Catalysts are materials widely used in chemistry and particularly in the field of refining to convert heavy oil products in light products present in gasoline pool. The improvement of new supports can be driven by the synthesis of controlled morphology materials, the increase of the exchange surface between the catalyst and the reagent or the increase of the contact area of the metallic particles with the reagent. The improvement and the development of new materials require the implementation of successful analytical tools which can follow their genesis. In this work, we developed a new NMR methodology based on the measurement of the transverse relaxation time (lasted the disappearance of the transverse magnetization) and the longitudinal relaxation time (lasted the return of the longitudinal magnetization). We were able to show that this technique allows to finely describe, during the synthesis, the characteristic parameters of formed particles. It is applicable to amorphous inorganic supports, hierarchically organized materials or crystallized materials, on a wide range of porosity from 4,5 Å to 240nm. It allows to reach in: The texture of particle: roughness (outer surface) and developed internal surface (micro, meso and macroporosity) the size and proportion of formed particles. For a given family of materials, this technique is particularly sensitive to surface composition: aluminum and hydroxyl proportion
