Versatile Spectroscopic Cell for Operando Studies in Heterogeneous Catalysis Using Tender X-ray Spectroscopy in Fluorescence Mode

IF 6.1 Q1 CHEMISTRY, MULTIDISCIPLINARY Chemistry methods : new approaches to solving problems in chemistry Pub Date : 2024-01-16 DOI:10.1002/cmtd.202300044
H. A. Suarez Orduz, S.-L. Heck, Dr. P. Dolcet, Dr. Y. Watier, Dr. M. Casapu, Prof. Dr. J.-D. Grunwaldt, Dr. P. Glatzel
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Abstract

The design and commissioning of a cell suitable for operando studies using high-energy-resolution fluorescence-detected X-ray absorption near-edge structure (HERFD-XANES) spectroscopy in the tender X-ray regime is reported. The cell is optimized for measurements within the energy range of 1.5 keV to 4.5 keV. It has a plug-flow geometry and can be used for sieved powder samples, analogous to reactors employed for laboratory tests. The functionality of the spectroscopic cell is demonstrated in the area of emission control using CO oxidation as target reaction over 1 wt.% Rh/γ-Al2O3 as catalyst. We show how HERFD-XANES at the Rh L3-edge captures variations in the noble metal structure resulting from the interaction with the support material and reactant molecules. Moreover, distinct structural changes were identified along the catalyst bed as a function of temperature and local gas mixture.

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利用荧光模式下的嫩 X 射线光谱进行异相催化操作研究的多功能光谱池
本研究报告介绍了一种适合在嫩 X 射线系统中使用高能量分辨荧光检测 X 射线吸收近边结构(HERFD-XANES)光谱进行操作研究的样品池的设计和调试情况。该样品池针对 1.5 keV 至 4.5 keV 能量范围内的测量进行了优化。它具有塞流几何形状,可用于筛分粉末样品,类似于实验室测试中使用的反应器。在以 1 wt.% Rh/γ-Al2O3 为催化剂、以 CO 氧化为目标反应的排放控制领域,演示了光谱池的功能。我们展示了 Rh L3 边沿的 HERFD-XANES 如何捕捉贵金属结构因与支撑材料和反应物分子相互作用而产生的变化。此外,我们还发现了催化剂床层在温度和局部气体混合物作用下的明显结构变化。
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