How the Method of Synthesis Governs the Local and Global Structure of Zinc Aluminum Layered Double Hydroxides
| Autor: | John V. Hanna, Suraj Shiv Charan Pushparaj, Ulla Gro Nielsen, Vanessa Prevot, Claude Forano, Andrew S. Lipton, Gregory J. Rees |
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| Přispěvatelé: | Department of Physics, Chemistry and Pharmacy, University of Southern Denmark, Campusvej 55, 5230 Odense, Denmark, Institut de Chimie de Clermont-Ferrand (ICCF), Université Blaise Pascal - Clermont-Ferrand 2 (UBP)-SIGMA Clermont (SIGMA Clermont)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Environmental Molecular Sciences Laboratory, Pacific Northwest National Laboratory, Department of Physics, University of Warwick, University of Warwick [Coventry], University of Southern Denmark (SDU) |
| Jazyk: | angličtina |
| Rok vydání: | 2015 |
| Předmět: |
Materials science
Coprecipitation Inorganic chemistry chemistry.chemical_element 02 engineering and technology Zinc engineering.material 010402 general chemistry 01 natural sciences Crystallinity [CHIM]Chemical Sciences Physical and Theoretical Chemistry Layered double hydroxides Nuclear magnetic resonance spectroscopy 021001 nanoscience & nanotechnology 0104 chemical sciences Surfaces Coatings and Films Electronic Optical and Magnetic Materials Amorphous solid General Energy chemistry Chemical engineering Transmission electron microscopy engineering 0210 nano-technology Powder diffraction |
| Zdroj: | Puschparaj, S S C, Forano, C, Prevot, V, Lipton, A S, Rees, G J, Hanna, J V & Nielsen, U G 2015, ' How the Method of Synthesis Governs the Local and Global Structure of Zinc Aluminum Layered Double Hydroxides ', The Journal of Physical Chemistry Part C, vol. 119, no. 49, pp. 27695-27707 . https://doi.org/10.1021/acs.jpcc.5b09490 Journal of Physical Chemistry C Journal of Physical Chemistry C, American Chemical Society, 2015, 119, pp.27695-27707. ⟨10.1021/acs.jpcc.5b09490⟩ Journal of Physical Chemistry C, 2015, 119, pp.27695-27707. ⟨10.1021/acs.jpcc.5b09490⟩ |
| ISSN: | 1932-7447 1932-7455 |
| Popis: | International audience; Seven zinc aluminum layered double hydroxides (ZnAl LDHs), [Zn1–xAlx(OH)2Ax·nH2O], A = NO3–, Cl–, or CO32–, prepared by the urea and coprecipitation synthesis methods were investigated to determine how the synthesis parameters (pH, metal ion concentration, and postsynthesis treatment) affect the local (atomic) and long (global) range structure of the LDH product. Sample composition, purity, crystal defects, and other structural aspects of the LDH products were obtained from powder X-ray diffraction (PXRD), transmission electron microscopy (TEM), micro-Raman, elemental analysis, and solid state 1H, 27Al, and 67Zn NMR spectroscopy. The urea method results in LDHs, which on the global scale are highly crystalline LDHs but disordered on the local scale. The disorder is correlated with the presence of Al-rich phases, which are undetected by bulk techniques (TEM, PXRD), as they are either defects within the LDH particles or separate phase(s) associated with LDHs. In contrast, samples prepared by coprecipitation with careful pH control and hydrothermal treatment have high local order and good crystallinity (large particle size). Our results show that both local (NMR) and bulk techniques are needed to assess the composition of LDHs, as the conventional PXRD and TEM analysis of LDHs failed to identify the many structural defects and/or amorphous phases present. |
| Databáze: | OpenAIRE |
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