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The results of a study of the microwave emission effect (power 700 W, frequency 2.45 GHz) on the structural changes in natural clay particles with effective diameters D≤630 μm are presented. The influence of the irradiation time (10 and 20 min) and the environment in the microwave chamber (atmospheric air and air saturated with water vapor) on the structural changes occurring in the particles were traced. During the first 10 min, capillary water was completely removed and agglomeration was carried out by attaching single dispersed particles (diffusion limited aggregation model). At the second stage (10-20 min), the already formed agglomerates grew (cluster-cluster aggregation model). A complex of independent optical-physical methods was used to analyze weak structural changes, including X-ray diffraction analysis, colorimetry and wavelet analysis. This approach increased the information content and reliability of measurements, quantitatively characterizing the structural responses in disperse clay systems. In the air, the removal of capillary water was accompanied by agglomerations of particles and polymorphic transformations of oxides: montmorillonite was completely decomposed and amorphous phases, in particular CaCO3, crystallized. The composition of the environment in the microwave chamber affected the type of phase transformations in iron compounds: iron-aluminum silicate (Fe2Al4Si5O18) was formed in the air; magnetite Fe.Fe2O4 (Fe3O4) appeared in the water vapor medium. The carried-out studies with the developed set of experimental methods indicated the possibility of regulating the processes of structure formation in dispersed clay systems by optimizing the regimes of exposure to microwave radiation.