Journal
JOURNAL OF THERMAL ANALYSIS AND CALORIMETRY
Volume 123, Issue 2, Pages 1563-1569Publisher
SPRINGER
DOI: 10.1007/s10973-015-5053-7
Keywords
Thermogravimetric analysis; IR spectroscopy; Metal N, N-dialkylcarbamates; Thermal stability; Nanopowders
Funding
- project PRIN - Italian Ministry of University and Research [2010C4R8M8]
- project FIRB - Italian Ministry of University and Research [RBFR12ETL5]
- project PRA - University of Pisa
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Thermogravimetric analysis coupled with IR spectroscopy was used to investigate the thermal stability and decomposition products of N,N-dialkylcarbamates of zirconium(IV), hafnium(IV), and niobium(IV), M(O2CNR2)(4). The niobium derivatives were less stable than the corresponding Zr(IV) and Hf(IV) derivatives, and the thermal stability was in the order of R = Et > Pr-i > Me. XRD analysis of the residue showed the formation of the oxides ZrO2 (tetragonal, P4 (2) /nmc), HfO2, (monoclinic, P2 (1)/c), and Nb2O5 (orthorhombic, Pbam). TEM analysis showed that all the oxides were obtained as nanopowders with a crystal size below 30 nm.
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