Tuning the NiO Thin Film Morphology on Carbon Nanotubes by Atomic Layer Deposition for Enzyme‐Free Glucose Sensing

Nanocomposites made of stacked‐cup carbon nanotubes coated with NiO (NiO/SCCNTs) via atomic layer deposition (ALD) were synthesized in order to obtain a material exhibiting enhanced and optimized electrochemical performance towards detections of glucose. The structure and morphology were characterized by transmission electron microscopy (TEM) and X‐ray diffraction (XRD). NiO deposited as nanocrystalline particles in the cubic modification, were well dispersed and directly anchored on SCCNTs forming a smooth particulate thin film, which becomes more dense with the increase of the number of ALD cycles. The NiO/SCCNTs samples with various thicknesses of the NiO coating (0.8 nm, 1.7 nm, 4.0 nm, 6.5 nm, 14.0 nm and 21.8 nm) were applied for enzyme‐free glucose sensing. Their electrochemical performance strongly depends on the thickness of the deposited NiO thin film. The best performing glucose sensors respond over a wide concentration range from 2 μM to 2.2 mM (R2=0.9979) with remarkably enhanced sensitivity (1252.3 μA cm−2 mM−1), with a limit of detection (LOD) of 0.10 μM (S/N=3) and with a fast response time (lower than 2 s). The significant performance improvement can be attributed to the conformal NiO coating, high surface to volume ratio and to the optimized thickness of the NiO thin film. The advantage of our sensors is also associated with the conductive supporting material (SCCNTs), simplicity of fabrication, high sensitivity, selectivity, stability and reproducibility for the rapid quantification of glucose. Ain't it sweet? Conductive stacked‐cup carbon nanotubes are conformally coated with NiO of variable thicknesses using atomic layer deposition (ALD). Their electrochemical performance towards glucose oxidation strongly depends on the thickness of the deposited NiO thin film. The NiO/SCCNTs electrode with 4.0 nm thickness of NiO exhibits the highest sensitivity and stability. The very thin NiO layer also protects the underneath SCCNT substrate from corrosion.