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
2014 ◽  
Vol 70 (a1) ◽  
pp. C94-C94
Author(s):  
Pawel Kuczera ◽  
Walter Steurer

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.


2017 ◽  
Vol 19 (31) ◽  
pp. 20867-20880 ◽  
Author(s):  
David C. Bock ◽  
Christopher J. Pelliccione ◽  
Wei Zhang ◽  
Janis Timoshenko ◽  
K. W. Knehr ◽  
...  

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


2020 ◽  
Vol 22 (34) ◽  
pp. 18964-18975
Author(s):  
Dorota Matras ◽  
Antonis Vamvakeros ◽  
Simon D. M. Jacques ◽  
Vesna Middelkoop ◽  
Gavin Vaughan ◽  
...  

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.


2019 ◽  
Vol 92 (7) ◽  
pp. 1013-1019 ◽  
Author(s):  
P. A. Novikov ◽  
A. E. Kim ◽  
K. A. Pushnitsa ◽  
Wang Quingsheng ◽  
M. Yu. Maksimov ◽  
...  

2003 ◽  
Vol 13 (12) ◽  
pp. 3017-3020 ◽  
Author(s):  
Sylvie Rossignol ◽  
Francois Gérard ◽  
Danielle Mesnard ◽  
Charles Kappenstein ◽  
Daniel Duprez

2019 ◽  
Vol 52 (5) ◽  
pp. 1104-1118
Author(s):  
Rocco Caliandro ◽  
Davide Altamura ◽  
Benny Danilo Belviso ◽  
Aurora Rizzo ◽  
Sofia Masi ◽  
...  

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.


2006 ◽  
Vol 524-525 ◽  
pp. 523-528 ◽  
Author(s):  
Jean Philippe Mathieu ◽  
Denis Bouscaud ◽  
Karim Inal ◽  
Sophie Berveiller ◽  
Olivier Diard

This paper reports experimental characterisation of stress heterogeneities in a French RPV bainitic steel (16MND5) determined by X-Ray diffraction during in-situ tensile testing at low temperature (until –150°C). Results are compared successfully to simulation results, obtained by post-processing of Finite Elements computations of realistic 3D aggregates.


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