Herein,
we report the preparation of novel spinel-type CuCo2O4 nanoplates (CCO NPs) through a cost-effective,
soft-template (citrate)-assisted method, followed by low-temperature
calcination. In the synthesis process, the metal cations such as Cu2+ and Co2+ can react with citrate molecules via
coordination interaction to form the CuCo-citrate at elevated temperature.
During the calcination process at 500 °C, the citrate molecules
were eliminated from the CuCo-citrate precursor via simple organic
species, and thus, spinel-type CuCo2O4 nanoplates
were formed successfully. Surface morphology, crystalline nature,
and phase purity of as-synthesized CCO NPs were assessed by transmission
electron microscopy (TEM), X-ray diffraction (XRD), and X-ray photoelectron
microscopy (XPS). As-synthesized CuCo2O4 nanoplates
were used to construct a sensitive and reliable enzyme-free electrochemical
sensor of acetylcholine (ACh) that shows a meaningful limit of detection
(30 nM) with broad dynamic range (0.2–3500 μM) covering
the clinical range of ACh. Furthermore, the developed ACh sensor delivered
long-term durability and good reproducibility. The point-of-care utility
of the ACh sensor was demonstrated in spiked blood serum samples with
acceptable recovery rates. The present work demonstrates a facile
synthesis method with an extensive potential toward the preparation
of binary transition metal oxides (BTMOs) for divergent electrocatalytic
applications.