I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[11204]
Abstract: The fracture resistance of load-bearing trabecular bone is adversely affected by diseases such as osteoporosis. However, there are few published measurements of trabecular bone fracture toughness due to the difficulty of conducting reliable tests in small specimens of this highly porous material. A new approach is demonstrated that uses digital volume correlation of X-ray computed tomographs to measure 3D displacement fields in which the crack shape and size can be objectively identified using a phase congruency analysis. The criteria for crack propagation, i.e. fracture toughness, can then be derived by finite element simulation, with knowledge of the elastic properties.
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Sep 2020
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I09-Surface and Interface Structural Analysis
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Diamond Proposal Number(s):
[21742]
Open Access
Abstract: Amorphous tin-gallium oxide (a-SGO) grown with atomic layer deposition was evaluated as a buffer layer in (Ag,Cu)(In,Ga)Se2 thin-film solar cells in search for a new material that is compatible with a variety of absorber band gaps. Hard and soft X-ray photoelectron spectroscopy on absorber/a-SGO stacks combined with J–V characterization of solar cells that were fabricated, showed that the conduction band alignment at the absorber/a-SGO interface can be tuned by varying the cation composition and/or growth temperature. Here, the surface band gap was 1.1 eV for the absorber. However, optical band gap data for a-SGO indicate that a suitable conduction band alignment can most likely be achieved even for wider absorber band gaps relevant for tandem top cells. A best efficiency of 17.0% was achieved for (Ag,Cu)(In,Ga)Se2/a-SGO devices, compared to η = 18.6% for the best corresponding CdS reference. Lower fill factor and open-circuit voltage values were responsible for lower cell efficiencies. The reduced fill factor is explained by a larger series resistance, seemingly related to interface properties, which are yet to be optimized. Some layer constellations resulted in degradation in fill factor during light soaking as well. This may partly be explained by light-induced changes in the electrical properties of a-SGO, according to analysis of Al/SGO/n-Si metal-oxide-semiconductor capacitors that were fabricated and characterized with J–V and C–V. Moreover, the introduction of a 1 nm thick Ga2O3 interlayer between the absorber and a-SGO improved the open-circuit voltage, which further indicates that the absorber/a-SGO interface can be improved.
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Sep 2020
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I05-ARPES
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Alfred J. H.
Jones
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Ryan
Muzzio
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Paulina
Majchrzak
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Sahar
Pakdel
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Davide
Curcio
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Klara
Volckaert
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Deepnarayan
Biswas
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Jacob
Gobbo
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Simranjeet
Singh
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Jeremy T.
Robinson
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Kenji
Watanabe
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Takashi
Taniguchi
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Timur K.
Kim
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Cephise
Cacho
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Nicola
Lanata
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Jill A.
Miwa
,
Philip
Hofmann
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Jyoti
Katoch
,
Soeren
Ulstrup
Diamond Proposal Number(s):
[24072]
Abstract: The possibility of triggering correlated phenomena by placing a singularity
of the density of states near the Fermi energy remains an intriguing avenue toward engineering the properties of quantum materials. Twisted bilayer gra- phene is a key material in this regard because the superlattice produced by the rotated graphene layers introduces a van Hove singularity and flat bands near the Fermi energy that cause the emergence of numerous correlated phases, including superconductivity. Direct demonstration of electrostatic control of the superlattice bands over a wide energy range has, so far, been critically missing. This work examines the effect of electrical doping on the electronic band structure of twisted bilayer graphene using a back-gated device archi- tecture for angle-resolved photoemission measurements with a nano-focused light spot. A twist angle of 12.2° is selected such that the superlattice Brillouin zone is sufficiently large to enable identification of van Hove singularities and flat band segments in momentum space. The doping dependence of these fea- tures is extracted over an energy range of 0.4 eV, expanding the combinations of twist angle and doping where they can be placed at the Fermi energy and thereby induce new correlated electronic phases in twisted bilayer graphene.
