How
to construct highly sensitive electrochemical sensors based
on single atoms is one of the hotspots. In this study, we reported
a strategy for regulating the electrocatalytic activity of nickel
single atoms (Ni SAs) based on directional assembly, which could be
used to construct a glucose electrochemical sensor. Nitrogen-doped
two-dimensionally ordered array carbon nanostructures with atomically
dispersed nickel (D-Ni SAs/CN) were synthesized by directional assembly
of interconnected carbon polyhedrons via ionic exchange, ice templating,
and high-temperature pyrolysis. The materials were characterized by
transmission electron microscopy (TEM), field emission scanning electron
microscopy (FESEM), high-angle annular dark-field scanning transmission
electron microscopy (HAADF-STEM), X-ray diffraction (XRD), X-ray photoelectron
spectroscopy (XPS), and Fourier transform infrared (FTIR) spectroscopy.
Electrochemical results revealed that the ordered arrangement of carbon
polyhedrons endowed the D-Ni SAs/CN with a stronger electrocatalytic
effect on glucose oxidation than that of isolated nitrogen-doped carbon
polyhedrons containing atomically dispersed nickel (Ni SAs/CN). The
linear range for detecting glucose was 0.002–1.1 mM with a
high sensitivity of 1418.7 μA·mM–1·cm–2 and a detection limit of 1.2 μM. Moreover,
the sensor could be used to accurately measure glucose levels in real
samples. This study not only demonstrated the feasibility of Ni SAs
as an excellent sensing material but also highlighted the importance
of two-dimensionally ordered carbon array nanostructures in enhancing
the electrochemical sensing performance.