High energy and spatial resolution XPS characterization of heterogeneous specimens

New methods must be developed for rapid and reliable characterization of heterogeneous materials by X-ray photoelectron spectroscopy (XPS). In this dissertation, a variety of XPS methods for high spatial resolution lateral and vertical analysis will be discussed.; Combining XPS imaging and spectroscopy can be critical in the analysis of heterogeneous samples. This is demonstrated in the evaluation of perfluoropolyether (PFPE) distributions in sandstone. Protecting historical buildings and monuments made of sandstone from deterioration can potentially be achieved by coating these structures with PFPEs. The PFPE coating does not form a rigid film on the surface of the sandstone but instead penetrates via capillary forces inside the pores of the stone. The successful development and application of these coatings requires insight into the polymer distribution within the sandstone. The uniformity of the coating and its impregnation into the sandstone were investigated by analysis of the surface and cross-sections of the sandstone, respectively.; Parallel photoelectron image acquisition provides new flexibility in the acquisition of image data. Acquiring a series of images as a function of binding energy allows for the development of a spectrum at every pixel. The focused ion beam (FIB) "lift-out" technique is dramatically altering preparation of samples from a variety of materials. Surface oxidation on the surface of Si (100) prepared by FIB was evaluated using the spectra-from-images approach to generate spectra from areas approximately 1 mum2. The Si (100) specimen was analyzed "as-received" and after 5 months in order to evaluate the native oxide formation on the surface as a function of age.; Rapid and reliable characterization of thin, nitrided gate oxide films remains a priority for the semiconductor industry. These films have previously been analyzed using XPS depth profiling, and vary in oxide thickness and nitrogen location. The focus of this study is the development of a rapid method for characterizing oxide thickness and nitrogen distribution. The high resolution photoelectron spectra of nitrided gate oxide films were evaluated by a variety of angle-resolved XPS (ARXPS) algorithms. Trade-offs between rapid data acquisition and high resolution nitrogen chemistry analysis were assessed with respect to ARXPS results.