Monolith Catalyst Design by Combining 3D Printing and Atomic Layer Deposition: Toward Green Palladium‐Catalyzed Cross‐Coupling Reactions

Catalysis plays a major role in various chemical processes including petroleum, pharmaceutical, fine chemistry, and energy. The development of highly functional catalysts is therefore essential. To meet the growing demand for advanced materials, we have developed ceramic catalyst supports known for their chemical inertness and thermal resistance. Using light‐assisted 3D printing, we designed complex architectures for ceramic substrates tailored to specific technical requirements. We developed ordered porous silicon oxycarbide (SiOC) ceramic monoliths with an architecture suitable for use as catalyst supports. The active sites are introduced by functionalizing the ceramic surface with palladium (Pd) nanoparticles using Atomic Layer Deposition (ALD). This technique is advantageous for achieving highly dispersed nanoparticles with uniform size distribution and minimal aggregation. We evaluated the catalytic performance by studying the effect of Pd loading on a Suzuki–Miyaura coupling reaction in water, as well as the reusability of the 3D‐printed catalytic monolith. The system demonstrates up to 82% yield and exhibits excellent stability, with no leaching of the active phase observed during the reaction cycles. These results underline the potential of 3D‐printed SiOC monoliths to create highly efficient and reusable catalytic systems, paving the way for advanced applications in a variety of industrial sectors.