反应的实时信息。在这里，我们回顾了粉末衍射和全散射方法在溶剂热和水热条件下合成的原位研究中的应用。介绍了用于原位 X 射线和中子研究的实验装置，并描述了数据分析方法。特别关注了从数据中提取结构信息的方法，例如，Rietveld 精修、全粉末图案建模和配分函数分析。给出了一些原位研究的例子来说明可以获得的化学洞察力的类型。
