AbstractA technique is described for quantitatively examining the diffraction pattern of polydimethylsiloxane at and below room temperature with the x‐ray diffractometer. The crystalline fraction of the unstretched material is determined by the classical method developed for natural rubber. In the case of the stretched elastomer, a modified procedure is required which takes into account the extent of preferred orientation of the molecular chains. As the extension ratio is increased, the crystallization temperature rises and preferential orientation of the crystallites with respect to the extension axis increases. The crystallinity increases with decreasing temperature and appears to be independent of the extension ratio below −60°C. An over‐all crystalline fraction of 0.42 was measured for a silicone rubber specimen at −60°C. and an extension rat