The influence of the nature of the Zn, Al and Pt precursors, and of the temperature of precipitation and aging have been studied in connection with the preparation of Zn/Al and Pt/Zn/Al layered double hydroxides (LDH) by the sol-gel method. Whatever the precursors the XRD analysis shows that LDH is formed at the expense of ZnO when the precipitation and aging temperatures decrease from 353 K to 273 K. Moreover, chemical composition and TG analysis suggest the presence of weak amounts of hydrozincite, hydrozincite-like and Al(OH) 3 phases. When the precursors are Zn acetate-2-hydrate or Al acetylacetonate the amount of LDH reaches a maximum of 50 mol% at 273 K. At variance, about 90 mol% of LDH is obtained when using Zn acetylacetonate and Al isopropoxide as precursors, which are precipitated at 273 K. This proportion is slightly improved for the Pt-containing sample prepared under the same conditions. The specific surface areas of the different samples obtained after calcination at 723 K increase with their LDH content, reaching values of 110-120 m 2 g À1 . They make them particularly attractive for catalytic applications.