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34 items found (0 items not approved), displaying 1 to 10.[First/Prev] 1, 2, 3, 4 [Next/Last]

Instruments / Technical Area	Publication Details	Published
I22-Small angle scattering & Diffraction	Gyroid‐nanostructured all‐solid polymer films combining high H+ conductivity with low H2 permeability Tsubasa Kobayashi , Ya‐xin Li , Yuichiro Hirota , Asako Maekawa , Norikazu Nishiyama , Xiang‐bing Zeng , Takahiro Ichikawa Macromolecular Rapid Communications 451 DOI: 10.1002/marc.202100115 Open Access Show Abstract ▼ Abstract: Gyroid‐nanostructured all‐solid polymer films with exceedingly high proton conductivity and low H2 gas permeability have been created via crosslinking polymerization of mixtures of a zwitterionic amphiphilic monomer and a polymerizable imide‐type acid that co‐organize into bicontinuous cubic liquid‐crystalline phases. The gyroid nanostructures are visualized by reconstructing a 3D electron map from the synchrotron X‐ray diffraction patterns. These films exhibit high proton conductivity of the order of 10−1 S cm−1 and extremely low H2 gas permeability of the order of 10−15 mol m m−2 s−1 Pa−1. These properties can be ascribed to the presence of the ionic liquid‐like layer along the gyroid minimal surface. Since these two characteristics are required for improving the performance of proton‐exchange membrane fuel cells, the present membrane design represents a promising strategy for the development of advanced devices, pertinent to establishing sustainable energy sources.	May 2021
I12-JEEP: Joint Engineering, Environmental and Processing	Visualizing plating-induced cracking in lithium-anode solid-electrolyte cells Ziyang Ning , Dominic Spencer Jolly , Guanchen Li , Robin De Meyere , Shengda D. Pu , Yang Chen , Jitti Kasemchainan , Johannes Ihli , Chen Gong , Boyang Liu , Dominic L. R. Melvin , Anne Bonnin , Oxana Magdysyuk , Paul Adamson , Gareth O. Hartley , Charles W. Monroe , James Marrow , Peter G. Bruce Nature Materials 1 DOI: 10.1038/s41563-021-00967-8 Diamond Proposal Number(s): [20795] Show Abstract ▼ Abstract: Lithium dendrite (filament) propagation through ceramic electrolytes, leading to short circuits at high rates of charge, is one of the greatest barriers to realizing high-energy-density all-solid-state lithium-anode batteries. Utilizing in situ X-ray computed tomography coupled with spatially mapped X-ray diffraction, the propagation of cracks and the propagation of lithium dendrites through the solid electrolyte have been tracked in a Li/Li6PS5Cl/Li cell as a function of the charge passed. On plating, cracking initiates with spallation, conical ‘pothole’-like cracks that form in the ceramic electrolyte near the surface with the plated electrode. The spallations form predominantly at the lithium electrode edges where local fields are high. Transverse cracks then propagate from the spallations across the electrolyte from the plated to the stripped electrode. Lithium ingress drives the propagation of the spallation and transverse cracks by widening the crack from the rear; that is, the crack front propagates ahead of the Li. As a result, cracks traverse the entire electrolyte before the Li arrives at the other electrode, and therefore before a short circuit occurs.	Apr 2021
	Oleylamine aging of PtNi nanoparticles giving enhanced functionality for the oxygen reduction reaction Gerard M. Leteba , Yi-Chi Wang , Thomas J. A. Slater , Rongsheng Cai , Conor Byrne , Christopher P. Race , David R. G. Mitchell , Pieter B. J. Levecque , Neil P. Young , Stuart M. Holmes , Alex Walton , Angus I. Kirkland , Sarah J. Haigh , Candace I. Lang Nano Letters DOI: 10.1021/acs.nanolett.1c00706 Open Access Show Abstract ▼ Abstract: We report a rapid solution-phase strategy to synthesize alloyed PtNi nanoparticles which demonstrate outstanding functionality for the oxygen reduction reaction (ORR). This one-pot coreduction colloidal synthesis results in a monodisperse population of single-crystal nanoparticles of rhombic dodecahedral morphology with Pt-enriched