Pol Vilas G, Thiyagarajan P, Moreno Jose M Calderon, Popa Monica, Kessler Vadim G, Gohil Suresh, Seisenbaeva Gulaim A
IPNS, Argonne National Laboratory, Argonne, IL 60439, USA.
Chem Asian J. 2009 Jul 6;4(7):1084-91. doi: 10.1002/asia.200900077.
The tetragonal BaTiO(3) nanopowder 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 degrees 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 HR-SEM, 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 as-prepared BaCO(3) with amorphous Ti phase.
通过在封闭反应器中于700℃自生压力下热解单一前驱体[Ba₂Ti₂(thd)₄(OnPr)₈(nPrOH)₂],随后进行燃烧,以无溶剂、高效的工艺合成了四方相的BaTiO₃纳米粉末。本文汇编了[Ba₂Ti₂(thd)₄(OnPr)₈(nPrOH)₂]前驱体的合成、其质谱分析以及通过可控高效热分解制备介电四方相BaTiO₃纳米粉末的实施过程。通过XRD、拉曼光谱和EDS测量系统地分析了所得纳米材料的初始、中间和最终形式,以获取结构和成分信息。采用高分辨率扫描电子显微镜(HR-SEM)、透射电子显微镜(TEM)和高分辨率透射电子显微镜(HR-TEM)技术,追踪了所有相结构演变过程中的形态变化。基于对初始[Ba₂Ti₂(thd)₄(OnPr)₈(nPrOH)₂]反应物以及制备的具有非晶态Ti相的BaCO₃获得的热重分析(TGA)和差示热分析(DTA)数据,对BaTiO₃纳米粉末的制备机理进行了阐释。