In Situ X-RAY Diffraction Studies of Li+ Insertion into V6O13

1992 ◽  
Vol 293 ◽  
Author(s):  
C. Lampe-Önnerud ◽  
T. Gustafsson ◽  
J.O. Thomas
Keyword(s):  
Structural Changes ◽  
Open Circuit ◽  
Line Broadening ◽  
X Ray Diffraction ◽  
X Ray ◽  
Gradual Loss ◽  
Set Up ◽  
Insertion Process ◽  
Reflection Intensity

AbstractA fast in situ X-ray powder diffraction set-up working in transmission mode is used to explore the structural changes occurring on Li+ insertion into the active V6O13 component of the cathode in a thin-film < Li I polymer electrolyte | V6O13 > battery. It is confirmed that the V6O13 is indeed converted reversibly into three discrete phases, LixV6O13 for x = 1, 4 and 8, as the fully charged cell (ca. 3.OV) is discharged to 1.8V. The effect on the insertion process of repeated cycling with different currents has been studied. Cell collapse was induced after ca. 35 cycles for 0.2 mA/cm2. This was not reflected, however, in any significant change in the diffraction pattern from the battery. Moreover, the battery returned to normal functioning after lying on open circuit for 7 days. A gradual loss of reflection intensity is observed, but no particle line-broadening. The implications of these results are discussed as they relate to the nature of the solid-state insertion process of Li+ into V6O13.

scholarly journals High temperature structural study of decagonal Al-Cu-Rh quasicrystal.

2014 ◽  
Vol 70 (a1) ◽  
pp. C94-C94
Author(s):  
Pawel Kuczera ◽  
Walter Steurer
Keyword(s):  
Structural Changes ◽  
Configurational Entropy ◽  
Lattice Vibrations ◽  
X Ray Diffraction ◽  
Stabilization Mechanism ◽  
X Ray ◽  
Comparative Structure ◽  
The Stability

The structure of d(ecagonal)-Al-Cu-Rh has been studied as a function of temperature by in-situ single-crystal X-ray diffraction in order to contribute to the discussion on energy or entropy stabilization of quasicrystals (QC) [1]. The experiments were performed at 293 K, 1223 K, 1153 K, 1083 K, and 1013 K. A common subset of 1460 unique reflections was used for the comparative structure refinements at each temperature. The results obtained for the HT structure refinements of d-Al-Cu-Rh QC seem to contradict a pure phasonic-entropy-based stabilization mechanism [2] for this QC. The trends observed for the ln func(I(T1 )/I(T2 )) vs.|k⊥ |^2 plots indicate that the best on-average quasiperiodic order exists between 1083 K and 1153 K, however, what that actually means is unclear. It could indicate towards a small phasonic contribution to entropy, but such contribution is not seen in the structure refinements. A rough estimation of the hypothetic phason instability temperature shows that it would be kinetically inaccessible and thus the phase transition to a 12 Å low T structure (at ~800 K) is most likely not phason-driven. Except for the obvious increase in the amplitude of the thermal motion, no other significant structural changes, in particular no sources of additional phason-related configurational entropy, were found. All structures are refined to very similar R-values, which proves that the quality of the refinement at each temperature is the same. This suggests, that concerning the stability factors, some QCs could be similar to other HT complex intermetallic phases. The experimental results clearly show that at least the ~4 Å structure of d-Al-Cu-Rh is a HT phase therefore entropy plays an important role in its stabilisation mechanism lowering the free energy. However, the main source of this entropy is probably not related to phason flips, but rather to lattice vibrations, occupational disorder unrelated to phason flips like split positions along the periodic axis.

