A new sal-gel synthesis route for rare earth (Ce and Pr) alumina hybrid aero- and xerogels is presented which is based on the so-called epoxide addition method. The resulting materials are characterized by TEM, XRD and nitrogen adsorption. The results reveal a different crystallization behavior for the praseodymia/alumina and the ceria/alumina gel. Whereas the first remains amorphous until 875 degrees C, small ceria domains form already after preparation in the second case which grow with increasing calcination temperature. The use of the calcined gels as CO oxidation catalysts was studied in a quartz tube (lab) reactor and in a (slit) microreactor and compared to reference catalysts consisting of the pure rare earth oxides. The Ce/Al hybrid gels exhibit a good catalytic activity and a thermal stability against sintering which was superior to the investigated reference catalyst. In contrast, the Pr/Al hybrid gels show lower CO oxidation activity which, due to the formation of PrAlO3, decreased with increasing calcination temperature. (c) 2014 Elsevier Inc. All rights reserved.