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211 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	High‐throughput discovery of a rhombohedral twelve‐connected zirconium‐based metal‐organic framework with ordered terephthalate and fumarate linkers Adam M. Tollitt , Rebecca Vismara , Luke M. Daniels , Dmytro Antypov , Michael W. Gaultois , Alexandros Katsoulidis , Matthew Rosseinsky Angewandte Chemie International Edition DOI: 10.1002/anie.202108150 Open Access Show Abstract ▼ Abstract: We report a metal-organic framework where an ordered array of two linkers with differing length and geometry connect [Zr 6 (OH) 4 O 4 ] 12+ clusters into a twelve-connected fcu net that is rhombohedrally distorted from cubic symmetry. The ordered binding of equal numbers of terephthalate and fumarate ditopic carboxylate linkers at the trigonal antiprismatic Zr 6 core creates close-packed layers of fumarate-connected clusters that are connected along the single remaining threefold axis by terephthalates. This well-defined linker arrangement retains the three-dimensional porosity of the Zr cluster-based UiO family while creating two distinct windows within the channels that define two distinct guest diffusion paths. The ordered material is accessed by a restricted combination of composition and process parameters that were identified by high-throughput synthesis.	Sep 2021
I15-Extreme Conditions	Pressure-induced chemical decomposition of copper orthovanadate (α-Cu3V2O8) Daniel Díaz-Anichtchenko , Robin Turnbull , Enrico Bandiello , Simone Anzellini , Srungarpu Nagabhusan Achary , Daniel Errandonea Journal Of Materials Chemistry C 43 DOI: 10.1039/D1TC02901K Diamond Proposal Number(s): [21610] Show Abstract ▼ Abstract: The high pressure stability of α-Cu3V2O8 has been investigated via complementary high pressure synchrotron X-ray diffraction experiments and theoretical density functional theory calculations. The results of both experiment and theory are in close agreement. The main result of this work is that α-Cu3V2O8 undergoes a pressure-induced chemical decomposition into CuO and V2O5 at a modest pressure of ∼1.35 GPa according to the experimental observations, and at ∼2.45 GPa according to the calculations. The decomposition is investigated with enthalpy calculations and one of the main driving factors is the stability of the octhedral oxygen-coordination of the metal atoms in the decompositon products. Additionally, we determine the bulk modulus of α-Cu3V2O8 to be the lowest of all known vanadates, at 52(2) GPa, due to its crystal structure, and determine the corresponding isothermal compressibility tensor.	Sep 2021
I11-High Resolution Powder Diffraction	Hole and electron doping of topochemically reduced Ni(I)/Ru(II) insulating ferromagnetic oxides Zheying Xu , Lun Jin , Julius-Konstantin Backhaus , Felicity Green , Michael A. Hayward Inorganic Chemistry 2 DOI: 10.1021/acs.inorgchem.1c02265 Diamond Proposal Number(s): [13284] Show Abstract ▼ Abstract: LaxSr2–xNiRuO6, LaxSr4–xNiRuO8, and LaxSr3–xNiRuO7 are, respectively, the n = ∞, 1, and 2 members of the (Lax/2Sr1–(x/2))nSr(Ni0.5Ru0.5)nO3n+1 compositional series. Reaction with CaH2, in the case of the LaxSr2–xNiRuO6 perovskite phases, or Zr oxygen getters in the case of the LaxSr4–xNiRuO8 and LaxSr3–xNiRuO7 Ruddlesden–Popper phases, yields the corresponding topochemically reduced (Lax/2Sr1–(x/2))nSr(Ni0.5Ru0.5)nO3n–1 compounds (LaxSr2–xNiRuO4, LaxSr4–xNiRuO6, and LaxSr3–xNiRuO5), which contain Ni and Ru cations in square-planar coordination sites. The x = 1 members of each series (LaSrNiRuO4, LaSr3NiRuO6, and LaSr2NiRuO5) exhibit insulating ferromagnetic behavior at low temperature, attributable to exchange couplings between the Ni1+ and Ru2+ centers they contain. Increasing the La3+ concentration (x > 1) leads to a reduction of some of the Ru2+ centers