ISSN 2321-807X 3097 | Page November 16, 2014 New acetate-intercalated CoNiFe, ZnNiFe and CoZnFe layered double hydroxides: Synthesis by forced hydrolysis in polyol medium and characterization Nawal Drici Setti *a, b , Zoubir Derriche b , Noureddine Jouini a a Laboratoire des sciences des procédés et des matériaux, CNRS-LSPM, UPR 3407 université paris 13, Sorbonne Paris Cité, 99 Avenue Jean- Baptiste Clément, 93430 Villetaneuse, France. jouini@univ-paris13.fr b Laboratoire de physico-chimie des matériaux, catalyse et environnement LPCMCE, Université des Sciences et de Technologie « Mohamed Boudiaf » d’Oran, USTO-MB, M’Nouar 1505, Oran 31000, Algérie drici_nawel@yahoo.fr (*Corresponding author) , derriche_zoubir@yahoo.com ABSTRACT New layered double hydroxides (LDHs) CoNiFe, ZnNiFe and CoZnFe with M II /M III molar ratio of 3, with acetate ions in the interlayer region have been prepared by forced hydrolysis in polyol medium. The physico-chemical properties of all products were characterized by the methods of powder X-ray Diffraction, Infrared Spectroscopy, UV-Spectroscopy, Elemental analysis, Thermal analysis, Transmission Electron Microscopy and Scanning Electron Microscopy. It was found that all compounds present the typical features of hydrotalcite-like structure and exhibit a turbostratic character. The insertion of acetate anions into LDHs was confirmed and the interlayer spacing values were respectively 12.47, 13.64 and 14.69 Å for CoNiFe, ZnNiFe and CoZnFe. We notice a difference between the interlayer spacing for all synthesized phases with and without zinc. This can be explained by a structural modification on the level of the layers and/ or different arrangement from the inserted species (anions + water) in the interlayer space for zinc materials. 57 Fe Mössbauer spectrometry allows concluding the presence of Fe 3+ cations which occupy octahedral sites and confirming the absence of Fe 2+ in the as-prepared compounds. Keywords Layered Double Hydroxide; Polyol; Forced Hydrolysis; Anionic Exchange; Chemical synthesis; X-ray diffraction; Mössbauer spectrometry Academic Discipline And Sub-Disciplines Solid State Chemistry – Layered Materials SUBJECT CLASSIFICATION Chemistry Subject Classification TYPE (METHOD/APPROACH) Experimental study- synthesis method Council for Innovative Research Peer Review Research Publishing System Journal: Journal of Advances in Chemistry Vol. 10, No. 9 editorjaconline@gmail.com www.cirjac.com