Fluidized beds are increasingly used in renewable energy and chemical production due to their versatility in handling different solids for multi-functional industrial applications. The diversity in size and density of solid particles impacts fluidization, influencing mixing and segregation behaviours critical for optimizing chemical processes and reactor design. This study investigates the expansion and segregation behaviours of mixed Geldart group powders in binary systems, simulating polydispersed beds with different materials and catalysts. By applying a modified Cheung equation and an adapted Gibilaro-Rowe model, the study analyzes segregation behaviours of Geldart Group A and B materials at varying mixing rates and gas flow velocities. Results show a good match between experimental data and model predictions. Using novel non-invasive X-ray imaging, the study provides real-time analysis of mixing and segregation at different fluidization regimes and temperatures. These findings aid in designing and optimizing advanced thermochemical conversion technologies, enhancing process efficiency and resilience.