A comprehensive analysis of composition and structure is essential for the development of new materials with tailored properties. We will demonstrate the application of SEM, XPS and XRD for the development of thin films containing nano-scaled electrical conductive particles for application in hybrid resistors.The films were prepared using the sol-gel process and precursor solutions were synthesized from an acid hydrolysis of a mixture of TEOS, water and ethanol. Alcoholic solutions of ruthenium chloride were then allocated to obtain up to 30 vol% filler in the films. The films were precipitated by dip-coating on silicon, silica or glass sheets and heat treated at up to 600• C in air or nitrogen atmospheres.A nano-structured morphology could be identified consisting of homogeneously dispersed crystalline RuO 2 particles of 10 to 180 nm in size, in an amorphous SiO 2 matrix. Film morphology can be varied using the synthesis process. The resistivity of the films was measured by an I-V measurement system. It changes drastically from 10 9 Z·cm to 10 −2 Z·cm according to the amount of dispersed conductive particles.The results show that composition-structure-property relations can be described by use of sophisticated analytical methods.