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The &lt;1 μm fraction of a trans-vacant 1M illite (RM30) was studied by conventional and synchrotron X-ray diffraction (XRD) techniques, combined with thermogravimetric (TG, DTG) methods to investigate the structural transformation of illite at different temperatures and degrees of dehydroxylation (D T ). The oriented specimens preheated at 300 and 680 °C correspond to the non-dehydroxylated (D T  = 0) and completely dehydroxylated (D T  = 100%) 1 M illite structures. Deviation of the basal reflection positions from rationality, expressed by the coefficient of variation of d(00l) values, progressively increase from 0.05 at D T  = 4%, to 0.14 at D T  = 51%, and then decrease to 0.06 at D T  = 95%. Similarly, for each 00l reflection the full width at half-maximum (FWHM) shows a bell-like evolution with increasing preheating temperature. Both of these features are characteristic for mixed-layered structures.

Mixed-layered structure formation during trans-vacant Al-rich illite partial dehydroxylation