Journal
JOURNAL OF PHYSICAL CHEMISTRY C
Volume 119, Issue 49, Pages 27695-27707Publisher
AMER CHEMICAL SOC
DOI: 10.1021/acs.jpcc.5b09490
Keywords
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Funding
- Villum Foundation via the Villum Young Investigator Programme (UGN, SSCP, SSNMR equipment)
- Office of Biological and Environmental Research
- UGN, SSCP, CF
- Clay Mineral Society (USA)
- EPSRC
- University of Warwick
- Birmingham Science City Program
- Advantage West Midlands (AWM)
- European Regional Development Fund (ERDF)
- Villum Fonden [00007169] Funding Source: researchfish
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Seven zinc aluminum layered double hydroxides (ZnAl LDHs), [Zn1-xAlx(OH)(2)A(x)center dot nH(2)O], 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 H-1, Al-27, and Zn-67 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.
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