This paper presented a novel method for the preparation of hybrid metallic tube arrays (MeTA) with Ag coated nickel‑iron layered double hydroxide (LDH) as highly sensitive surface-enhanced Raman scattering (SERS) substrates for the detection of toxic dyes. Nickel‑iron LDH was used as a two-dimensional material with a brucite-like structure featured a large surface area and excellent adsorption capacity. This study leveraged the sharp edges of the array structures in conjunction with the plasmonic properties of silver (a noble metal) to amplify local electromagnetic fields to create plasmonic hot spots. A hybrid heterojunction composed of Ag and LDH on MeTA enhanced the capacity of the substrate to absorb target analytes such as rhodamine 6G (R6G) and malachite green (MG). The substrate demonstrated enhanced SERS performance, as indicated by high enhancement factors in the detection of R6G (2.6 × 108) and MG (1.8 × 106). The arrays exhibited a broad linear dynamic range (R6G: 10−4 to 10−14 mol L−1; MG: 10−4 to 10−10 mol L−1), exceeded the ranges reported in previous studies. The structure of the array also revealed good reproducibility and variability. In addition, the limit of detection for R6G was determined to be 6.0 × 10−9 mol L−1 based on band height calibration and 2.57 × 10−9 mol L−1 based on band height ratio calibration, respectively. These results underscored the importance of adsorption capacity in developing advanced SERS substrates.
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