AB ST R ACT : In order to improve the optical properties and enhance the stability of Zn 1Àx Cd x S nanoparticles, which are important optoelectrical materials, the ternary Zn 1Àx Cd x S nanoparticles were enclosed in a layered octosilicate by a three-step process, namely (i) protonation of Naoctosilicate, (ii) ion-exchange in order to introduce Zn and Cd ions into the interlayer space, and (iii) addition of S 2À to form Zn 1Àx Cd x S particles in the interlayer space of the octosilicate. The basal spacing (~10 Å ) of the final ZnCdS-Oct-n (n = 1, 2, 3, 4) composites noticeably increased in comparison with that of the precursor H-Oct (7.5 Å ). This may be attributed to the incorporation of larger size Zn 1Àx Cd x S particles into the interlayer space of H-Oct. The UV-visible spectra of the composites suggested that the transmission band-edges gradually shifted to low energy with increasing molar ratio of Cd/Zn. Moreover, the transmission band-edges of the composites are between those of layered Octosilicate, ZnS, and CdS. TEM observation confirmed that the size of Zn 1Àx Cd x S nanoparticles enclosed in the layered silicate was about~3À5 nm.