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It is known that the efficiency of organic light-emitting devices (OLEDs) is strongly influenced by the ’quality′ of the thin films [1]. On the basis of this conviction, the work presented in this thesis aimed to obtain a better understanding of the structure of organic thin films of general interest in the field of organic light emitting devices by using scanning probe microscopies (SPMs). A not yet reported crystal structure of quaterthiophene film grown on potassium hydrogen (KHP) is determined by optical measurements, a simulation program, diffraction at both normal incidence and grazing angle and AFM. The crystal cell is triclinic with parameters a = 0.721 nm, b = 0.632 nm, c = 0.956 nm and a = 91°, b = 91.4°, g = 91° [2]. The morphologies of four organic thin films deposited on gold are characterized by ultra high vacuum scanning tunneling microscopy (UHV-STM). Terraces in an hexanethiol monolayer, lamellar structures in an azobenzenethiol monolayer, rods in a a poly(paraphenylenevinylene) oligomer film and a granular morphology in an oxadiazole film are shown. The topographies of a series of poly(3,4-ethylenedioxythiophene)/poly(styrenesulfonate) (PEDOT/PSS) films deposited on indium-tin oxide (ITO) and gold obtained from dispersions with PEDOT:PSS weight ratios of 1:20, 1:6 and 1:1 are investigated by AFM. It is demonstrated that the films show the same topography on gold and on ITO. It is shown that the PEDOT films eliminate the spike features of ITO. It is reported that PEDOT 1:20 and 1:6 appear indistinguishable between each other but different from PEDOT 1:1 (the most conductive). Coupling STM and I-d measurements, a not yet reported structural model of PEDOT 1:1 on gold is obtained [3]. In this model the surface presents grains and the bulk particles/domains rich in PEDOT embedded in a PEDOT-poor matrix. The equation of conductivity is derived. A STM investigation of four PEDOT films deposited on ITO obtained from dispersions with the same PEDOT:PSS weight ratio of 1:1 is carried out [4]. The films differ either for the presence of sorbitol or for a different synthetic route (and they present different conductivities). For the first time a quantitative and qualitative correlation between the nanometer-scale morphology of PEDOT films with and without sorbitol and their conductivity is established.