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In this work, a statistical design and analysis platform was used to develop cobalt oxide based oxidation catalysts prepared via one pot metal salt reduction. An emphasis was placed upon understanding the effects of synthesis conditions, such as heating regimen and Co 2+  concentration on the metal salt reduction mechanism, the resultant nanomaterial properties (i.e., size, crystal structure, and crystal faceting), and the catalytic activity in CO oxidation. This was accomplished by carrying out XRD, TEM, and FTIR studies on synthesis intermediates and products. Additionally, high-throughput experimentation was employed to study the performance of Co 3 O 4  oxidation catalysts over a wide range of reaction conditions using a 16-channel fixed bed reactor equipped with a parallel infrared imaging system. Specifically, Co 3 O 4  nanomaterials of varying properties were evaluated for their performance as CO oxidation catalysts. Figure-of-merits including light-off temperatures and activation energies were measured and mapped back to the catalyst properties and synthesis conditions. Statistical analysis methods were used to elucidate significant property-activity relationships as well as the design rules relevant in the synthesis of active catalysts. It was found that the degree of grain boundary consolidation and anisotropic growth in fcc and hcp CoO intermediates significantly influenced the catalytic activity. By utilizing the discovered synthesis-structure-activity relationships, CO oxidation light off temperatures were decreased to <90°C.

Synthesis-Structure-Activity Relationships in Co3O4 Catalyzed CO Oxidation