CuCo
2O
4 decoration carbon nanofibers (CNFs) as an enzyme-free glucose sensor were fabricated via electrospinning technology and carbonization treatment. The CNFs with advantages of abundant nitrogen amounts, porosity, large surface area, and superior electrical conductivity were used as an ideal matrix
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CuCo
2O
4 decoration carbon nanofibers (CNFs) as an enzyme-free glucose sensor were fabricated via electrospinning technology and carbonization treatment. The CNFs with advantages of abundant nitrogen amounts, porosity, large surface area, and superior electrical conductivity were used as an ideal matrix for CuCo
2O
4 decoration. The resultant CuCo
2O
4–CNF hybrids possessed favorable properties of unique three-dimensional architecture and good crystallinity, accompanied by the CuCo
2O
4 nanoparticles uniformly growing on the CNF skeleton. To further enhance the selective molecular recognition capacity of the developed sensor, a conductive film was synthesized through the electropolymerization of thiophene and thiophene-3-boronic acid (TBA). Based on the synergistic effects of the performances of CNFs, CuCo
2O
4 nanoparticles, and boronic acid-decorated polythiophene layer, the obtained poly(thiophene-3-boronic acid) (PTBA)/CuCo
2O
4–CNF-modified electrodes (PTBA/CuCo
2O
4–CNFs/glassy carbon electrode (GCE)) displayed prominent electrocatalytic activity toward electro-oxidation of glucose. The fabricated sensor presented an outstanding performance in the two linear ranges of 0.01–0.5 mM and 0.5–1.5 mM, with high selectivity of 2932 and 708 μA·mM
−1·cm
−2, respectively. The composite nanofibers also possessed good stability, repeatability, and excellent anti-interference selectivity toward the common interferences. All these results demonstrate that the proposed composite nanofibers hold great potential in the application of constructing an enzyme-free glucose sensing platform.
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