Simmler Mira, Meier Manuel, Nirschl Hermann
Institute of Mechanical Process Engineering and Mechanics, Karlsruhe Institute of Technology, 76131 Karlsruhe, Germany.
Materials (Basel). 2022 Mar 14;15(6):2124. doi: 10.3390/ma15062124.
In this work, we take on an in-depth characterization of the complex particle structures made by spray flame synthesis. Because of the resulting hierarchical aggregates, very few measurement techniques are available to analyze their primary particle and fractal properties. Therefore, we use small-angle X-ray scattering (SAXS) and transmission electron microscopy (TEM) to investigate the influence of the precursor concentration on the fractal structures of zirconia nanoparticles. The combination of information gained from these measurement results leads to a detailed description of the particle system, including the polydispersity and size distribution of the primary particles. Based on our findings, unstable process conditions could be identified at low precursor concentrations resulting in the broadest size distribution of primary particles with rough surfaces. Higher precursor concentrations lead to reproducible primary particle sizes almost independent of the initial precursor concentration. Regarding the fractal properties, the typical shape of aggregates for aerosols is present for the investigated range of precursor concentrations. In conclusion, the consistent results for SAXS and TEM show a conclusive characterization of a complex particle system, allowing for the identification of the underlying particle formation mechanism.
在这项工作中,我们对喷雾火焰合成制备的复杂颗粒结构进行了深入表征。由于形成了分级团聚体,很少有测量技术可用于分析其初级颗粒和分形特性。因此,我们使用小角X射线散射(SAXS)和透射电子显微镜(TEM)来研究前驱体浓度对氧化锆纳米颗粒分形结构的影响。从这些测量结果中获得的信息相结合,得出了对颗粒系统的详细描述,包括初级颗粒的多分散性和尺寸分布。基于我们的研究结果,在前驱体浓度较低时可识别出不稳定的工艺条件,这会导致初级颗粒尺寸分布最宽且表面粗糙。较高的前驱体浓度会导致可重复的初级颗粒尺寸,几乎与初始前驱体浓度无关。关于分形特性,在所研究的前驱体浓度范围内,气溶胶团聚体呈现出典型形状。总之,SAXS和TEM的一致结果显示了对复杂颗粒系统的确切表征,从而能够识别潜在的颗粒形成机制。