In-situ TEM analysis of the reduction of nanometre-sized Mn3O4 precipitates in a metal matrix Original Research Article

The objective of the present work is the in-situ study of the transformation of small oxide precipitates in a metal matrix by conventional and high-resolution transmission electron microscopy (HRTEM). As an example the reduction of Mn3O4 into MnO for nano-sized oxide precipitates in a silver matrix was studied in detail. A convenient method for monitoring the reduction process is shown for a large number of precipitates simultaneously. It is based on two-beam dark-field images showing distinct Moiré patterns for the MnO and the various types of Mn3O4 precipitates embedded within an Ag matrix. A controlling factor of the transformation kinetics appeared to be the rate in which the system can relax the strains due to the accompanying volume reduction of the precipitates. Other interesting aspects of the Mn3O4 to MnO transformation scrutinized and explained were the shape change of the precipitates upon reduction and the fact that mixed Mn3O4/MnO precipitates were only detected within a small temperature/time interval. Ostwald ripening of the MnO precipitates was observed as well.