This study assesses the physical and electrochemical changes of bimetallic Ag-Au nanoparticle-functionalized bentonite nanoclay. Nanoclay was studied to deduce a better sensing material/film. A chemical co-reduction method was used to synthesize bimetallic Ag-Au c nanoparticles, which were used to prepare a Ag-Au/PGV bentonite composite. Bimetallic Ag-AuNPs and their nanoclay composite were optically characterized using the scanning electron microscope, ultraviolet visible spectroscopy, X-ray diffraction, and Fourier transform infrared, whilst cyclic voltammetry (CV) and differential pulse voltammetry (DPV) were used to ascertain their electrochemical activity and properties. The results of surface morphological inspection showed an average size of 10 nm, in agreement with XRD. The bimetallic Ag-AuNPs UV/Vis characteristic wavelengths of 414 nm and 516 nm confirmed the presence of Ag and Au metals, respectively. XRD exhibited diffraction planes related to 2θ values of Ag and Au metals, whilst FTIR indicated mainly COO- functional groups from the citrate capping of bimetallic Ag-Au NPs. CV and DPV showed that bentonite nanoclay is largely insulated by silicates but exhibited a small electroactivity of Fe. The electroactivity of Ag-Au/PGV bentonite exhibited peak potentials due to Ag/Ag+ and Au/Au3+ redox couples at 0.19 V/−0.20 V and 1.37 V/0.42, respectively. The Ag-Au/PGV bentonite nanocomposite exhibited the highest surface concentration of 3.25 × 10−2 cm2, a diffusion coefficient of 2.36 × −11 cm2/s, and an electron transfer rate constant (Ks) of 1.99 × 10−4 cm2. The outcome of these results indicated that the Ag-Au/PGV bentonite nanocomposite was more electroactive than PGV. Therefore, this study accentuates Ag-Au/PGV bentonite nanocomposite as a novel and promising platform for electrochemical sensing with higher sensitivity and efficiency than other sensing materials.