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Jun 2020
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B18-Core EXAFS
I15-1-X-ray Pair Distribution Function (XPDF)
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Diamond Proposal Number(s):
[16168, 16460]
Abstract: Perovskite‐like NaNbO3‐Bi1/3NbO3 solid solutions are studied to understand the interactions between octahedral rotations, which dominate the structural behavior of NaNbO3 and displacive disorder of Bi present in Bi1/3NbO3. Models of instantaneous structures for representative compositions are obtained by refining atomic coordinates against X‐ray total scattering and extended X‐ray‐absorption fine structure data, with additional input obtained from transmission electron microscopy. A mixture of distinct cations and vacancies on the cuboctahedral A‐sites in Na1−3x Bix NbO3 (x ≤ 0.2) results in 3D nanoscale modulations of structural distortions. This phenomenon is determined by the inevitable correlations in the chemical composition of adjacent unit cells according to the structure type—an intrinsic property of any nonmolecular crystals. Octahedral rotations become suppressed as x increases. Out‐of‐phase rotations vanish for x > 0.1, whereas in‐phase tilts persist up to x = 0.2, although for this composition their correlation length becomes limited to the nanoscale. The loss of out‐of‐phase tilting is accompanied by qualitative changes in the probability density distributions for Bi and Nb, with both species becoming disordered over loci offset from the centers of their respective oxygen cages. Symmetry arguments are used to attribute this effect to different strengths of the coupling between the cation displacements and out‐of‐phase versus in‐phase rotations. The displacive disorder of Bi and Nb combined with nanoscale clustering of lattice distortions are primarily responsible for the anomalous broadening of the temperature dependence of the dielectric constant.
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Jun 2020
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I07-Surface & interface diffraction
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Diamond Proposal Number(s):
[14937]
Abstract: In this study in situ wide angle X-ray scattering (WAXS) has been measured during the spin coating process used to make the precursor films required for the formation of thin films of perovskite. A customized hollow axis spin coater was developed to permit the scattered X-rays to be collected in transmission geometry during the deposition process. Spin coating is the technique most commonly used in laboratories to make thin perovskite films. The dynamics of spin casting MAPbI3-xClx and FAPbI3-xClx films have been investigated and compared to investigate the differences between the dynamics of MAPbI3-xClx and FAPbI3-xClx film formation. In particular we focus on the crystallization dynamics of the precursor film formation. When casting MAPbI3-xClx we observed relatively fast 1D crystallization of the intermediate product MA2PbI3Cl. There was an absence of the desired perovskite phase formed directly; it only appeared after an annealing step which converted the MA2PbI3Cl to MAPbI3. In contrast, slower crystallization via a 3D precursor was observed for FAPbI3-xClx film formation compared to MAPbI3-xClx. Another important finding was that some FAPbI3-xClx perovskite was generated directly during spin casting before annealing. These findings indicate that there are significant differences between the crystallization pathways for these two perovskite materials. These are likely to explain the differences in the lifetime of the resulting perovskite solar cell devices produced using FA and MA cations.
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Jun 2020
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I22-Small angle scattering & Diffraction
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Diamond Proposal Number(s):
[18563]
Abstract: Solvent vapour annealing (SVA) is a common post-processing technique used to increase the average grain size of lead halide perovskite films and thus enhance device performance. The prevailing wisdom is that large grain perovskite films lead to enhanced stability, however, we observed the reverse in CH3NH3PbI3 (MAPbI3) with dimethylformamide vapour treatment compared to non-SVA controls. Using a range of microstructural characterisation techniques, we reveal that SVA is not a chemically benign grain-growth process, but leads to substantial stoichiometric changes in the perovskite films. Intrinsic material degradation is investigated under external loading with in situ X-ray scattering, and combined with lifetime testing on full devices. We show that the operational stability of SVA devices greatly depends on the initial stoichiometry of the MAPbI3 with PbI2-excess compositions being least stable. However, the incorporation of excess organic-halides in the precursor solution helps to mitigate the deleterious effects of SVA on device stability. This work critically re-evaluates current thinking around grain structure and stoichiometry in achieving long-term stability for perovskite solar cells.
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Jun 2020
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Zilu
Liu
,
Tianjun
Liu
,
Christopher N.
Savory
,
José P.
Jurado
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Juan Sebastián
Reparaz
,
Jianwei
Li
,
Long
Pan
,
Charl F. J.
Faul
,
Ivan P.
Parkin
,
Gopinathan
Sankar
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Satoru
Matsuishi
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Mariano
Campoy‐quiles
,
David O.
Scanlon
,
Martijn A.
Zwijnenburg
,
Oliver
Fenwick
,
Bob C.
Schroeder
Open Access
Abstract: Organometallic coordination polymers (OMCPs) are a promising class of thermoelectric materials with high electrical conductivities and thermal resistivities. The design criteria for these materials, however, remain elusive and so far material modifications have been focused primarily on the nature of the metal cation to tune the thermoelectric properties. Herein, an alternative approach is described by synthesizing new organic ligands for OMCPs, allowing modulation of the thermoelectric properties of the novel OMCP materials over several orders of magnitude, as well as controlling the polarity of the Seebeck coefficient. Extensive material purification combined with spectroscopy experiments and calculations furthermore reveal the charge‐neutral character of the polymer backbones. In the absence of counter‐cations, the OMCP backbones are composed of air‐stable, ligand‐centered radicals. The findings open up new synthetic possibilities for OMCPs by removing structural constraints and putting significant emphasis on the molecular structure of the organic ligands in OMCP materials to tune their thermoelectric properties.
