We report here, for the first time, the use of a solid state microwave source for the synthesis, calcination and functionalization of a UVM‐7 based hybrid mesoporous silica material. The synthesis of the UVM‐7 material is obtained in 2 min at low power (50 W) by the combination of a microwave irradiation and the atrane route. Moreover, it has been successfully calcined and functionalized in just 13 and 4 min respectively with microwave assisted procedures. A total synthesis comprising each individually optimized step, can be executed in only 4 h including work‐up, by contrast to a typical synthesis that comprises several days. Savings higher than one order or magnitude are obtained in time and energy. Our example is a proof of concept of the potential use of solid state microwave generators for the ultrafast on‐command preparation of hybrid nanomaterials due to their accurate control and accelerating properties.
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