Development of Pore Morphology During Nitrate Group Removal by Calcination of Mesoporous Ce x Zr 1-x-y-z Y y La z O 2-δ Powders.

Here, we present a study of the development of the micro- and mesoporosity of a Ce x Zr 1- x - y - z Y y La z O 2-δ oxygen storage material upon treatment at temperatures up to 1050 °C. The investigated powder, obtained from nitrate-based metal oxide precursors in a specially developed hydrothermal synthesis, is highly crystalline, features a high surface area and does not show phase segregation at high temperatures. By employing an advanced methodology, consisting of state-of-the-art argon physisorption, thermogravimetric analysis coupled with mass spectrometry (TG-MS) and X-ray powder diffraction (XRD) along with Raman spectroscopy, we correlate the stability of the mesopore system to the presence of surface-bound nitrate groups introduced during synthesis, which prevent sintering up to a temperature of 600 °C. In addition, the connectivity of mesopores was further studied by hysteresis scanning within the argon physisorption measurements. These advanced physisorption experiments suggest a three-dimensionally interconnected pore system and, in turn, a 3D network of the material itself on the nanometer scale which appears to be beneficial to endow the mesopore space with enhanced stability against sintering and mesopore collapse once the removal of nitrate groups is completed.