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Laser induced breakdown spectroscopy (LIBS) provides the opportunity to analyze almost any element, from any material, in any environment. Among the many applications of LIBS is the analysis of thin films and multilayered structures. An automated system was designed and built to conduct LIBS using Nd:YAG and Ti:Sapphire lasers, broadband and high-resolution spectrometers and detectors. This system incorporates the sample manipulation as well as laser and spectrometer control and timing.

A series of experiments were conducted to analyze the ability of nanosecond and femtosecond lasers to detect Mg impurities in thin TiO₂ films using LIBS. It was determined that optimal detection occurs early in the plasma ionic/atomic emission with detection capabilities in the parts-per-million range. Another series of experiments were conducted using LIBS to analyze thin transparent organic films, with specific emphasis on the effect of film thickness and interplay between film and substrate. The challenges of ablating and measuring multiple layers have also been explored using various laser wavelengths. The effectiveness of LIBS has been demonstrated for depth profiling of CIGS solar cells. Ablation crater and ablation threshold analysis aided in understanding and overcoming some of the obstacles in depth profiling. One of the challenges with LIBS is the identification and mitigation of matrix effects. This problem was explored using a Mg tracer element and various compositions of the suspected elements Si, Ca, and Sr which can cause errors in LIBS analysis. The goal of this dissertation is to investigate the ability of LIBS to conduct detailed thin film analysis for a variety of materials and potential applications. This includes analyzing trace elements from a traditionally noisy background, measuring difficult to ablate thin films, and the unique challenges associated with multilayered structures.