We develop a coprecipitation synthesis route to prepare NbVO(5) with simple oxide Nb(2)O(5) and NH(4)VO(3) as starting materials. No metal alkoxide or organometallic substance was used in the process. Nano-crystal NbVO(5) was obtained by calcination of the coprecipitates at 550 °C for 2 h. DSC/TG and XRD investigations indicate that the target compound NbVO(5) is completely formed up to 504.5 °C and is thermally stable below 658 °C. Rietveld XRD refinements give an orthorhombic structure with space group Pnma and lattice parameters, a=11.8453(2), b=5.5126(3) and c=6.9212(2) Å, respectively. In particular, HTXRD determinations show a negative thermal expansion in NbVO(5) with a TEC of -6.63 × 10(-6) °C(-1) in the temperature range of RT-600 °C. This fact is ascribed to the tilting of NbO(6) octahedra and VO(4) tetrahedra in the flexible framework structure. The present synthesis route is facile and easy to be extended to prepare analogues such as TaVO(5), etc.
© The Royal Society of Chemistry 2011