Powdered natural Mg-vermiculite (Letovice, Czech Republic), with the formula (Mg0.35K0.02Ca0.01) (Mg2.39Fe0.51(3+)Fe0.02(2+)Al0.08) (Si2.64Al1.33Ti0.03) O10(OH)2 x 4.97H2O and particle size < 5 microm, was used for the investigation of exfoliation after hydrogen peroxide and/or microwave treatment (600 W). A sample heated in the microwave oven for 40 min exhibits a 11% mass loss and reduction of the 001 peak intensity in the X-ray diffraction pattern. The basal 001 peak intensity of untreated Mg-vermiculite sample (/001 = 100%) drops to 35% in the microwave treated sample. Only the sample treated for 5 h at 80 degrees C fully rehydrated after 120 min at room temperature. A more pronounced reduction of the 001 peak intensity (to 8%) was observed after hydrogen peroxide treatment of the sample at 25 degrees C. The combination of a five-hour hydrogen peroxide treatment at 80 degrees C and subsequent microwave heating leads to an effective extinction of the 001 diffraction in the XRD pattern. The 001 diffraction profile becomes very diffuse with peak intensity less than 1%. The degree of reduction of the 001 diffraction intensity also depends on the time and temperature of hydrogen peroxide treatment and on the peroxide concentration. An even more pronounced reduction of the peak intensity is caused by exfoliation of particles to nano-domains coupled with a randomization of the c-axes.