Issue 6, 2013

Synthesis and characterization of terephthalate-intercalated NiAl layered double hydroxides with high Al content

Abstract

Terephthalate-intercalated nickel–aluminum layered double hydroxides (LDHs) were prepared by a co-precipitation method, with nominal x values in the general formula Ni(1−x)Alx(OH)2(C8H4O4)x/2 in the range 0.3–0.8. The materials were characterized by X-ray diffraction, X-ray fluorescence spectroscopy, CHN analysis, thermogravimetric analysis, FTIR spectroscopy, EXAFS at the Ni edge and 27Al NMR spectroscopy. A combination of XRD, XRF and CHN analysis indicated that crystalline LDHs with true x values up to 0.5 were obtained, along with increasing segregation of an aluminum hydroxide phase with increasing aluminum content. The EXAFS analysis indicated an upper limit of ca. 0.6 for the atomic fraction of aluminum at the second nickel coordination sphere. The 27Al NMR analysis suggested that a phase containing octahedrally co-ordinated Al3+ is segregated for nominal x values from 0.6 upwards.

Graphical abstract: Synthesis and characterization of terephthalate-intercalated NiAl layered double hydroxides with high Al content

Supplementary files

Article information

Article type
Paper
Submitted
09 Jul 2012
Accepted
08 Nov 2012
First published
08 Nov 2012

Dalton Trans., 2013,42, 2084-2093

Synthesis and characterization of terephthalate-intercalated NiAl layered double hydroxides with high Al content

S. Arias, J. G. Eon, R. A. S. San Gil, Y. E. Licea, L. A. Palacio and A. C. Faro, Dalton Trans., 2013, 42, 2084 DOI: 10.1039/C2DT31502E

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