Na-kenyaite, a layered silicate, was synthesized via the hydrothermal method at 190 °C for 24 h using amorphous SiO 2 blocks as a starting material. Changes in the thermal structure of Na-kenyaite were investigated using the in situ high-temperature synchrotron X-ray diffraction data. Na-kenyaite was dehydrated at 200 °C, and its crystal structure was maintained from 200 to 700 °C despite its low crystallinity. It finally decomposed and crystallized to cristobalite via ¡-quartz. Na-kenyaite was ion-exchanged with Ag + and Cu 2+ ions in different ratios (Ag/Si = 0.01-0.077 and Cu/Si = 0.009-0.044), and the antibacterial properties of the ion-exchanged compounds were evaluated using gram-negative [Escherichia coli (E. coli)] and gram-positive [Staphylococcus aureus (S. aureus)] bacteria. Ion-exchanged compounds exhibited an increasing bactericidal effect when the ionexchange ratios of the compounds increased owing to the release of metal ions with antibacterial properties from the host material. The antibacterial activity of the ion-exchanged compounds was compared based on the relative antibacterial activity, calculated using the inhibition zone obtained after two days of incubation. Cukenyaite exhibited better antibacterial activity than Ag-kenyaite against E. coli and S. aureus.