to Ru1+ centers and a suppression of the ferromagnetic state (lower Tc, reduced saturated ferromagnet moment). In contrast, increasing the Sr2+ concentration (x < 1) oxidizes some of the Ru2+ centers to Ru3+ centers and enhances the ferromagnetic coupling (increased Tc, increased saturated ferromagnet moment) for the n = ∞ and n = 2 samples but appears to have no influence on the magnetic ordering temperature of the n = 1 samples. The magnetic couplings and influence of doping are discussed on the basis of superexchange and direct exchange couplings between the square-planar Ni and Ru centers.	Sep 2021
I11-High Resolution Powder Diffraction I12-JEEP: Joint Engineering, Environmental and Processing	Intercalates of Bi2Se3 studied in situ by time-resolved powder X-ray diffraction and neutron diffraction Machteld E. Kamminga , Simon J. Cassidy , Partha P. Jana , Mahmoud Elgaml , Nicola D. Kelly , Simon J. Clarke Dalton Transactions 7 DOI: 10.1039/D1DT00960E Diamond Proposal Number(s): [18786, 20375] Open Access Show Abstract ▼ Abstract: Intercalation of lithium and ammonia into the layered semiconductor Bi2Se3 proceeds via a hyperextended (by >60%) ammonia-rich intercalate, to eventually produce a layered compound with lithium amide intercalated between the bismuth selenide layers which offers scope for further chemical manipulation.	Aug 2021
I11-High Resolution Powder Diffraction	Directed synthesis of a hybrid improper magnetoelectric multiferroic material Tong Zhu , Fabio Orlandi , Pascal Manuel , Alexandra S. Gibbs , Weiguo Zhang , P. Shiv Halasyamani , Michael A. Hayward Nature Communications 12 DOI: 10.1038/s41467-021-25098-1 Diamond Proposal Number(s): [13284] Open Access Show Abstract ▼ Abstract: Preparing materials which simultaneously exhibit spontaneous magnetic and electrical polarisations is challenging as the electronic features which are typically used to stabilise each of these two polarisations in materials are contradictory. Here we show that by performing low-temperature cation-exchange reactions on a hybrid improper ferroelectric material, Li2SrTa2O7, which adopts a polar structure due to a cooperative tilting of its constituent TaO6 octahedra rather than an electronically driven atom displacement, a paramagnetic polar phase, MnSrTa2O7, can be prepared. On cooling below 43 K the Mn2+ centres in MnSrTa2O7 adopt a canted antiferromagnetic state, with a small spontaneous magnetic moment. On further cooling to 38 K there is a further transition in which the size of the ferromagnetic moment increases coincident with a decrease in magnitude of the polar distortion, consistent with a coupling between the two polarisations.	Aug 2021
I11-High Resolution Powder Diffraction I19-Small Molecule Single Crystal Diffraction	Structural and electronic effects of X-ray irradiation on prototypical [M(COD)Cl]2 catalysts Nathalie K. Fernando , Andrew B. Cairns , Claire A. Murray , Amber L. Thompson , Joshua L. Dickerson , Elspeth F. Garman , Nayera Ahmed , Laura E. Ratcliff , Anna Regoutz The Journal Of Physical Chemistry A DOI: 10.1021/acs.jpca.1c05759 Diamond Proposal Number(s): [19420, 22705] Show Abstract ▼ Abstract: X-ray characterization techniques are invaluable for probing material characteristics and properties, and have been instrumental in discoveries across materials research. However, there is a current lack of understanding of how X-ray-induced effects manifest in small molecular crystals. This is of particular concern as new X-ray sources with ever-increasing brilliance are developed. In this paper, systematic studies of X-ray–matter interactions are reported on two industrially important catalysts, [Ir(COD)Cl]2 and [Rh(COD)Cl]2, exposed to radiation in X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) experiments. From these complementary techniques, changes to structure, chemical