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463 items found (0 items not approved), displaying 1 to 10.[First/Prev] 1, 2, 3, 4, 5, 6, 7, 8 [Next/Last]

Instruments / Technical Area	Publication Details	Published
I11-High Resolution Powder Diffraction	Layered titanium sulfide cathode for all-solid-state magnesium batteries Lasse N. Skov , Jakob B. Grinderslev , Torben R. Jensen Batteries & Supercaps DOI: 10.1002/batt.202300185 Show Abstract ▼ Abstract: Magnesium solid-state batteries attract significant attention as a future mean of energy storage. Here we present the first cathode study of an inorganic all-solid-state magnesium battery using a magnesium metal anode, a nanocomposite electrolyte Mg(BH4)2·1.6NH3-MgO(75 wt%), and a layered titanium disulfide (TiS2) as cathode active material. The structural transformations of TiS2 particles with different size are investigated at different stages of battery life. Reversible Mg2+ intercalation occurs via three structurally distinct phases of MgxTiS2, identified by powder X-ray diffraction. Magnesium intercalates initially on octahedral sites and at higher depth of discharge on tetrahedral sites in the interlayers of TiS2, which leads to an expansion initially mainly along the c-axis and later along both the a- and c-axes. A maximum discharge capacity of 172 mAh g-1 (Δx = 0.36 in MgxTiS2) is observed for smaller TiS2 particles. Parasitic reactions could be reduced by decreasing the cut-off voltage by a constant current constant voltage cycling procedure. The chemical diffusion coefficient of the entire cell is found from galvanostatic intermittent titration technique experiments to be in the order of 10-15 to 10-19 cm2 s-1.	Jun 2023
	Multi-dimensional characterization of battery materials Ralf F. Ziesche , Thomas M. M. Heenan , Pooja Kumari , Jarrod Williams , Weiqun Li , Matthew E. Curd , Timothy L. Burnett , Ian Robinson , Dan J. L. Brett , Matthias J. Ehrhardt , Paul D. Quinn , Layla B. Mehdi , Philip J. Withers , Melanie Britton , Nigel D. Browning , Paul R. Shearing Advanced Energy Materials 101 DOI: 10.1002/aenm.202300103 Open Access Show Abstract ▼ Abstract: Demand for low carbon energy storage has highlighted the importance of imaging techniques for the characterization of electrode microstructures to determine key parameters associated with battery manufacture, operation, degradation, and failure both for next generation lithium and other novel battery systems. Here, recent progress and literature highlights from magnetic resonance, neutron, X-ray, focused ion beam, scanning and transmission electron microscopy are summarized. Two major trends are identified: First, the use of multi-modal microscopy in a correlative fashion, providing contrast modes spanning length- and time-scales, and second, the application of machine learning to guide data collection and analysis, recognizing the role of these tools in evaluating large data streams from increasingly sophisticated imaging experiments.	May 2023
B18-Core EXAFS	Electrodeposition of manganese dioxide coatings onto graphene foam substrates for electrochemical capacitors Filipe Braga , Gabriel Casano , Luke M. Daniels , Marco Caffio , Laurence J. Hardwick Electrochimica Acta 7 DOI: 10.1016/j.electacta.2023.142433 Diamond Proposal Number(s): [14239] Open Access Show Abstract ▼ Abstract: Optimisation of electrodeposition routes of birnessite manganese dioxide (MnO2) coatings onto 3D graphene foam substrates enabled greater attainable capacitances. Current pulse deposition method resulted in highest achievable areal capacitance of 530 mF/cm2 under a 10 mA/cm2 current rate, cycling performance with 91% retention after 9000 cycles, as well as improved rate capability when compared to the cyclic voltammetry or galvanostatic deposition. Introduction of oxygen functional groups to the graphene foam added initial pseudocapacitance and accelerated the rate for nucleation and growth of the MnO2 crystal grains, resulting in an areal capacitance of 410 mF/cm2 under a 10 mA/cm2 current rate. However, in this case the increase in specific capacitance was accompanied by sluggish kinetic for charge storage seen via impedance spectroscopy. The charge storage mechanism of the deposited MnO2 films was investigated using in situ Raman microscopy and analysis of peak shifts revealed expansion and contraction of birnessite MnO2, relating to exchange of Na+ and H2O at the MnO2 interface.	Apr 2023
