Nickel nanoparticles (NPs) have garnered considerable interest due to their distinct magnetic, chemical, physical and electrochemical properties.

Nickel based nanomaterials with notable electrochemical redox activity, has gained attention as a highly promising electrode material. It offers several advantages, including its affordability, well defined electrochemical behaviour, and the potential for improved performance through various preparation techniques thereby making its application as an electrochemical sensor. The thesis focuses on synthesis of nickel-based nanomaterials and exploring their applications in electrochemical sensing. The synthesized materials include nickel hydroxide nanosheets, nickel hydroxide-molybdenum sulphide nanocomposites, nickel dodecanethiol protected clusters and nickel α-lipoic acid protected clusters. The synthesized materials show 2D and 0D structures. A thorough analysis of the morphology and electrochemical properties of these substances has been conducted, showcasing their utility as electrochemical sensors for identifying biological, environmental, and industrially significant analyte molecules. These materials can be used for real sample analysis and thereby fabricating a device can also be considered as future perspectives.