The
use of a catalyst support for the design of nanoscale heterogeneous
catalysts based on cerium oxide offers vast possibilities for future
catalyst development, particularly with regard to an increased focus
on the use of renewable biogas and an emerging hydrogen economy. In
this study, zirconia-supported ceria catalysts were synthesized, activated
by using different thermochemical treatments, and characterized by
way of temperature-programmed reduction (TPR), oxygen storage capacity,
X-ray diffraction, electron microscopy, and luminescence spectroscopy
using Eu3+ as a spectroscopic probe. Through reduction–oxidation
pretreatment routines, reactive pyrochlore structures were created
at temperatures as low as 600 °C and identified through TPR and
electron microscopy experiments. A structural relationship and alignment
of the crystal planes is revealed in high-resolution scanning transmission
electron microscopy experiments through the digital diffraction patterns.
Low-temperature pretreatment induces the formation of reactive pyrochlore
domains under retention of the surface area of the catalyst system,
and no further morphological changes are detected. Furthermore, the
formation of pyrochlore domains achieved through severe reduction
and mild reoxidation (SRMO) treatments is reversible. Over multiple
alternating SRMO and severe reduction and severe reoxidation (SRSO)
treatments, europium spectroscopy and TPR results indicate that pyrochlore
structures are recreated over consecutive treatments, whenever the
mild oxidation step at 500 °C is the last treatment (SRMO, SRMO–SRSO–SRMO,
etc.).