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Instruments / Technical Area	Publication Details	Published	Actions
I15-1-X-ray Pair Distribution Function (XPDF)	In situ total scattering experiments of nucleation and crystallisation of tantalum-based oxides: from highly dilute solutions via cluster formation to nanoparticles Ezgi Onur Sahin , Harun Tueysuez , Candace K. Chan , Gun-hee Moon , Yitao Dai , Wolfgang Schmidt , Joohun Lim , Christina Scheu , Claudia Weidenthaler Nanoscale DOI: 10.1039/D0NR07871A Diamond Proposal Number(s): [16372] Open Access Show Abstract ▼ Abstract: The exact formation mechanism of tantalum oxides (and in general, metal/mixed metal oxides) from alkoxide precursors is still not fully understood, particularly when forming cluster-like or amorphous materials. The structural evolution of Ta-based oxides was studied in detail using X-ray total scattering experiments along with subsequent pair distribution function (PDF) analyses. Starting from a tantalum alkoxide precursor (Ta2(OEt)10), the formation of hydrolysed TaxOyHz clusters in highly diluted aqueous solution was analysed. From the PDF data, the connectivity and arrangement of TaxOy octahedra in the cluster could be deduced as well as the approximate size of the clusters (<1 nm). Construction of cluster models allowed for identification of common structural motifs in the TaxOyHz clusters, ruling out the formation of chain- or ring-like clusters. More likely, bulky clusters with a high number of corner-sharing octahedra are formed. After separation of the amorphous solid from the liquid, temperature-induced crystallisation processes were monitored via in situ total scattering experiments. Between room temperature and 600 °C, only small rearrangements of the amorphous structure are observed. At about 610 °C, amorphous TaxOyHz transforms directly into crystalline orthorhombic L-Ta2O5 without formation of any crystalline intermediate structures.	Nov 2020
I20-Scanning-X-ray spectroscopy (XAS/XES)	Tailoring morphology and electronic structure of cobalt iron oxide nanowires for electrochemical oxygen evolution reaction Eko Budiyanto , Mingquan Yu , Minmin Chen , Serena Debeer , Olaf Rudiger , Harun Tuysuz Acs Applied Energy Materials DOI: 10.1021/acsaem.0c01201 Diamond Proposal Number(s): [21526] Open Access Show Abstract ▼ Abstract: Herein, the influence of iron on nanocasting of cobalt oxide nanowires and the performance of these materials for the oxygen evolution reaction (OER) are investigated. Pristine Co3O4 and mixed cobalt iron oxide nanowires with a diameter of 7 nm have been synthesized via a nanocasting route by using SBA 15 silica as a template. A small amount of iron added during the synthesis results in a decrease in the nanowires’ array length and induces the formation of a bimodal pore size distribution. Raman Spectroscopy, X-ray emission and high-energy resolution X-ray absorption spectroscopies further show that Fe incorporation alters the electronic structure by increasing the average distortion around the cobalt centers and the amount of Co2+ in tetrahedral sites. These affect the OER activity significantly; the overpotential of pristine Co3O4 at 10 mA/cm2 decreases from 398 to 378 mV, and the current density at 1.7 V increases from 107 to 150 mA/cm2 with the addition of iron at Co/Fe atomic ratio of 32. Furthermore, post-reaction characterization confirmed that both the morphology and electronic structure of nanowires remain intact after a long-term stability test.	Aug 2020

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