I20-EDE-Energy Dispersive EXAFS (EDE)	Structural transformation of metal–organic frameworks and identification of electrocatalytically active species during the oxygen evolution reaction under neutral condition Xiaoqiang Liang , Sen Wang , Jingyu Feng , Zhen Xu , Zhenyu Guo , Hui Luo , Feng Zhang , Wen Chen , Lei Feng , Chengan Wan , Maria-Magdalena Titirici Inorganic Chemistry Frontiers DOI: 10.1039/D2QI02436E Diamond Proposal Number(s): [28663] Show Abstract ▼ Abstract: Electrocatalytic oxygen evolution reaction (OER) under neutral or near-neutral conditions has attracted research interest due to its environmental friendliness and economic sustainability in comparison with currently available acidic and alkaline conditions. However, it is challenging to identify electrocatalytically active species in the OER procedure under neutral environments due to non-crystalline forms of catalysts. Crystalline metal-organic framework (MOF) materials could provide novel insights into electrocatalytical active species because of their well-defined structures. In this study, we synthesized two isostructural two-dimensional (2D) MOFs [Co(HCi)2(H2O)2·2DMF]n (Co-Ci-2D) and [Ni(HCi)2(H2O)2·2DMF]n (Ni-Ci-2D) (H2Ci = 1H-indazole-5-carboxylic acid, DMF = N, N-Dimethyl-formamide) to investigate their OER performance in a neutral environment. Our results indicate that Co-Ci-2D holds a current density of 3.93 mA cm-2 at 1.8 V vs. RHE and a OER durability superior to the benchmark catalyst IrO2. Utilizing the advantages of structural transformation of MOF materials which are easier to characterize and analyze compared to ill-defined amorphous materials, we found out that a mononuclear coordination compound [Co(HCi)2(H2O)4] (Co-Ci-mono-A) and its isomer (Co-Ci-mono-B) were proven to be active species of Co-Ci-2D in the neutral OER process. For Ni-Ci-2D, mononuclear coordination compounds similar to structures of the cobalt material (Ni-Ci-mono-A and Ni-Ci-mono-B) together with NiHPO4 formed by the precipitation were confirmed as active species for the neutral OER catalysis. Additionally, the difference in OER activities between Co-Ci-2D and Ni-Ci-2D, approximately one order of magnitude, originates primarily from the opposite tendency of bond length changes in coordination octahedron after being treated by the PBS solution. These findings contribute to a better comprehension of the OER procedure in the neutral media.	Apr 2023
B18-Core EXAFS	Complex defect chemistry of hydrothermally-synthesized Nb-substituted β′-LiVOPO4 Krystal Lee , Hui Zhou , Mateusz J. Zuba , Carol M. Kaplan , Yanxu Zong , Linna Qiao , Guangwen Zhou , Natasha A. Chernova , Hao Liu , Stanley Whittingham Journal Of Materials Chemistry A DOI: 10.1039/D3TA01152F Open Access Show Abstract ▼ Abstract: Lithium vanadyl phosphate (LiVOPO4) is a next-generation multielectron battery cathode that can intercalate up to two Li-ions per V-ion through the redox couples of V4+/V3+ and V5+/V4+. However, its rate capacity is undermined by the sluggish Li-ion diffusion in the high-voltage region (4 V for V5+/V4+ redox). Nb substitution was used to expand the crystal lattice to facilitate Li-ion diffusion. In this work, Nb substitution was achieved via hydrothermal synthesis, which resulted in a new, lower symmetry β′-LiVOPO4 phase with preferential Nb occupation of one of the two V sites. This phase presents complex defect chemistries, including cation vacancies and hydrogen interstitials, characterized by a combination of X-ray and neutron diffraction, elemental and thermogravimetric analyses, X-ray absorption spectroscopy, and magnetic susceptibility measurements. The Nb-substituted samples demonstrated improved capacity retention and rate capabilities in the high-voltage region, albeit an enlarged voltage hysteresis related to a partial V4+/V3+ redox reaction, as evidenced by ex-situ X-ray absorption spectroscopy and pair distribution function analysis. This work highlights the importance of understanding the complex defect chemistry and its consequence on electrochemistry in polyanionic intercalation compounds.	Apr 2023
