CdS0.65Se0.35 nanoparticles are grown in a glass matrix by thermally annealing a base glass material, in which Cd, S, and Se were introduced by diffusion. The starting base material contains no crystalline structure. A comparative study of the confinement effects on the annealed samples using photoluminescence, low-frequency Raman, and optical Raman scattering experiments is presented. Growth of nanoparticles is observed with the three independent experimental techniques as the annealing temperature is varied from 550 to 800 °C. Radii of the thermally grown nanoparticles calculated from the three independent techniques are found to be in good agreement. In addition, surface phonon modes are observed in the optical spectral range, the frequencies of which agree well with those calculated theoretically. As expected from the theory, the positions of the surface phonons are found to be independent of the particle size. © 2000 American Institute of Physics.