environments, and electronic structure are observed as a function of X-ray exposure, allowing comparisons of stability to be made between the two catalysts. Radiation dose is estimated using recent developments to the RADDOSE-3D software for small molecules and applied to powder XRD and XPS experiments. Further insights into the electronic structure of the catalysts and changes occurring as a result of the irradiation are drawn from density functional theory (DFT). The techniques combined here offer much needed insight into the X-ray-induced effects in transition-metal catalysts and, consequently, their intrinsic stabilities. There is enormous potential to extend the application of these methods to other small molecular systems of scientific or industrial relevance.	Aug 2021
I11-High Resolution Powder Diffraction	Size-distribution of irradiation-induced dislocation-loops in materials used in the nuclear industry Tamás Ungár , Philipp Frankel , Gábor Ribárik , Christopher P. Race , Michael Preuss Journal Of Nuclear Materials 550 DOI: 10.1016/j.jnucmat.2021.152945 Diamond Proposal Number(s): [8395, 10006] Show Abstract ▼ Abstract: Neutron or proton irradiation induced dislocation loops in Zr and its alloys are usually characterized by electron microscopy methods. In plastically deformed materials X-ray line profile analysis (XLPA) is now a well-established tool to determine dislocation densities (DDs) with excellent agreement between XLPA and TEM analysis. In irradiated zirconium alloys, however, XLPA determined DDs are often considerably larger than those obtained by TEM. In ion irradiated Cu and W it was shown that X-ray diffraction or MD simulations give significantly larger dislocation loop densities than conventional TEM analysis, which suggests that the smallest loops remain undetected by TEM. Based on these results we developed a new methodology to determine power-law size-distributions of irradiation-induced dislocation loops. We assume that only loops larger than a certain threshold are fully counted in TEM micrographs, whereas XLPA detects all the loops in the entire size range. This new analysis procedure shows that in neutron irradiated Zircaloy-2 in the channel-box materials the total DD is larger than in the cladding materials, even though TEM counting shows the opposite. We also found that there is a correlation between the reciprocal square-root of loop DDs and the diameter of loops. Our work shows that irradiation induced loop-formation and irradiation-damage in general can be better determined when we combine TEM investigations with XLPA.	Jul 2021
I11-High Resolution Powder Diffraction	Compositional flexibility in Li–N–H materials: implications for ammonia catalysis and hydrogen storage Joshua W. Makepeace , Jake M. Brittain , Alisha Sukhwani Manghnani , Claire A. Murray , Thomas J. Wood , William I. F. David Physical Chemistry Chemical Physics 420 DOI: 10.1039/D1CP02440J Diamond Proposal Number(s): [14926] Open Access Show Abstract ▼ Abstract: Li–N–H materials, particularly lithium amide and lithium imide, have been explored for use in a variety of energy storage applications in recent years. Compositional variation within the parent lithium imide, anti-fluorite crystal structure has been related to both its facile storage of hydrogen and impressive catalytic performance for the decomposition of ammonia. Here, we explore the controlled solid-state synthesis of Li–N–H solid-solution anti-fluorite structures ranging from amide-dominated (Li4/3(NH2)2/3(NH)1/3 or Li1.333NH1.667) through lithium imide to majority incorporation of lithium nitride–hydride (Li3.167(NH)0.416N0.584H0.584 or Li3.167NH). Formation of these solid solutions is demonstrated to cause significant changes to the thermal stability and ammonia reactivity of the samples, highlighting the potential use of compositional variation to control the properties of the material in gas storage and catalytic applications.	Jul 2021
