HREM Studies of Structural Changes Induced by Phase Transformations in Zirconia Powders
The use of microcrystalline (submicron) and nanocrystalline (≤10nm) particles as powder materials for sintering of advanced ceramics like oxide-based ceramics or high-Tc superconductors , requires new techniques for characterization. Thus classical optical microscopy or even scanning electron microscopy are no longer effective for examination of 1-10 nm particles. In previous work we developed quantitative analysis of transmission electron microscopy (TEM) observations at medium resolution (0.4-1 nm, typically) to study morphology, size distribution, agglomeration and/or aggregation state of elementary powder particles characterized by bright- and dark - field imaging as well as diffraction TEM techniques.Here the high resolution TEM (HREM) techniques (at 200 kV) have been used to investigate phase transformations occuring in ultrafine zirconia powders processed by calcination of an amorphous hydrated zirconium oxide prepared at low temperature. X-ray examination showed the sequence : amorphous , cubic (C) or tetragonal (T) , monoclinic (M), at increasing temperatures.