Size dependent behavior of Fe3O4crystals during electrochemical (de)lithiation: an in situ X-ray diffraction, ex situ X-ray absorption spectroscopy, transmission electron microscopy and theoretical investigation

2017 ◽  
Vol 19 (31) ◽  
pp. 20867-20880 ◽  
Author(s):  
David C. Bock ◽  
Christopher J. Pelliccione ◽  
Wei Zhang ◽  
Janis Timoshenko ◽  
K. W. Knehr ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Structural Changes ◽  
Ex Situ ◽  
X Ray Diffraction ◽  
X Ray ◽  
Size Dependent ◽  
Transmission Electron ◽  
Dependent Behavior ◽  
X Ray Absorption

Crystal and atomic structural changes of Fe3O4upon electrochemical (de)lithiation were determined.

scholarly journals In situ X-ray diffraction computed tomography studies examining the thermal and chemical stabilities of working Ba0.5Sr0.5Co0.8Fe0.2O3−δ membranes during oxidative coupling of methane

2020 ◽  
Vol 22 (34) ◽  
pp. 18964-18975
Author(s):  
Dorota Matras ◽  
Antonis Vamvakeros ◽  
Simon D. M. Jacques ◽  
Vesna Middelkoop ◽  
Gavin Vaughan ◽  
...  
Keyword(s):  
Computed Tomography ◽  
Solid State ◽  
Oxidative Coupling ◽  
Structural Changes ◽  
Oxidative Coupling Of Methane ◽  
Membrane Reactors ◽  
Solid State Chemistry ◽  
X Ray Diffraction ◽  
X Ray

In situ XRD-CT and post-reaction SEM/EDX were used to study the solid-state chemistry and structural changes of Ba0.5Sr0.5Co0.8Fe0.2O3−δ membrane reactors during the oxidative coupling of methane reaction.

Study of Structural Changes in LiNi0.8Co0.1Mn0.1O2 Cathode Material for Lithium-Ion Batteries by X-Ray Diffraction Analysis in the In Situ Mode

2019 ◽  
Vol 92 (7) ◽  
pp. 1013-1019 ◽  
Author(s):  
P. A. Novikov ◽  
A. E. Kim ◽  
K. A. Pushnitsa ◽  
Wang Quingsheng ◽  
M. Yu. Maksimov ◽  
...  
Keyword(s):  
Cathode Material ◽  
Diffraction Analysis ◽  
Lithium Ion Batteries ◽  
Structural Changes ◽  
Lithium Ion ◽  
X Ray Diffraction ◽  
X Ray

Structural changes of Ce–Pr–O oxides in hydrogen: a study by in situ X-ray diffraction and Raman spectroscopy

2003 ◽  
Vol 13 (12) ◽  
pp. 3017-3020 ◽  
Author(s):  
Sylvie Rossignol ◽  
Francois Gérard ◽  
Danielle Mesnard ◽  
Charles Kappenstein ◽  
Daniel Duprez
Keyword(s):  
Raman Spectroscopy ◽  
Structural Changes ◽  
X Ray Diffraction ◽  
X Ray

A scanning Kelvin probe for synchrotron investigations: thein situdetection of radiation-induced potential changes

2011 ◽  
Vol 19 (1) ◽  
pp. 48-53 ◽  
Author(s):  
Bekir Salgin ◽  
Dirk Vogel ◽  
Diego Pontoni ◽  
Heiko Schröder ◽  
Bernd Schönberger ◽  
...  
Keyword(s):  
High Performance ◽  
Structural Changes ◽  
Kelvin Probe ◽  
X Ray ◽  
Scanning Kelvin Probe ◽  
Wide Range ◽  
First Results ◽  
Radiation Induced ◽  
Set Up

A wide range of high-performance X-ray surface/interface characterization techniques are implemented nowadays at every synchrotron radiation source. However, these techniques are not always `non-destructive' because possible beam-induced electronic or structural changes may occur during X-ray irradiation. As these changes may be at least partially reversible, anin situtechnique is required for assessing their extent. Here the integration of a scanning Kelvin probe (SKP) set-up with a synchrotron hard X-ray interface scattering instrument for thein situdetection of work function variations resulting from X-ray irradiation is reported. First results, obtained on bare sapphire and sapphire covered by a room-temperature ionic liquid, are presented. In both cases a potential change was detected, which decayed and vanished after switching off the X-ray beam. This demonstrates the usefulness of a SKP forin situmonitoring of surface/interface potentials during X-ray materials characterization experiments.