B18-Core EXAFS	Template‐ and surfactant‐free room temperature synthesis of Pt/C and Pt–Rh/C nanowires/nanoparticles for ethanol electro‐oxidation Edmundo S. Valério Neto , Caio V. S. Almeida , Haolian Huang , Andrea E. Russell , Katlin I. B. Eguiluz , Giancarlo R. Salazar-Banda Chemcatchem DOI: 10.1002/cctc.202300048 Diamond Proposal Number(s): [15151] Show Abstract ▼ Abstract: The synthesis of Pt–Rh alloy nanowires (NWs) using straightforward methodologies remains a challenge. Here, we report the synthesis of carbon-supported Pt and Pt–Rh nanowire catalysts by chemical reduction at room temperature, without using surfactants or templates. The method of synthesis used yielded Pt/C NWs and a mixture of nanowires with some nanoparticles for the Pt–Rh/C catalysts (characterised using XRD, TEM, EDX, XPS, and XAS). The nanoparticles form due to differences in the surface energy and atomic radius between Pt and Rh. The binary NWs are found to be more active towards ethanol oxidation than the commercial Pt/C reference catalyst. Additionally, the Pt–Rh/C NW catalyst displays a specific activity 2.5-fold higher than the Pt/C NWs and Pt/C reference catalysts after 15 min of chronoamperometric tests (at 0.5 V). Thus, the synthesised carbon-supported Pt NWs and Pt–Rh nanowires-nanoparticles are promising alternatives for direct ethanol fuel cell anodes.	Apr 2023
B18-Core EXAFS	Tuning of oxygen electrocatalysis in perovskite oxide nanoparticles by the cationic composition Madeleine Han , Isabel Gómez-Recio , Daniel Gutiérrez Martín , Nathaly Ortiz Peña , Maria Luisa Ruiz-González , Mohamed Selmane , José M. González-Calbet , Ovidiu Ersen , Andrea Zitolo , Benedikt-Kaiser Lassalle , David Portehault , Christel Laberty-Robert Acs Catalysis 23, 5733 - 5743 DOI: 10.1021/acscatal.3c00461 Diamond Proposal Number(s): [21747] Show Abstract ▼ Abstract: Manganese and cobalt perovskite oxides are among the most active precious metal-free electrocatalysts for the oxygen reduction reaction (ORR) and the oxygen evolution reaction (OER), respectively. Herein, we question the role of the cationic composition and charge state in manganite, cobaltite, and mixed Mn/Co perovskites in the mechanism of oxygen electrocatalysis for ORR and OER. We synthesize in molten salts a range of perovskite nanoparticles active in ORR (single B-site (LaMn)1−γO3 and (La0.7Sr0.3Mn)1−γO3), in OER (single B-site La0.67Sr0.33CoO3−δ), and in both ORR and OER (mixed B-site (LaMn0.6Co0.4)1−γO3). By using operando X-ray absorption spectroscopy coupled to ex situ electron energy loss spectroscopy, we show that Mn and Co in single B-site perovskites undergo changes in oxidation states at the steady state during electrocatalysis, while their oxidation states remain unchanged in the mixed Mn/Co perovskite during OER and ORR. We relate these distinct behaviors to modifications of the rate-determining steps of both the OER and ORR electrocatalytic cycles, triggered by an increased covalency of B–O bonds in the mixed perovskites. These results highlight how simple cationic substitutions, accompanied by a control of cationic vacancies, offer a pathway to tune oxygen electrocatalysis.	Apr 2023
