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Instruments / Technical Area	Publication Details	Published
B07-C-Versatile Soft X-ray beamline: Ambient Pressure XPS and NEXAFS	Revealing the role of CO during CO2 hydrogenation on Cu surfaces with in situ soft X-ray spectroscopy Jack E. N. Swallow , Elizabeth S. Jones , Ashley R. Head , Joshua S. Gibson , Roey Ben David , Michael W. Fraser , Matthijs A. Van Spronsen , Shaojun Xu , Georg Held , Baran Eren , Robert S Weatherup Journal Of The American Chemical Society 10 DOI: 10.1021/jacs.2c12728 Diamond Proposal Number(s): [25834] Open Access Show Abstract ▼ Abstract: The reactions of H2, CO2, and CO gas mixtures on the surface of Cu at 200 °C, relevant for industrial methanol synthesis, are investigated using a combination of ambient pressure X-ray photoelectron spectroscopy (AP-XPS) and atmospheric-pressure near edge X-ray absorption fine structure (AtmP-NEXAFS) spectroscopy bridging pressures from 0.1 mbar to 1 bar. We find that the order of gas dosing can critically affect the catalyst chemical state, with the Cu catalyst maintained in a metallic state when H2 is introduced prior to the addition of CO2. Only on increasing the CO2 partial pressure is CuO formation observed that coexists with metallic Cu. When only CO2 is present, the surface oxidizes to Cu2O and CuO, and the subsequent addition of H2 partially reduces the surface to Cu2O without recovering metallic Cu, consistent with a high kinetic barrier to H2 dissociation on Cu2O. The addition of CO to the gas mixture is found to play a key role in removing adsorbed oxygen that otherwise passivates the Cu surface, making metallic Cu surface sites available for CO2 activation and subsequent conversion to CH3OH. These findings are corroborated by mass spectrometry measurements, which show increased H2O formation when H2 is dosed before rather than after CO2. The importance of maintaining metallic Cu sites during the methanol synthesis reaction is thereby highlighted, with the inclusion of CO in the gas feed helping to achieve this even in the absence of ZnO as the catalyst support.	Mar 2023
B07-B-Versatile Soft X-ray beamline: High Throughput	Nanostructured silicon matrix for materials engineering Poting Liu , Alexander Schleusener , Gabriel Zieger , Arne Bochmann , Matthijs A. Van Spronsen , Vladimir Sivakov Small 4 DOI: 10.1002/smll.202206318 Diamond Proposal Number(s): [31119] Open Access Show Abstract ▼ Abstract: Tin-containing layers with different degrees of oxidation are uniformly distributed along the length of silicon nanowires formed by a top-down method by applying metalorganic chemical vapor deposition. The electronic and atomic structure of the obtained layers is investigated by applying nondestructive surface-sensitive X-ray absorption near edge spectroscopy using synchrotron radiation. The results demonstrated, for the first time, a distribution effect of the tin-containing phases in the nanostructured silicon matrix compared to the results obtained for planar structures at the same deposition temperatures. The amount and distribution of tin-containing phases can be effectively varied and controlled by adjusting the geometric parameters (pore diameter and length) of the initial matrix of nanostructured silicon. Due to the occurrence of intense interactions between precursor molecules and decomposition by-products in the nanocapillary, as a consequence of random thermal motion of molecules in the nanocapillary, which leads to additional kinetic energy and formation of reducing agents, resulting in effective reduction of tin-based compounds to a metallic tin state for molecules with the highest penetration depth in the nanostructured silicon matrix. This effect will enable clear control of the phase distributions of functional materials in 3D matrices for a wide range of applications.	Jan 2023