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Jun 2020
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I15-1-X-ray Pair Distribution Function (XPDF)
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Abstract: The crystal structure of the organic pigment 2-monomethyl-quinacridone (Pigment Red 192, C21H14N2O2) was solved from X-ray powder diffraction data. The resulting average structure is described in space group [P\overline 1], Z = 1 with the molecule on the inversion centre. The molecules are arranged in chains. The molecules, which have no inversion symmetry, show orientational head-to-tail disorder. In the average structure, the methyl group is disordered and found on both ends of the molecule with an occupancy of 0.5 each. The disorder and the local structure were investigated using various ordered structural models. All models were analysed by three approaches: Rietveld refinement, structure refinement to the pair distribution function (PDF) and lattice-energy minimization. All refinements converged well. The Rietveld refinement provided the average structure and gave no indication of a long-range ordering. The refinement to the PDF turned out to be very sensitive to small structural details, giving insight into the local structure. The lattice-energy minimizations revealed a significantly preferred local ordering of neighbouring molecules along the [0[\bar 1]1] direction. In conclusion, all methods indicate a statistical orientational disorder with a preferred parallel orientation of molecules in one direction. Additionally, electron diffraction revealed twinning and faint diffuse scattering.
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Jun 2020
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I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[19533]
Abstract: Capillary driven ink infiltration through a porous powder bed in 3D binderjet printing (inkjet printing onto a powder bed) controls the printing resolution and as-printed ‘green’ strength of the resulting object. However, a full understanding of the factors controlling the kinetics of the infiltration remains incomplete. Here, high resolution in situ synchrotron radiography provides time resolved imaging of the penetration of an aqueous solution of eythylene glycol through a porous alumina powder bed, used as a model system. A static drop-on-demand inkjet printer was used to dispense liquid droplets onto a powder surface. The subsequent migration of the liquid front and its interactions with powder particles was tracked using fast synchrotron X-radiography in the Diamond Synchrotron, with phase contrast imaging at a frame rate of 500 Hz. Image processing and analysis reveal both the time dependent increment in the wetting area and the propagation of the ‘interface leading edge’ exhibit heterogeneous behavior in both the temporal and spatial domain. However, mean infiltration kinetics are shown to be consistent with existing infiltration models based on the Washburn equation modified to account for the spreading of the liquid drop on the powder surface and using a modified term for the bed porosity.
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Jun 2020
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Benedetto
Bozzini
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Alessandra
Gianoncelli
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Georgios
Kourousias
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Marco
Boniardi
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Andrea
Casaroli
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Simone Dal
Zilio
,
Rafaqat
Hussain
,
Majid
Kazemian Abyaneh
,
Maya
Kiskinova
,
Claudio
Mele
,
Sandra
Tedeschi
,
Gian Pietro
De Gaudenzi
Abstract: The corrosion control of WC-Co type hardmetals is steadily gaining momentum for novel crucial applications in the Oil & Gas and food industries. The corrosion rate of the Co-based binder, and the extent to which coupling to WC speeds it up, are strongly influenced by alloying. In this paper, we investigate the impact of Cr on the corrosion-product film formation of Co- and CoNi based hardmetal binders in acidic, neutral and alkaline aqueous solutions. We centred our study on the role of Cr in driving the distribution of oxidized Co and Ni at the micrometre scale, thanks to synchrotron-based soft-X ray microspectroscopy. We have investigated morphochemical distributions for the following grades: Co96Cr4, Co48Ni48Cr4, Co50Cr50. Chemical-state mapping has been complemented by electrochemical measurements and metallographic observations. Amounts of Cr and Ni of ca. 50% notably increase the corrosion resistance in all ambients, with a stronger beneficial effect of the former element. 4% addition of Cr results in slight positive effects, with the exception of the CoNi system in alkaline ambient, that, together with Co50Cr50, outperforms the other grades. In all investigated alloy-ambient combinations, a continuous oxidized metal film grows, onto which micrometric island form of shape and dimensions that depend on the specific grade and aggressive conditions. Quantitative descriptors of chemical-state maps and their theoretical interpretation in terms of electrochemical phase-formation by oxy-hydroxide precipitation, allow to correlate the island patterns with the degree of pseudopassivation.
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Jun 2020
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