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Dalton Trans. 2014 Feb 21;43(7):2755-63. doi: 10.1039/c3dt52929k.

Synthesis and characterisation of new MO(OH)2 (M = Zr, Hf) oxyhydroxides and related Li2MO3 salts.

Dalton transactions (Cambridge, England : 2003)

Yana V Baklanova, Tatyana A Denisova, Lidiya G Maksimova, Alexander P Tyutyunnik, Inna V Baklanova, Igor R Shein, Reinhard B Neder, Nadezda V Tarakina

Affiliations

  1. Institute of Solid State Chemistry, Ural Branch of the Russian Academy of Sciences, 91 Pervomayskaya str, 620990, Ekaterinburg, Russia. [email protected].

PMID: 24343584 DOI: 10.1039/c3dt52929k

Abstract

Two new solid MO(OH)2 (M = Zr, Hf) oxyhydroxides have been synthesised by an ion-exchange reaction from Li2MO3 (M = Zr, Hf) precursors obtained by a citrate combustion technique. The crystal structure of the oxyhydroxides has been solved by direct methods and refined using Rietveld full profile fitting based on X-ray powder diffraction data. Both oxyhydroxides crystallize in a P2(1)/c monoclinic unit cell and have a structure resembling that of the related salts. Detailed characterisation of the fine-structure features and chemical bonding in precursors and oxyhydroxide powders has been performed using vibrational spectroscopy, nuclear magnetic resonance spectroscopy, scanning electron microscopy, pair distribution function analysis and quantum-chemical modelling.

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