B07-B-Versatile Soft X-ray beamline: High Throughput B07-C-Versatile Soft X-ray beamline: Ambient Pressure XPS and NEXAFS	The Versatile Soft X-ray (VerSoX) beamline at Diamond Light Source David C. Grinter , Federica Venturini , Pilar Ferrer , Matthijs A. Van Spronsen , Rosa Arrigo , Wilson Quevedo Garzon , Kanak Roy , Alexander I. Large , Santosh Kumar , Georg Held Synchrotron Radiation News 73, 1 - 9 DOI: 10.1080/08940886.2022.2082181 Open Access	Jul 2022
B07-C-Versatile Soft X-ray beamline: Ambient Pressure XPS and NEXAFS	Plasma jet printing induced high-capacity graphite anodes for sustainable recycling of lithium-ion batteries Madhushri Bhar , Avishek Dey , Sourav Ghosh , Matthijs A. Van Spronsen , Vimalnath Selvaraj , Yalamanchili Kaliprasad , Satheesh Krishnamurthy , Surendra K. Martha Carbon 183 DOI: 10.1016/j.carbon.2022.07.027 Diamond Proposal Number(s): [27982] Show Abstract ▼ Abstract: Graphite is an integral part of lithium-ion batteries (LIBs). However, due to limited resources and high production cost of the highly purified (battery grade) graphite are becoming a challenge to meet the ever-increasing demands for energy storage devices. One viable approach is to recycle the spent graphite anodes from end-of-life LIBs. Importantly, recycling of spent lithium-ion batteries (LIBs) is off utmost importance to address the global challenge of electronic waste management. Herein, we present an environment friendly technique of graphite recycling from the spent LIB by water leaching, followed by atmospheric plasma jet printing. The major advantage of this method is that it does not require any binders or conductive diluents. Plasma printed recycled graphite showed significantly enhanced specific capacity of 402 mAh g−1 at 500 mA g−1 at the end of the 1000th charge-discharge cycles, in comparison to with water-washed recycled graphite (112 mAh g−1) and a 23.35 times faster diffusivity of Li+. A detailed experimental investigation revealed the plasma activation of the graphitic structure resulted in the improved reversible Li+ storage. This work provides a new perspective on the recycling strategy of graphite anodes using the in-situ plasma functionalization strategy, a significant step towards the sustainable future of LIBs.	Jul 2022
	Interface sensitivity in electron/ion yield X-ray absorption spectroscopy: The TiO2–H2O interface Matthijs A. Van Spronsen , Xiao Zhao , Maximilian Jaugstetter , Carlos Escudero , Tomas Duchon , Adrian Hunt , Iradwikanari Waluyo , Peidong Yang , Kristina Tschulik , Miquel B. Salmeron The Journal Of Physical Chemistry Letters DOI: 10.1021/acs.jpclett.1c02115 Open Access Show Abstract ▼ Abstract: To understand corrosion, energy storage, (electro)catalysis, etc., obtaining chemical information on the solid–liquid interface is crucial but remains extremely challenging. Here, X-ray absorption spectroscopy (XAS) is used to study the solid–liquid interface between TiO2 and H2O. A thin film (6.7 nm) of TiO2 is deposited on an X-ray-transparent SiNx window, acting as the working electrode in a three-electrode flow cell. The spectra are collected based on the electron emission resulting from the decay of the X-ray-induced core-hole-excited atoms, which we show is sensitive to the solid–liquid interface within a few nm. The drain currents measured at the working and counter electrodes are identical but of opposite sign. With this method, we found that the water layer next to anatase is spectroscopically similar to ice. This result highlights the potential of electron-yield XAS to obtain chemical and structural information with a high sensitivity for the species at the electrode–electrolyte interface.	Oct 2021
	Hydrogen, H2 (g), by near-ambient-pressure soft x-ray synchrotron-radiation photoelectron spectroscopy Christopher R. O'Connor , Jorge Anibal Boscoboinik , Mustafa Karatok , Matthijs A. Van Spronsen Surface Science Spectra 28 DOI: 10.1116/6.0001066 Open Access Show Abstract ▼ Abstract: In this article, we show the survey and H 1s spectra acquired with a photon energy of 400.02 eV and H2(g) electron-energy loss of Ag 3d5/2 spectra with a photon energy of 451.3 eV using high-resolution synchrotron-radiation NAP-XPS.	Jun 2021

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