Mechanistic and Kinetic Studies of Guest Ion Intercalation into Layered Double Hydroxides Using Time-resolved, In-situ X-ray Powder Diffraction

Author(s):  
Gareth R. Williams ◽  
Aamir I. Khan ◽  
Dermot O'Hare
2010 ◽  
Vol 43 (3) ◽  
pp. 434-447 ◽  
Author(s):  
Rune E. Johnsen ◽  
Frank Krumeich ◽  
Poul Norby

Anion-exchange processes in cobalt–aluminium layered double hydroxides (LDHs) were studied byin situsynchrotron X-ray powder diffraction (XRPD). The processes investigated were CoAl–CO3→ CoAl–Cl → CoAl–CO3, CoAl–Cl → CoAl–NO3and CoAl–CO3→ CoAl–SO4. The XRPD data show that the CoAl–CO3→ CoAl–Cl process is a two-phase transformation, where the amount of the CoAl–CO3phase decreases exponentially while that of the CoAl–Cl phase increases exponentially. Energy-dispersive X-ray spectroscopy (EDXS) studies of a partially chloride-exchanged CoAl–CO3LDH sample along within situXRPD data suggested that the individual particles in the CoAl–CO3sample are generally anion-exchanged with chloride one at a time. In contrast with the CoAl–CO3→ CoAl–Cl transformation, the XRPD data show that the reverse CoAl–Cl → CoAl–CO3process is a one-phase transformation. Rietveld refinements indicate that the occupancy factors of the carbon and oxygen sites of the carbonate group increase, while that of the chloride site decreases. In the CoAl–Cl → CoAl–NO3anion-exchange reaction, the XRPD patterns reveal the existence of two intermediate phases in addition to the initial CoAl–Cl and final CoAl–NO3phases. Thein situdata indicate that one of these intermediates is a mixed nitrate- and chloride-based LDH phase, where the disorder decreases as the nitrate content increases. The XRPD data of the partial CoAl–CO3→ CoAl–SO4anion-exchange reaction show that the process is a two-phase transformation involving a sulfate-containing LDH with a 1H polytype structure.


2020 ◽  
Author(s):  
Luzia S. Germann ◽  
Sebastian T. Emmerling ◽  
Manuel Wilke ◽  
Robert E. Dinnebier ◽  
Mariarosa Moneghini ◽  
...  

Time-resolved mechanochemical cocrystallisation studies have so-far focused solely on neat and liquid-assisted grinding. Here, we report the monitoring of polymer-assisted grinding reactions using <i>in situ</i> X-ray powder diffraction, revealing that reaction rate is almost double compared to neat grinding and independent of the molecular weight and amount of used polymer additives.<br>


2008 ◽  
Vol 72 (2) ◽  
pp. 683-695 ◽  
Author(s):  
J. P. Perrillat

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.


2006 ◽  
Vol 42 (2) ◽  
pp. 534-538 ◽  
Author(s):  
Daniel X. Gouveia ◽  
Odair P. Ferreira ◽  
Antonio G. Souza Filho ◽  
M. G. da Silva ◽  
J. A. C. de Paiva ◽  
...  

2019 ◽  
Vol 4 (4) ◽  
pp. 101
Author(s):  
Neza Rahayu Palapa ◽  
Bakri Rio Rahayu ◽  
Tarmizi Taher ◽  
Aldes Lesbani ◽  
Risfidian Mohadi

Zn/Al and Zn/Fe layered double hydroxides has successfully synthesized by co-precipitation methods with molar ration 3:1. The samples were characterized using X-Ray Diffraction, Fourier Transform Infrared Spectroscopy and Surface Area using BET method. In this study, Zn/Al and Zn/Fe layered double hydroxides were used to remove direct yellow dye in aqueous solution. The experiments were carried out time variations with the aim of observing the kinetic studies. The results showed that the adsorption of direct yellow onto Zn/Al and Zn/Fe layered double hydroxides based on co-efficient correlation kinetic models more fit using pseudo-second-order than pseudo-first-order.


ChemInform ◽  
2006 ◽  
Vol 37 (11) ◽  
Author(s):  
Giuseppe M. Lombardo ◽  
Giuseppe C. Pappalardo ◽  
Francesco Punzo ◽  
Ferdinando Costantino ◽  
Umberto Costantino ◽  
...  

1997 ◽  
pp. 521-522 ◽  
Author(s):  
Robin J. Francis ◽  
Stephen J. Price ◽  
Stephen O’Brien ◽  
Andrew M. Fogg ◽  
Dermot O’Hare ◽  
...  

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