edges and compositions close to Pt1Ni2. We use nanoscale 3D compositional analysis to reveal for the first time that oleylamine (OAm)-aging of the rhombic dodecahedral Pt1Ni2 particles results in Ni leaching from surface facets, producing aged particles with concave faceting, an exceptionally high surface area, and a composition of Pt2Ni1. We show that the modified atomic nanostructures catalytically outperform the original PtNi rhombic dodecahedral particles by more than two-fold and also yield improved cycling durability. Their functionality for the ORR far exceeds commercially available Pt/C nanoparticle electrocatalysts, both in terms of mass-specific activities (up to a 25-fold increase) and intrinsic area-specific activities (up to a 27-fold increase).	Apr 2021
B07-C-Versatile Soft X-ray beamline: Ambient Pressure XPS and NEXAFS B18-Core EXAFS	Study of the evolution of FeNxCy and Fe3C species in Fe/N/C catalysts during the oxygen reduction reaction in acid and alkaline electrolyte Álvaro García , Laura Pascual , Pilar Ferrer , Diego Gianolio , Georg Held , David C. Grinter , Miguel A. Peña , Maria Retuerto , Sergio Rojas Journal Of Power Sources 490 DOI: 10.1016/j.jpowsour.2021.229487 Diamond Proposal Number(s): [26554] Open Access Show Abstract ▼ Abstract: The nature and evolution of FeNxCy moieties in Fe/C/N catalysts has been studied by analysing Fe and N environments. TEM and Fe-XAS reveal the presence of FeNx moieties and Fe3C particles in the fresh catalyst. NEXAFS reveals the presence of two groups of (Fe)NxCy ensembles, namely (Fe)Nx-pyridinic and (Fe)Nx-pyrrolic. The architecture of the FeNxCy ensembles and their evolution during the ORR has been analysed by XAS, NEXAFS, and identical locations TEM. NxCy, FeNxCy and Fe3C species are partially removed during the ORR, resulting in the formation of Fe2O3 and Fe3O4 particles with different morphologies. The process is more severe in acid electrolyte than in alkaline one. (Fe)Nx-pyrrolic moieties are the main ones in the fresh catalysts, but (Fe)Nx-pyridinic groups are more stable after the ORR. The correlation between the evolution of the ORR activity and that of the FeNxCy ensembles indicates that FeNx-pyridinic ensembles are responsible for the ORR activity.	Apr 2021
I13-2-Diamond Manchester Imaging	Tracking lithium penetration in solid electrolytes in 3D by in-situ synchrotron X-ray computed tomography Shuai Hao , Sohrab R. Daemi , Thomas M. M. Heenan , Wenjia Du , Chun Tan , Malte Storm , Christoph Rau , Dan J. I. Brett , Paul R. Shearing Nano Energy 82 DOI: 10.1016/j.nanoen.2021.105744 Diamond Proposal Number(s): [22198] Show Abstract ▼ Abstract: Solid state batteries have attracted extensive attention, but the lithium penetration through the solid electrolyte remains a critical barrier to commercialisation and is not yet fully understood. In this study, the 3D morphological evolution of cracks with deposited lithium were tracked as they penetrated through the solid electrolyte during repetitive plating. This is achieved by utilising in-situ synchrotron X-ray computed tomography with high spatial and temporal resolutions. Thin-sheet cracks were observed to penetrate the solid electrolyte without immediate short-circuiting of the cell. Changes in their width and volume were quantified. By calculating the volume of deposited lithium, it was found that the lithium was only partially filled in cracks, and its filling ratio quickly dropped from 94.95% after the 1st plating to ca. 20% after the 4th plating. The filling process was revealed through tracking the line profile of grayscale along cracks. It was found that lithium grew much more slowly than cracks, so that the cracks near the cathode side were largely hollow and the cell could continue to operate. The deposited lithium after short circuit was segmented and its distribution was visualised. DVC analysis was applied to map local high stress and strain, which aggregated along cracks and significantly increased at areas where new cracks formed.	Apr 2021
