(89b) Calorimetry Study of Solution Combustion Synthesis of Ni-Nano Particles in a Closed Environment

Solution combustion synthesis (SCS) is a simple, low-cost, and energy-efficient technique for the synthesis of nanomaterials with desired properties suitable for a wide range of applications. Scaling up this synthesis method to an industrial production scale is a very challenging task. The reaction is highly exothermic and releases a significant amount of gas which contains toxic gases. So far, most research works carried out on this route are carried out in an open environment. Containing this chemistry in a closed vessel can help bring it to an industrial production environment. However, it increases the associated hazard due to an accelerated pressure buildup in the closed environment. Calorimetry is a well-established laboratory tool to measure the thermal events associated with material phase change or chemical reactions occurring at different temperatures. Such properties are central to the inherently safer design of processes involving highly exothermic reactions. In this work, calorimetric analyses are carried out for SCS under adiabatic conditions using Accelerating Rate Calorimeter (Phi-TEC I) in batch conditions. Such laboratory equipment provides highly accurate data acquisition of higher resolution temperature-pressure data versus time scale for accurate characterization of the rapid exothermic reaction. The maximum heat and pressure generation can be obtained and linked to the reaction enthalpy and the stoichiometric gas production. Here we study the reaction chemistry of nickel nitrate-fuel mixture in the Phi-TEC I for the synthesis of Ni nanoparticles at different fuel types, metal precursors, solvents, and amount of initial solution in a closed calorimetry cell. This study paves the way to identify the design requirements to scale up the solution combustion synthesis technology in a closed environment, which is an important step in scaling up this technology to an industrial production scale.