Straw-sheaf-like Co₃O₄ for preparation of an electrochemical non-enzymatic glucose sensor

3D straw-sheaf-like cobalt oxide (SS-Co₃O₄) was prepared via the hydrothermal method and inert gas calcination of precursors without the assistance of any template or surfactant. It was composed of numerous nanoneedles with a length of ~ 8 µm and a diameter of ~ 30 nm strongly tied in the center. The SS-Co₃O₄ exhibited high crystallinity, a large surface area (39.01 m².g^-1), a smaller pore size (6 nm), and lower charge transfer resistance (R_ct = 9.35 Ω) at the electrode/electrolyte interface. A non-enzymatic glucose oxidizing electrode fabricated with SS-Co₃O₄ showed a high sensitivity (669 µA.mM^-1.cm^-2), wide linear range (0.04-4.85 mM), low limit of detection (0.31 µM), good selectivity, fast response time (5 s), and high reproducibility with a relative standard deviation of 2.25%. In addition, its robust structure demonstrated excellent electrochemical stability by retaining 83.8% of the initial sensitivity when its current density vs. time response was measured for 75 min in bare electrolytes prior to the glucose-sensing test. Furthermore, it demonstrated excellent repeatability performance by retaining 87.0% of the initial sensitivity when a single electrode was tested for 4 cycles. The proposed robust structured 3D SS-Co₃O₄ electrode successfully responds to the content of glucose in human saliva, which substantially proves its suitability in practical application. The synthesis technique is advantageous to prepare other metal oxides with interesting morphology and robust structure for the development of more reliable non-enzymatic glucometers and other electrochemical devices.