The main focus of our research is to develop cost-effective, stable, and scalable transition metal-based electrocatalysts for the efficient conversion of CO2 to useful fuels and chemicals along with water splitting, fuel cell and selective organic oxidation studies. This strategy can be expanded in the broader field of the electrochemistry community to design sustainable catalyst materials for other electrochemical processes water splitting, fuel cell applications, and selective organic transformation as well. Designing of the plethora of catalysts by various synthesis techniques like solid-state high temperature, ball milling process, solvothermal synthesis, colloidal synthesis, multi-step chemical reduction process, etc for the electrocatalytic process. Different solid-state catalyst materials like monometallic, bimetallic, alloy, intermetallic, metal-oxide, and metal carbide have been properly synthesized. All of these materials have been well-characterized by different classical and advanced spectroscopic and microscopic techniques. The evaluation of the electrocatalytic performances has been examined by the utilization of both traditional H-type cell as well as the flow cell in the gas diffusion configuration to enhance the catalytic performance and the current density. We have also tried to unravel the reaction mechanism and to determine the active site by various advanced in situ spectroscopic techniques like ATR-FTIR, Raman, XAFS, and DEMS. With the help of all of these studies, we have not only obtained the idea about the real-time electronic and structural evolution of the catalyst, we could also be able to identify underlying structure-property relationships which can help in designing more efficient catalysts in the future.