Fe,Al/M-MMs were prepared by swelling of layered aluminosilicate (90–95 wt.% 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.