Fe,Al/M-MMs were prepared by swelling of layered alumino silicate (90–95wt.% montmorillonite) from a bed located in Mukhortala (Buryatia, Russia) in Na+, Ca2+ and Ba2+ forms by means of the exchange of these cations with bulky Fe,Al-polyoxocations prepared at Al/Fe=10/1 and OH/(Al+Fe)=2.0, and then calcinated at 500◦C