The chemical coupling of NiO nanostructures with thermally treated multiwall carbon nanotubes (MWCNTs) is not reported as it provides an enhanced dispersion of composite material in water. The dispersion of MWCNTs has been considered a big challenge. For this purpose, we first thermally treated MWCNTs at 1000°C in air for 30 min. Then, thermally treated MWCNTs were chemically coupled with NiO nanostructures by a hydrothermal method. The material characterization in terms of structure, morphology, and composition is well studied by different analytical techniques. The NiO composite (sample 2) with highest weight of MWCNTs had a leaf-like morphology and it exhibits a cubic phase of NiO. Cyclic voltammetry (CV) was used to study the electrochemical activity of prepared composite material towards the oxidation of uric acid in the phosphate buffer solution of pH 7.0. Sample 2 showed a well-behaved anodic peak with enhanced peak current and exhibited a linear range from 0.01 mM to 2.5 mM for uric acid with a low limit of detection 0.001mM. Sample 2 was found to be very selective under the environment of competing interferents such as urea, glucose, lactic acid and ethanol. This sample exhibits significant stability, thus it is a potential protocol for the monitoring of uric acid from real samples. This study provides a low-cost platform for the fabrication of efficient materials for various applications such as batteries, fuel cells and water splitting.