Kinetics of high-pressure mineral phase transformations using in situ time-resolved X-ray diffraction in the Paris-Edinburgh cell: a practical guide for data acquisition and treatment

2008 ◽  
Vol 72 (2) ◽  
pp. 683-695 ◽  
Author(s):  
J. P. Perrillat
Keyword(s):  
High Pressure ◽  
Phase Transformations ◽  
Kinetic Studies ◽  
X Ray Diffraction ◽  
Time Resolved ◽  
X Ray ◽  
Practical Guide ◽  
Set Up ◽  
Isothermal Kinetic

AbstractSynchrotron X-ray diffraction (XRD) is a powerful technique to study in situ and in real-time the structural and kinetic processes of pressure-induced phase transformations. This paper presents the experimental set-up developed at beamline ID27 of the ESRF to perform time-resolved angle dispersive XRD in the Paris-Edinburgh cell. It provides a practical guide for the acquisition of isobaric-isothermal kinetic data and the construction of transformation-time plots. The interpretation of experimental data in terms of reaction mechanisms and transformation rates is supported by an overview of the kinetic theory of solid-solid transformations, with each step of data processing illustrated by experimental results of relevance to the geosciences. Reaction kinetics may be affected by several factors such as the sample microstructure, impurities or differential stress. Further high-pressure kinetic studies should investigate the influence of such processes, in order to acquire kinetic information more akin to natural or technological processes.

Structural changes during tensile testing of an all-cellulose composite by in situ synchrotron X-ray diffraction

2006 ◽  
Vol 66 (15) ◽  
pp. 2639-2647 ◽  
Author(s):  
Wolfgang Gindl ◽  
Klaus J. Martinschitz ◽  
Peter Boesecke ◽  
Jozef Keckes
Keyword(s):  
Tensile Testing ◽  
Structural Changes ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cellulose Composite

Investigating temperature-induced structural changes of lead halide perovskites by in situ X-ray powder diffraction

2019 ◽  
Vol 52 (5) ◽  
pp. 1104-1118
Author(s):  
Rocco Caliandro ◽  
Davide Altamura ◽  
Benny Danilo Belviso ◽  
Aurora Rizzo ◽  
Sofia Masi ◽  
...  
Keyword(s):  
Multivariate Analysis ◽  
Structural Changes ◽  
Lattice Distortion ◽  
Data Matrix ◽  
Cubic Phase ◽  
X Ray Diffraction ◽  
Temperature Variations ◽  
Temperature Changes ◽  
X Ray

In situ X-ray diffraction experiments offer a unique opportunity to investigate structural dynamics at atomic resolution, by collecting several patterns in an appropriate time sequence (data matrix) while varying the applied stimulus (e.g. temperature changes). Individual measurements can be processed independently by refinement procedures that are based on prior knowledge of the average structure of each crystal phase present in the sample. If the refinement converges, parameters of the average structural model can be assessed and studied as a function of the stimulus variations. An alternative approach consists in applying a multivariate analysis to the data matrix as a whole. Methods such as principal component analysis (PCA) and phase-sensitive detection perform fast, blind and model-independent calculations that can be used for on-site analysis to identify trends in data actually related to the applied stimulus. Both classical and multivariate approaches are here applied to the in situ X-ray diffraction pair distribution function (PDF) setup on two samples of the hybrid perovskite methylammonium (MA) lead iodide obtained by different synthetic routes, subjected to temperature variations. The PDF refinement allows assessing the occurrence of temperature-induced rotations of the PbI6 octahedra and variations in the relative amount of MAPbI3 and intermediate PbI2–MAI–DMSO (dimethyl sulfoxide) crystal phases. A change in the orientation of the methylammonium molecule with temperature is also characterized. Results of the multivariate analysis tools, which include a newly introduced space-dependent variant of PCA, are described, interpreted and validated against simulated data, and their specificity and relation to refinement results are highlighted. The interaction between nearby octahedra is identified as the driving force for the tetragonal-to-cubic phase transition, and three fundamental trends in data having different temperature behaviours are unveiled: (i) irreversible weight-fraction variations of the MAPbI3 and PbI2–MAI–DMSO phases; (ii) reversible structural changes related to the MAPbI3 crystalline phase and its lattice distortion in the ab plane, having the same frequency as the temperature variations; (iii) reversible lattice distortion along the c axis, occurring at twice the frequency of the temperature changes.

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