I11-High Resolution Powder Diffraction	Structural features in some layered hybrid copper chloride perovskites: ACuCl4 or A2CuCl4 Ceng Han , Alasdair J. Bradford , Alexandra M. Z. Slawin , Bela E. Bode , Edoardo Fusco , Stephen L. Lee , Chiu C. Tang , Philip Lightfoot Inorganic Chemistry DOI: 10.1021/acs.inorgchem.1c00705 Diamond Proposal Number(s): [23579] Show Abstract ▼ Abstract: We present three new hybrid copper(II) chloride layered perovskites of generic composition ACuCl4 or A2CuCl4, which exhibit three distinct structure types. (m-PdH2)CuCl4 (m-PdH22+ = protonated m-phenylenediamine) adopts a Dion–Jacobson (DJ)-like layered perovskite structure type and exhibits a very large axial thermal contraction effect upon heating, as revealed via variable-temperature synchrotron X-ray powder diffraction (SXRD). This can be attributed to the contraction of an interlayer block, via a slight repositioning of the m-PdH22+ moiety. (3-AbaH)2CuCl4 (3-AbaH+ = protonated 3-aminobenzoic acid) and (4-AbaH)2CuCl4 (4-AbaH+ = protonated 4-aminobenzoic acid) possess the same generic formula as Ruddlesden–Popper (RP) layered perovskites, A2BX4, but adopt different structures. (4-AbaH)2CuCl4 adopts a near-staggered structure type, whereas (3-AbaH)2CuCl4 adopts a near-eclipsed structure type, which resembles the DJ rather than the RP family. (3-AbaH)2CuCl4 also displays static disorder of the [CuCl4]∞ layers. The crystal structures of each are discussed in terms of the differing nature of the templating molecular species, and these are compared to related layered perovskites. Preliminary magnetic measurements are reported, suggesting dominant ferromagnetic interactions.	Jul 2021
I11-High Resolution Powder Diffraction	Cation ordering and exsolution in copper‐containing forms of the flexible zeolite Rho (Cu,M‐Rho; M = H, Na) and their consequences for CO2 adsorption Magdalena Lozinska , Sophie Jamieson , Maarten Verbraeken , David Miller , Bela Bode , Claire Murray , Stefano Brandani , Paul Anthony Wright Chemistry – A European Journal DOI: 10.1002/chem.202101664 Diamond Proposal Number(s): [22322] Show Abstract ▼ Abstract: The flexibility of the zeolite Rho framework offers great potential for tunable molecular sieving. The fully copper-exchanged form of Rho and mixed Cu,H- and Cu,Na-forms have been prepared. EPR spectroscopy reveals Cu 2+ cations are present in the dehydrated forms and Rietveld refinement shows these prefer S6R sites, away from the d8r windows that control diffusion. Fully exchanged Cu-Rho remains in an open form upon dehydration, the d8r windows remain nearly circular and the occupancy of window sites is low, so that it adsorbs CO 2 rapidly at room temperature. Breakthrough tests with 10% CO 2 /40% CH 4 mixtures show that Cu 4.9 -Rho is able to produce pure methane, albeit with a relatively low capacity at this p CO2 due to the weak interaction of CO 2 with Cu cations. This is in strong contrast with Na-Rho, where cations in narrow elliptical window sites enable CO 2 to be adsorbed with high selectivity and uptake but too slowly to enable the production of pure methane in similar breakthrough experiments. A series of Cu,Na-Rho materials was prepared to improve uptake and selectivity compared to Cu-Rho, and kinetics compared to Na-Rho. Remarkably, Cu,Na-Rho with >2 Cu cations per unit cell exhibited exsolution, due to the preference of Na cations for narrow S8R sites in distorted Rho and of Cu cations for S6R sites in the centric, open form of Rho. The exsolved Cu,Na-Rho showed improved performance in CO 2 /CH 4 breakthrough tests, producing pure CH 4 with improved uptake and CO 2 /CH 4 selectivity compared to that of Cu 4.9 -Rho.	Jul 2021

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