B18-Core EXAFS	Active and durable R2MnRuO7 pyrochlores with low Ru content for acidic oxygen evolution Dmitry Galyamin , Jorge Torrero , Isabel Rodríguez , Manuel J. Kolb , Pilar Ferrer , Laura Pascual , Mohamed Abdel Salam , Diego Gianolio , Veronica Celorrio , Mohamed Mokhtar , Daniel Garcia Sanchez , Aldo Saul Gago , Kaspar Andreas Friedrich , Miguel A. Peña , José Antonio Alonso , Federico Calle-Vallejo , Maria Retuerto , Sergio Rojas Nature Communications 14 DOI: 10.1038/s41467-023-37665-9 Open Access Show Abstract ▼ Abstract: The production of green hydrogen in water electrolyzers is limited by the oxygen evolution reaction (OER). State-of-the-art electrocatalysts are based on Ir. Ru electrocatalysts are a suitable alternative provided their performance is improved. Here we show that low-Ru-content pyrochlores (R2MnRuO7, R = Y, Tb and Dy) display high activity and durability for the OER in acidic media. Y2MnRuO7 is the most stable catalyst, displaying 1.5 V at 10 mA cm−2 for 40 h, or 5000 cycles up to 1.7 V. Computational and experimental results show that the high performance is owed to Ru sites embedded in RuMnOx surface layers. A water electrolyser with Y2MnRuO7 (with only 0.2 mgRu cm−2) reaches 1 A cm−2 at 1.75 V, remaining stable at 200 mA cm−2 for more than 24 h. These results encourage further investigation on Ru catalysts in which a partial replacement of Ru by inexpensive cations can enhance the OER performance.	Apr 2023
B18-Core EXAFS	K2Fe(C2O4)2: an oxalate cathode for Li/Na-ion batteries exhibiting a combination of multielectron cation and anion redox Atin Pramanik , Alexis G. Manche , Moulay Tahar Sougrati , Alan V. Chadwick , Philip Lightfoot , A. Robert Armstrong Chemistry Of Materials DOI: 10.1021/acs.chemmater.3c00063 Diamond Proposal Number(s): [25120] Open Access Show Abstract ▼ Abstract: The development of multielectron redox-active cathode materials is a top priority for achieving high energy density with long cycle life in the next-generation secondary battery applications. Triggering anion redox activity is regarded as a promising strategy to enhance the energy density of polyanionic cathodes for Li/Na-ion batteries. Herein, K2Fe(C2O4)2 is shown to be a promising new cathode material that combines metal redox activity with oxalate anion (C2O42–) redox. This compound reveals specific discharge capacities of 116 and 60 mAh g–1 for sodium-ion batterie (NIB) and lithium-ion batterie (LIB) cathode applications, respectively, at a rate of 10 mA g–1, with excellent cycling stability. The experimental results are complemented by density functional theory (DFT) calculations of the average atomic charges.	Mar 2023
B18-Core EXAFS	Largely pseudocapacitive two-dimensional conjugated metal–organic framework anodes with lowest unoccupied molecular orbital localized in nickel-bis(dithiolene) linkages Panpan Zhang , Mingchao Wang , Yannan Liu , Yubin Fu , Mingming Gao , Gang Wang , Faxing Wang , Zhiyong Wang , Guangbo Chen , Sheng Yang , Youwen Liu , Renhao Dong , Minghao Yu , Xing Lu , Xinliang Feng Journal Of The American Chemical Society 15 DOI: 10.1021/jacs.2c12684 Show Abstract ▼ Abstract: Although two-dimensional conjugated metal–organic frameworks (2D c-MOFs) provide an ideal platform for precise tailoring of capacitive electrode materials, high-capacitance 2D c-MOFs for non-aqueous supercapacitors remain to be further explored. Herein, we report a novel phthalocyanine-based nickel-bis(dithiolene) (NiS4)-linked 2D c-MOF (denoted as Ni2[CuPcS8]) with outstanding pseudocapacitive properties in 1 M TEABF4/acetonitrile. Each NiS4 linkage is disclosed to reversibly accommodate two electrons, conferring the Ni2[CuPcS8] electrode a two-step Faradic reaction with a record-high specific capacitance among the reported 2D c-MOFs in non-aqueous electrolytes (312 F g–1) and remarkable cycling stability (93.5% after 10,000 cycles). Multiple analyses unveil that the unique electron-storage capability of Ni2[CuPcS8] originates from its localized lowest unoccupied molecular orbital (LUMO) over the nickel-bis(dithiolene) linkage, which allows the efficient delocalization of the injected electrons throughout the conjugated linkage units without inducing apparent bonding stress. The Ni2[CuPcS8] anode is used to demonstrate an asymmetric supercapacitor device that delivers a high operating voltage of 2.3 V, a maximum energy density of 57.4 Wh kg–1, and ultralong stability over 5000 cycles.	Mar 2023

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