Time resolved in situ X-ray diffraction study of crystallisation processes of large pore nanoporous aluminophosphate materials

2015 ◽  
Vol 177 ◽  
pp. 237-247 ◽  
Author(s):  
Kerry Simmance ◽  
Wouter van Beek ◽  
Gopinathan Sankar

Time resolved high-resolution X-ray powder diffraction was utilized to obtain detailed changes in the crystal structure parameters during the hydrothermal crystallization process of the nanoporous aluminophosphate AlPO-5 (AFI) structure. This in situ study offered not only the influence of metal ions on the onset of crystallization and estimation of the activation energy of the process, but also allowed us to determine in detail the changes in lattice parameters during this process. More importantly the time-resolved study clearly showed the lattice expansion in the divalent metal ions substituted system right from the on-set of crystallization process, compared to the one without any dopant ions, which suggest that an amorphous or poorly crystalline network is formed prior to crystallization that contains the large divalent ions (compared to Al(iii), the substituting element), which is in agreement with the combined XAS/XRD study reported earlier. A mechanism based on this and the earlier study is suggested.

2005 ◽  
Vol 37 (1) ◽  
pp. 27-34 ◽  
Author(s):  
S. Paris ◽  
E. Gaffet ◽  
D. Vrel ◽  
D. Thiaudiere ◽  
M. Gailhanou ◽  
...  

The control of Mechanically Activated Field Activated Pressure Assisted Synthesis hereafter called the MAFAPAS process is the main objective to be achieved for producing nanostructure materials with a controlled consolidation level. Consequently, it was essential to develop characterization tools "in situ" such as the Time Resolved X-ray Diffraction (TRXRD), with an X-ray synchrotron beam (H10, LURE Orsay) coupled to an infrared thermography to study simultaneously structural transformations and thermal evolutions. From the 2003 experiments, we took the opportunity to modify the sample-holder in order to reproduce the better synthesis conditions of the MAFAPAS process, but without the consolidation step. The versatility of the setup has been proved and could even be enhanced by the design of new sample holders. In addition, this work clearly shows that this equipment will allow, on the one hand, to make progress of the understanding of MAFAPAS mechanisms and, on the other hand, to adjust reaction parameters (mechanical activation and combustion synthesis) for producing many materials with an expected microstructure.


RSC Advances ◽  
2017 ◽  
Vol 7 (37) ◽  
pp. 22964-22973 ◽  
Author(s):  
Pei Sheng ◽  
Guofu Wang ◽  
Mei Dong ◽  
Gang Chen ◽  
Huanhuan Yang ◽  
...  

Systematic study of the hydrothermal crystallization process of CrAPO-5 by in situ high resolution X-ray powder diffraction (HRXRD).


Carbon ◽  
2015 ◽  
Vol 87 ◽  
pp. 246-256 ◽  
Author(s):  
Périne Landois ◽  
Mathieu Pinault ◽  
Stéphan Rouzière ◽  
Dominique Porterat ◽  
Cristian Mocuta ◽  
...  

2017 ◽  
Vol 111 (8) ◽  
pp. 082907 ◽  
Author(s):  
Seiji Nakashima ◽  
Osami Sakata ◽  
Hiroshi Funakubo ◽  
Takao Shimizu ◽  
Daichi Ichinose ◽  
...  

2008 ◽  
Vol 72 (1) ◽  
pp. 201-204 ◽  
Author(s):  
A. Sumoondur ◽  
S. Shaw ◽  
I. Ahmed ◽  
L. G. Benning

AbstractIn this study, direct evidence for the formation of magnetite via a green rust intermediate is reported. The Fe(II) induced transformation of ferrihydrite, was quantified in situ and under O2-free conditions using synchrotron-based time-resolved energy dispersive X-ray diffraction. At pH 9 and Fe(II)/Fe(III) ratios of 0.5 and 1, rapid growth (6 min) of sulphate green rust and its subsequent transformation to magnetite was observed. Electron microscopy confirmed these results, showing the initial rapid formation of hexagonal sulphate green rust particles, followed by the corrosion of the green rust as magnetite growth occurred, indicating that the reaction proceeds via a dissolution-reprecipitation mechanism. At pH 7 and Fe(II)/Fe(III) ratio of 0.5, sulphate green rust was the stable phase, with no transformation to magnetite.


1998 ◽  
Vol 21 (4-6) ◽  
pp. 253-262 ◽  
Author(s):  
Dermot O'Hare ◽  
John S.O. Evans ◽  
Robin J. Francis ◽  
P. Shiv Halasyamani ◽  
Poul Norby ◽  
...  

2020 ◽  
Author(s):  
Bikash Garai ◽  
Volodymyr Bon ◽  
Francesco Walenszus ◽  
Azat Khadiev ◽  
Dmitri Novikov ◽  
...  

Variation in the metal centres of M-M paddle-wheel SBU results in the formation of isostructural DUT-49(M) frameworks. However, the porosity of the framework was found to be different for each of the structures. While a high and moderate porosity was obtained for DUT-49(Cu) and DUT-49(Ni), respectively, other members of the series [DUT-49(M); M= Mn, Fe, Co, Zn, Cd] show very low porosity and shapes of the adsorption isotherms which is not expected for op phases of these MOFs. Investigation on those MOFs revealed that those frameworks undergo structural collapse during the solvent removal at the activation step. Thus, herein, we aimed to study the detailed structural transformations that are possibly occurring during the removal of the subcritical fluid from the framework.


2013 ◽  
Vol 117 (8) ◽  
pp. 3915-3922 ◽  
Author(s):  
Xianqin Wang ◽  
Jonathan C. Hanson ◽  
Ja Hun Kwak ◽  
Janos Szanyi ◽  
Charles H. F. Peden

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