This paper illustrates the implementation of various X-ray techniques for the characterization of SiGe and high K metal gate films, including HRXRD, XRR, XPS. Parameters of interest such as strain, thickness, composition could be determined by corresponding technique. The strength and drawback of each technique are presented. Repeatability tests were performed in order to check the measurement tool capability. An innovative approach of hybrid techniques for such applications is also explored and suggested.