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Multicomponent oxide microspheres with interconnected macroporosity (MICROSCAFS^®) are new materials with great potential as support materials for photocatalysis, optimized for real life applications and for other uses that are still being explored. They are obtained from an adapted sol–gel process combined with phase separation phenomena that occur within the water droplets of an emulsion. We present here a methodology based on cryogenic scanning electron microscopy (cryo-SEM) that allows, with minimal specimen preparation, the direct and in situ visualization of ‘wet’ alkoxide-derived microstructures, for the mechanistic study of the complex process of MICROSCAFS^® generation. It is simultaneously combined with energy dispersive X-ray spectroscopy (EDS) to visualize phase separation phenomena and study the chemical elemental composition at specific regions of the sample and reaction times.