Methodical Thermolysis of [Ba_(2)Ti_(2)(thd)_(4)(OnPr)_(8)(nPrOH)_(2)] under Autogenous Pressure Followed by Combustion for the Synthesis of Dielectric Tetragonal BaTiO_(3) Nanopowder

摘要

The tetragonal BaTiO_(3) nano-powder is synthesized in a solvent-less, efficient process by the thermolysis of a single [Ba_(2)Ti_(2)(thd)_(4)(OnPr)_(8)(nPrOH)_(2)] precursor in a closed reactor at 700 deg C under autogenous pressure, followed by combustion. This paper compiles the synthesis of the [Ba_(2)Ti_(2)(thd)_(4) (OnPr)_(8)(nPrOH)_(2)] precursor, its analysis by mass spectrometry, and implementation for the fabrication of dielectric tetragonal BaTiO_(3) nanopowder by controlled efficient thermal decomposition. The as-prepared, intermediate, and final forms of the obtained nanomaterials are systematically analysed by XRD, Raman, and EDS measurements to gain structural and compositional information. Employing HRSEM, TEM, and HR-TEM techniques, the morphological changes during the structural evolution of all the phases are pursued. The mechanistic elucidation for the fabrication of BaTiO_(3) nanopowder is developed on the basis of TGA and DTA data obtained for the initial [Ba_(2)Ti_(2)(thd)_(4)(OnPr)_(8) (nPrOH)_(2)] reactant as well as the asprepared BaCO_(3) with amorphous Ti phase.