Mechanochemical synthesis and intercalation of Ca(II)Fe(III)-layered double hydroxides

Journal Article · Thu Jan 14 23:00:00 EST 2016 · Journal of Solid State Chemistry

DOI:https://doi.org/10.1016/J.JSSC.2015.10.038· OSTI ID:22577737

Ferencz, Zs.; Szabados, M.; Varga, G.; Csendes, Z. ^[1]; Kukovecz, Á. ^[2]; Kónya, Z. ^[2]; Carlson, S. ^[3]; Sipos, P. ^[4]; others, and

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1. Department of Organic Chemistry, University of Szeged, Dóm tér 8, Szeged H-6720 (Hungary)
2. Department of Applied and Environmental Chemistry, University of Szeged, Rerrich Béla tér 1, Szeged H-6720 (Hungary)
3. MAX IV Laboratory, Ole Römers väg 1, Lund SE-223 63 (Sweden)
4. Materials and Solution Structure Research Group, Institute of Chemistry, University of Szeged, Aradi Vértanúk tere 1, Szeged H-6720 (Hungary)

A mechanochemical method (grinding the components without added water – dry grinding, followed by further grinding in the presence of minute amount of water or NaOH solution – wet grinding) was used in this work for the preparation and intercalation of CaFe-layered double hydroxides (LDHs). Both the pristine LDHs and the amino acid anion (cystinate and tyrosinate) intercalated varieties were prepared by the two-step grinding procedure in a mixer mill. By systematically changing the conditions of the preparation method, a set of parameters could be determined, which led to the formation of close to phase-pure LDH. The optimisation procedure was also applied for the intercalation processes of the amino acid anions. The resulting materials were structurally characterised by a range of methods (X-ray diffractometry, scanning electron microscopy, energy dispersive analysis, thermogravimetry, X-ray absorption and infra-red spectroscopies). It was proven that this simple mechanochemical procedure was able to produce complex organic–inorganic nanocomposites: LDHs intercalated with amino acid anions. - Graphical abstract: Amino acid anion-Ca(II)Fe(III)-LDHs were successfully prepared by a two-step milling procedure. - Highlights: • Synthesis of pristine and amino acid intercalated CaFe-LDHs by two-step milling. • Identifying the optimum synthesis and intercalation parameters. • Characterisation of the samples with a range of instrumental methods.

• OSTI ID: 22577737
• Journal Information: Journal of Solid State Chemistry, Journal Name: Journal of Solid State Chemistry Vol. 233; ISSN 0022-4596; ISSN JSSCBI
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
77 NANOSCIENCE AND NANOTECHNOLOGY
ABSORPTION
ANIONS
CLATHRATES
CYSTINE
GRINDING
MILLING
NANOCOMPOSITES
SCANNING ELECTRON MICROSCOPY
SODIUM HYDROXIDES
SPECTROSCOPY
SYNTHESIS
THERMAL GRAVIMETRIC ANALYSIS
TYROSINE
WATER
X RADIATION
X-RAY DIFFRACTION