	Solvent engineered synthesis of layered SnO for high-performance anodes Sonia Jaśkaniec , Seán R. Kavanagh , João Coelho , Seán Ryan , Christopher Hobbs , Aron Walsh , David O. Scanlon , Valeria Nicolosi Npj 2d Materials And Applications 5 DOI: 10.1038/s41699-021-00208-1 Open Access Show Abstract ▼ Abstract: Batteries are the most abundant form of electrochemical energy storage. Lithium and sodium ion batteries account for a significant portion of the battery market, but high-performance electrochemically active materials still need to be discovered and optimized for these technologies. Recently, tin(II) oxide (SnO) has emerged as a highly promising battery electrode. In this work, we present a facile synthesis method to produce SnO microparticles whose size and shape can be tailored by changing the solvent nature. We study the complex relationship between wet-chemistry synthesis conditions and resulting layered nanoparticle morphology. Furthermore, high-level electronic structure theory, including dispersion corrections to account for van der Waals forces, is employed to enhance our understanding of the underlying chemical mechanisms. The electronic vacuum alignment and surface energies are determined, allowing the prediction of the thermodynamically favoured crystal shape (Wulff construction) and surface-weighted work function. Finally, the synthesized nanomaterials were tested as Li-ion battery anodes, demonstrating significantly enhanced electrochemical performance for morphologies obtained from specific synthesis conditions.	Mar 2021
B18-Core EXAFS I20-Scanning-X-ray spectroscopy (XAS/XES)	Surface galvanic formation of Co-OH on Birnessite and its catalytic activity for the oxygen evolution reaction Yayun Pu , Veronica Celorrio , Jöerg M. Stockmann , Oded Sobol , Zongzhao Sun , Wu Wang , Matthew J. Lawrence , Jörg Radnik , Andrea E. Russell , Vasile-Dan Hodoroaba , Limin Huang , Paramaconi Rodriguez Journal Of Catalysis 355 DOI: 10.1016/j.jcat.2021.02.025 Diamond Proposal Number(s): [21659, 19850] Show Abstract ▼ Abstract: Low cost, high-efficient catalysts for water splitting can be potentially fulfilled by developing earth abundant metal oxides. In this work, surface galvanic formation of Co-OH on K0.45MnO2 (KMO) was achieved via the redox reaction of hydrated Co2+ with crystalline Mn4+. The synthesis method takes place at ambient temperature without using any surfactant agent or organic solvent, providing a clean, green route for the design of highly efficient catalysts. The redox reaction resulted in the formation of ultrathin Co-OH nanoflakes with high electrochemical surface area. X-ray adsorption spectroscopy (XAS) and X-ray photoelectron spectroscopy (XPS) analysis confirmed the changes in the oxidation state of the bulk and surface species on the Co-OH nanoflakes supported on the KMO. The effect of the anions, chloride, nitrate and sulfate, on the preparation of the catalyst was evaluated by electrochemical and spectrochemical means. XPS and Time of flight secondary ion mass spectrometry (ToF-SIMS) analysis demonstrated that the layer of CoOxHy deposited on the KMO and its electronic structure strongly depends on the anion of the precursor used during the synthesis of the catalyst. In particular, it was found that Cl favors the formation of Co-OH, changing the rate determining step of the reaction, which enhances the catalytic activity towards the OER, producing the most active OER catalyst in alkaline media.	Mar 2021
I11-High Resolution Powder Diffraction	Synthetic pathway determines the nonequilibrium crystallography of Li- and Mn-rich layered oxide cathode materials Ashok S. Menon , Seda Ulusoy , Dickson O. Ojwang , Lars Riekehr , Christophe Didier , Vanessa K. Peterson , German Salazar-Alvarez , Peter Svedlindh , Kristina Edström , Cesar Pay Gomez , William R. Brant Acs Applied Energy Materials DOI: 10.1021/acsaem.0c03027 Diamond Proposal Number(s): [21804] Open Access Show Abstract ▼ Abstract: Li- and Mn-rich layered oxides show significant promise as electrode materials for future Li-ion batteries. However, an accurate