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Instruments / Technical Area	Publication Details	Published
B18-Core EXAFS	Enabling the terpyridine ligand motif for Ir-based solid molecular catalysts Keanu V. A. Birkelbach , Heinrich Hartmann , Astrid Besmehn , Alexander Meledin , Isabella Kappel , Peter J. C. Hausoul , Regina Palkovits Ees Catalysis 43 DOI: 10.1039/D4EY00281D Diamond Proposal Number(s): [32235] Open Access Show Abstract ▼ Abstract: Terpyridine (tpy) and its derivatives are strongly coordinating ligands with a high degree of customizability. Due to their tendency to form stable bis(tpy) complexes with transition metals such as Ir and Ru, their application in thermal catalysis is limited, instead revolving mostly around electro-, photo- and supramolecular chemistry. Herein, it is demonstrated that immobilization of the tpy motif via incorporation into a polymer suppresses their formation in Ir-catalyzed formic acid dehydrogenation (FADH), highlighting a distinct advantage of solid molecular catalysts (SMCs). A catalytic activity of up to 175[thin space (1/6-em)]000 h−1 was achieved at 160 °C and maintained at temperatures as low as 80 °C. Based on the results of a kinetic isotope effect (KIE) study, a catalytic cycle is proposed and the rate-determining step is identified. In a continuous setup, the most active SMC retained its activity over the course of 5 days, resulting in a TON upwards of 2[thin space (1/6-em)]800[thin space (1/6-em)]000. Through XPS, HAADF-STEM (-EDX) and EXAFS analyses, insights into the interaction between a metal precursor and poly-terpyridine are gained.	Mar 2025
B18-Core EXAFS I20-EDE-Energy Dispersive EXAFS (EDE)	Structural selectivity of supported Pd nanoparticles: selective ethanol ammoxidation to acetonitrile Khaled Mohammed , Reza Vakili , Donato Decarolis , Shaojun Xu , Luke L. Keenan , Apostolos Kordatos , Nikolay Zhelev , Chris K. Skylaris , Marina Carravetta , Emma K. Gibson , Haresh Manyar , Alexandre Goguet , Peter P. Wells Ees Catalysis DOI: 10.1039/D4EY00044G Diamond Proposal Number(s): [28666, 34632] Open Access Show Abstract ▼ Abstract: The need to achieve net zero requires decarbonisation across all areas of our industrialised society, including the production of chemicals. One example is the production of acetonitrile, which currently relies on fossil carbon. Recently, supported Pd nanoparticles have been shown to promote the selective transformation of bio-derived ethanol to acetonitrile. Elsewhere, current research has demonstrated the importance of interstitial structures of Pd in promoting specific transformations. In this study, we demonstrate through a spatially resolved operando energy-dispersive-EXAFS (EDE) technique that the selectivity to acetonitrile (up to 99%) is concurrent with the formation of a PdNx phase. This was evidenced from the features observed in the X-ray Absorption near edge structure validated against PdNx samples made via known synthesis methods. . Above 240 ℃, the Pd nanoparticles became progressively oxidised which led to the production of unwanted byproducts, primarily CO2. The spatially resolved analysis indicated that the Pd speciation was homogeneous across the catalyst profile throughout the series of studies performed. This work resolved the structural selectivity of Pd nanoparticles that directs ethanol ammoxidation towards acetonitrile, and provides important information on the performance descriptors required to advance this technology.	Apr 2024
I20-EDE-Energy Dispersive EXAFS (EDE)	Deconvoluting kinetics and transport effects of ionic liquid layers on FeN4-based oxygen reduction catalysts Silvia Favero , Ifan E. L. Stephens , Maria-Magdalena Titirici Ees Catalysis DOI: 10.1039/D3EY00166K Open Access Show Abstract ▼ Abstract: The use of ionic liquid layers has been reported to improve both the activity and durability of several oxygen reduction catalysts. However, the development of this technology has been hindered by the lack of understanding of the mechanism behind this performance enhancement. In this work, we use a library of ionic liquids to modify a model FeN4 catalyst (iron phthalocyanine), to decouple the effects of ionic liquid layers on oxygen reduction kinetics and oxygen transport. Our results show that oxygen reduction activity at low overpotentials it determined by the ionic liquids’ influence on the *OH binding energy on the active sites, while oxygen solubility and diffusivity controls transport at high overpotentials. Finally, using nitrogen physisorption, we have demonstrated that the distribution of the ionic liquids on the catalyst is inhomogeneous, and depends on the nature of the ionic liquid used.	Jul 2023

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