Development of bio-composite scaffolds for osteoradionecrosis treatment will be addressed here from a new concept based on bioactive glass nanoparticles and the freeze-casting process. The proposal aims to shed light on the mechanisms involved on the colloidal assembly process starting from a solid/solution interface and using time-resolved small-angle X-ray scattering experiments at ID02/ESRF over a broad q-range (USAXS, SAXS and WAXS). We will study the structure and interactions of the elementary bricks (Hybrid bioglass and in-operando material formation, reaching macroscopic scaffold via freeze-casting from the solid/solution interface using a dedicated user supplied sample environment.