description of its crystallography remains elusive, with both single-phase solid solution and multiphase structures being proposed for high performing materials such as Li1.2Mn0.54Ni0.13Co0.13O2. Herein, we report the synthesis of single- and multiphase variants of this material through sol–gel and solid-state methods, respectively, and demonstrate that its crystallography is a direct consequence of the synthetic route and not necessarily an inherent property of the composition, as previously argued. This was accomplished via complementary techniques that probe the bulk and local structure followed by in situ methods to map the synthetic progression. As the electrochemical performance and anionic redox behavior are often rationalized on the basis of the presumed crystal structure, clarifying the structural ambiguities is an important step toward harnessing its potential as an electrode material.	Feb 2021
B18-Core EXAFS	Identification of C2-C5 products from CO2 hydrogenation over PdZn/TiO2-ZSM-5 hybrid catalysts Jonathan Ruiz Esquius , Hasliza Bahruji , Michael Bowker , Graham Hutchings Faraday Discussions DOI: 10.1039/D0FD00135J Diamond Proposal Number(s): [19850] Open Access Show Abstract ▼ Abstract: The combination of a methanol synthesis catalyst and a solid acid catalyst opens the possibility to obtain olefins or paraffins directly from CO2 and H2 in one step. In this work several PdZn/TiO2-ZSM-5 hybrid catalysts were employed under CO2 hydrogenation conditions (240-360 °C, 20 bar, CO2/N2/H2 = 1/1/3) for the synthesis of CH3OH, consecutive dehydration to dimethyl ether and further oxygenate conversion to hydrocarbons. No significant changes after 36 h reaction on the methanol synthesis catalyst (PdZn/TiO2) were observed by XRD, XAS or XPS. No olefins were observed, indicating that light olefins undergo further hydrogenation under reaction conditions, yielding the corresponding alkanes. Increasing the aluminium sites in the zeolites (Si:Al ratio 80:1, 50:1 and 23:1) lead to a higher concentration of mild Brønstead acid sites promoting hydrocarbon chain growth.	Feb 2021
I15-1-X-ray Pair Distribution Function (XPDF)	Observation of elemental inhomogeneity and its impact on ionic conductivity in Li‐conducting garnets prepared with different synthesis methods J. Mark Weller , Andrew Dopilka , Candace K. Chan Advanced Energy And Sustainability Research DOI: 10.1002/aesr.202000109 Diamond Proposal Number(s): [23152] Open Access Show Abstract ▼ Abstract: Tantalum‐doped lithium lanthanum zirconate garnet (Li7‐xLa3Zr2‐xTaxO12, LLZTO) has received interest as a solid electrolyte for solid‐state lithium batteries due to its good electrochemical properties and ionic conductivity. However, the source of discrepancies for reported values of ionic conductivity in nominally or nearly equivalent compositions of LLZTO is not completely clear. Herein, synthesis‐related factors that may contribute to the differences in performance of garnet electrolytes are systematically characterized. The conductivity of samples with composition Li6.4La3Zr1.4Ta0.6O12 prepared by various methods including solid‐state reaction, combustion, and molten salt synthesis are compared. Varying levels of elemental inhomogeneity, comprising a variation in Ta and Zr‐content on the level of individual LLZTO particles, are identified. The elemental inhomogeneity is found to be largely preserved even after high temperature sintering and correlated with reduced ionic conductivity. We show that the various synthesis and processing‐related variables in each of the preparation methods play a role in these compositional variations, and that even LLZTO synthesized via conventional, high‐temperature solid‐state reaction can exhibit substantial variability in local composition. However, by improving reagent mixing and employing LLZTO powder with low agglomeration and small particle size distribution, the compositional uniformity, and hence ionic conductivity, of sintered garnet electrolytes can be improved.	Feb 2021

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