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Instruments / Technical Area	Publication Details	Published	Actions
B18-Core EXAFS	Exploring the influence of atomic level structure, porosity, and stability of bismuth(iii) coordination polymers on electrocatalytic CO2 reduction Sara Frank , Erik Svensson Grape , Espen Drath Bøjesen , Rasmus Larsen , Paolo Lamagni , Jacopo Catalano , A. Ken Inge , Nina Lock Journal Of Materials Chemistry A 28 DOI: 10.1039/D1TA06564E Diamond Proposal Number(s): [22410] Show Abstract ▼ Abstract: Bismuth-based coordination polymers (CPs) have recently attracted attention as catalyst precursors for the electrocatalytic CO2 reduction reaction (eCO2RR). We present a comparative study by investigating six bismuth-based compounds in-depth to elucidate the correlation between their structures and their catalytic CO2-to-formate conversion. Thereby, we identify structural indicators of the pristine CPs resulting in optimized catalytic performance, paving the way for future design of CP derived catalysts. The structural properties of the six pristine materials vary in terms of porosity (from non-porous to 495 m2 g−1), linker type (carboxylate- or phenolate-based), thermal- and chemical stability, and metal content. Herein, electrochemical studies are combined with comprehensive structural investigations using electron microscopy, powder X-ray diffraction, and X-ray absorption spectroscopy. Our study reveals that low chemical stability of the pristine CPs is crucial for the conversion of the precursors into active Bi2O2CO3 and of paramount importance for the eCO2RR activity, while the nature of the pristine material mostly influence the catalyst morphology and transport properties. Of the six investigated CPs, the best performing compounds selectively convert CO2 to formate with faradaic efficiencies in the range 80(3)–95(3)% and current densities of 5(1)–8(1) mA cm−2 at −0.97 VRHE.	Nov 2021
I15-1-X-ray Pair Distribution Function (XPDF)	Breaking with the principles of coreduction to form stoichiometric intermetallic PdCu nanoparticles Jette K. Mathiesen , Espen D. Bøjesen , Jack K. Pedersen , Emil T. S. Kjær , Mikkel Juelsholt , Susan Cooper , Jonathan Quinson , Andy S. Anker , Geoff Cutts , Dean S. Keeble , Maria S. Thomsen , Jan Rossmeisl , Kirsten M. Ø. Jensen Small Methods 68 DOI: 10.1002/smtd.202200420 Diamond Proposal Number(s): [20187] Open Access Show Abstract ▼ Abstract: Intermetallic nanoparticles (NPs) have shown enhanced catalytic properties as compared to their disordered alloy counterparts. To advance their use in green energy, it is crucial to understand what controls the formation of intermetallic NPs over alloy structures. By carefully selecting the additives used in NP synthesis, it is here shown that monodisperse, intermetallic PdCu NPs can be synthesized in a controllable manner. Introducing the additives iron(III) chloride and ascorbic acid, both morphological and structural control can be achieved. Combined, these additives provide a synergetic effect resulting in precursor reduction and defect-free growth; ultimately leading to monodisperse, single-crystalline, intermetallic PdCu NPs. Using in situ X-ray total scattering, a hitherto unknown transformation pathway is reported that diverges from the commonly reported coreduction disorder–order transformation. A Cu-rich structure initially forms, which upon the incorporation of Pd(0) and atomic ordering forms intermetallic PdCu NPs. These findings underpin that formation of stoichiometric intermetallic NPs is not limited by standard reduction potential matching and coreduction mechanisms, but is instead driven by changes in the local chemistry. Ultimately, using the local chemistry as a handle to tune the NP structure might open new opportunities to expand the library of intermetallic NPs by exploiting synthesis by design.	Apr 2022

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