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Instruments / Technical Area	Publication Details	Published
I20-EDE-Energy Dispersive EXAFS (EDE)	Important role of open copper sites on adsorption of various molecules in Cu-BTC metal organic framework Iuliia Mikulska , Roberto Boada , Shusaku Hayama , Matteo Aramini , Luke Keenan , Monica Amboage , Sofia Diaz-Moreno XAFS2021 Show Abstract ▼ Abstract: Cu-BTC metal-organic framework (MOF) has been found to be a promising candidate for removing hazardous substances from air via adsorption1. To understand the role that the copper sites in Cu-BTC play in the adsorption process, we have performed a detailed X-ray absorption spectroscopy (XAS) study. Conventional XAS and high energy resolution fluorescence detection XAS (HERFD-XAS) were collected on degassed Cu-BTC, and after being exposed to CO2, water and benzene. The EXAFS analysis reveals that, although the local environment around the copper centers in all samples is similar, differences can be found in the first and second coordination shells. We have found that the Cu-O distance in the first coordination shell is slightly larger when the sample is immersed in water and benzene than in the degassed sample, while it does not change for the sample exposed to CO2. Small differences are also observed in the Cu-Cu distance, gradually increasing from 2.49 Å in the degassed sample, to 2.52 Å, 2.58 Å and 2.63 Å upon adsorption of CO2, benzene and water, respectively. HERFD-XAS has been used to obtain information about the electronic and geometric structure around the copper metal centers, as the use of high energy resolution enhances the features in the XANES spectrum enabling the detection of subtle changes2. We have observed differences in the intensity and the energy position of some of the XANES spectral features upon adsorption of different adsorbates that can be attributed to changes in the local environment around the copper centers, as detected in the EXAFS analysis. In this study we show that XAS is a powerful and very sensitive tool for studying host-guest interactions in MOFs, providing atomic-level insights into adsorption mechanisms.	Jul 2021
I20-Scanning-X-ray spectroscopy (XAS/XES) Detectors	First results using the new DLS Xspress4 digital pulse processor with monolithic segmented HPGe detectors on XAS beamlines G. Dennis , W. Helsby , D. Omar , I. Horswell , N. Tartoni , S. Hayama , I. Mikulska , S. Diaz-Moreno 13th International Conference on Synchrotron Radiation Instrumentation – SRI2018 DOI: 10.1063/1.5084696 Open Access Show Abstract ▼ Abstract: Diamond Light Source (DLS) I20-Scanning is a high flux X-ray Absorption Spectroscopy (XAS) beamline optimized for challenging samples, operating between 4keV and 20keV. The principal detector used for collecting XAS in fluorescence mode is a Canberra 64-pixel Monolithic Segmented Hyper Pure Germanium Detector (HPGe) historically partnered with the STFC Xspress2 Digital Pulse Processor (DPP). Prior signal analysis had shown that key parameters such as Energy Resolution and Peak-to-Background ratio are compromised by pixel-to-pixel crosstalk within the detector, especially at higher count rates (>250kcps per pixel). The DLS Detector Group have developed the new Xspress4 DPP to address such issues. This results in typically a factor 3-7 increase in detector system count rate for the same Energy Resolution and Peak-to-Background ratio compared to the previous state-of-the-art DPP. An overview of the complete detector system is given and recent results obtained during the commissioning on the beamline are shown. Further, comparative results from challenging experiments are also shown, demonstrating the improved performance attainable at the previous high count rate by partnering legacy HPGe Detectors with the latest DPP technology.	Jan 2019
B18-Core EXAFS I18-Microfocus Spectroscopy I20-EDE-Energy Dispersive EXAFS (EDE) I20-Scanning-X-ray spectroscopy (XAS/XES) Controls Detectors Optics	The Spectroscopy Village at Diamond Light Source Sofia Diaz-Moreno , Monica Amboage , Mark Basham , Roberto Boada , Nicholas E. Bricknell , Giannantonio Cibin , Thomas Cobb , Jacob Filik , Adam Freeman , Kalotina Geraki , Diego Gianolio , Shusaku Hayama , Konstantin Ignatyev , Luke Keenan , Iuliia Mikulska , J. Frederick W. Mosselmans , James J. Mudd , Stephen A. Parry Journal Of Synchrotron Radiation 25 DOI: 10.1107/S1600577518006173 Open Access Show Abstract ▼ Abstract: This manuscript presents the current status and technical details of the Spectroscopy Village at Diamond Light Source. The Village is formed of four beamlines: I18, B18, I20-Scanning and I20-EDE. The village provides the UK community with local access to a hard X-ray microprobe, a quick-scanning multi-purpose XAS beamline, a high-intensity beamline for X-ray absorption spectroscopy of dilute samples and X-ray emission spectroscopy, and an energy-dispersive extended X-ray absorption fine-structure beamline. The optics of B18, I20-scanning and I20-EDE are detailed; moreover, recent developments on the four beamlines, including new detector hardware and changes in acquisition software, are described.	Jul 2018
	Chemical instability of an interface between silver and Bi2Se3 topological insulator at room temperature Katja Ferfolja , Matjaz Valant , Iuliia Mikulska , Sandra Gardonio , Mattia Fanetti The Journal Of Physical Chemistry C DOI: 10.1021/acs.jpcc.8b01543 Show Abstract ▼ Abstract: Understanding an interaction at an interface between a topological insulator and a metal is of critical importance when designing electronic and spintronic devices or when such systems are used in catalysis. In this paper, we report on a chemical instability of the interface between Bi2Se3 and Ag studied by X-Ray Powder Diffraction and Electron Microscopy. We present strong experimental evidence of a redox solid-state reaction occurring at the interface with kinetics that is significant already at room temperature. The reaction yields Ag2Se, AgBiSe2 and Bi. The unexpected room-temperature chemical instability of the interface should be considered for all future theoretical and applicative studies involving the interface between Bi2Se3 and Ag.	Apr 2018

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