This study presents the post-synthetic functionalization of Ni-Co bimetallic nanoparticles (NPs) with a β-cyclodextrin (β-CD) framework using a green synthesis approach with Illicium verum (Star anise) extract. The synthesized nanocomposite was verified using physicochemical characterization techniques such as FTIR, XRD, Zeta potential, DLS, SEM, and TEM. This surface modification successfully yielded a stable core–shell architecture with a reduced crystallite size of 29.5 nm, compared to 41.2 nm for bare Ni-Co NPs. The β-CD coating shifted the Zeta potential from −33.07 mV to −27.65 mV, establishing an electro-steric stabilization mechanism. Sensing performance toward Cd2+ ions was evaluated via the QCM-D technique. The Ni-Co/β-CD nanocomposite demonstrated a superior sensitivity of 34.72 Hz/mM and a remarkably low limit of detection (LOD) of 17.3 µM, representing a 27-fold enhancement over the bare Ni-Co NPs (LOD: 472.2 µM). The mechanical signature, characterized by negative dissipation shifts and a high acoustic ratio (ΔD/Δf = 79.410 × 10−6), confirms an analyte-induced conformational rigidification driven by a host–guest interaction mechanism. These findings establish a robust method of producing bio-based, “smart” nanocomposites for high-precision environmental sensing.
Wafa Al-Gethami (Thu,) studied this question.