Fe3+‐montmorillonite clay catalyst was used for the first time for pyrroles preparation by Paal–Knorr condensation. The features of this catalytic system are improved yields, mild conditions, a simple procedure, and high catalytic efficiency. The catalyst could be easily recycled and reused for three times without visible losing of activity.

Three-dimensional (3D) plasmonic metamaterials have become a trend in the application of nanophotonic devices. In this paper, a convenient and inexpensive method for the design of 3D multilayer plasmonic metamaterials is constructed using a one-step self-shielded reactive-ion-etching process (OSRP) and a thermal evaporation system, which provides an efficient and low-cost method for the preparation of surface-enhanced Raman spectroscopy (SERS) substrates. The near-field enhancement of the 3D plasmonic metamaterials provides highly efficient electromagnetic resonance, and highly sensitive and uniform SERS sensing capabilities. The SERS detection results of rhodamine B (Rh. B) and rhodamine 6G (R6G) on this substrate show that the detection limit could reach 10^–13 mol/L, and the signal could give expression to excellent uniform stability. The results show that high sensitivity and high robustness SERS substrates can be prepared with high efficiency and low cost.