The nanocrystals of PbTe and related compounds (Pb1−xSnxTe, PbTe1−xSex), differing by size and composition, have been synthesized using a chemical vapor transport (CVD) technique. The size–selective precipitation mechanism relying on the variation of heating temperatures, Ar flow rates and admixture with Au particles, enables a relatively good control of particle size distribution. In addition, the doping ratios of those nanocrystals are readily modified by changing the atomic ratio in the raw starting materials. Subsequently, a yield of hundreds of milligrams of nanocrystals which exhibit narrow size distributions at 100 nm, 300 nm and 600 nm and controllable composition have been obtained. XRD patterns taken on the PbTe samples show sharp, which indicate good crystallinity of samples. According to the shift of the Bragg reflections, the lattice constants of (Sn / Se) doped PbTe change with the variation of the doping ratios.