This thesis aims to develop a technique to characterize microelectronic interfaces based on Second Harmonic Generation (SHG) method. In the experiment part of this study, silicon wafers with thermal and native oxide, silicon-on-insulator (SOI), pure glass and glass with TiO2 thin film samples were used to observe Second Harmonic (SH) signal. The experiments have been performed in IMEP-LAHC laboratory in Grenoble, France. In addition, the measurements were carried out with “Harmonic F1X” which is a femtosecond laser developed by the company FemtoMetrix based in California/USA (FemtoMetrix). Three contributions to SHG were investigated experimentally: the electric dipole approximation due to symmetry breaking at the surface/interface, a dc electric field because of the charge separation at the interface, and lastly bulk contributions. Then, the phenomenological model of surface SHG (Mizrahi & Sipe, 1988) was simulated in MATLAB, and the ratios of the elements of second order nonlinear susceptibility (χzzz/χzii and χizi/χzii) for the silicon wafers were identified with comparing the model with the experimental results. In addition, it was shown that surface and bulk contributions can be separated by using specific polarization states and azimuthal orientations. To show this separation, Fourier coefficients, which describes the crystal facial orientations of the total SHG, were determined for the silicon wafers. Furthermore, it was observed that there are some critical parameters which have an effect to SHG: the polarization states of the incident light and second harmonic light, the angle of incidence of the incoming light and the oxidation types of silicon. Finally, SOI has been used to check whether the effecting factors are same for silicon wafers. The findings demonstrate that SHG is a powerful technique to characterize the surface/interface and the bulk of the sample in microelectronic industry.