Mechanical Characterization of Nanoporous Thin Films by Nanoindentation and Laser-induced Surface Acoustic Waves
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Thin films represent a critical sector of modern engineering that strives to produce functional coatings at the smallest possible length scales. They appear most commonly in semiconductors where they form the foundation of all electronic circuits, but exist in many other areas to provide mechanical, electrical, chemical, and optical properties. The mechanical characterization of thin films has been a continued challenge due foremost to the length scales involved. However, emerging thin films focusing on materials with significant porosity, complex morphologies, and nanostructured surfaces produce additional difficulties towards mechanical analysis. Nanoindentation has been the dominant thin film mechanical characterization technique for the last decade because of the quick results, wide range of sample applicability, and ease of sample preparation. However, the traditional nanoindentation technique encounters difficulties for thin porous films. For such materials, alternative means of analysis are desirable and the lesser known laser-induced surface acoustic wave technique (LiSAW) shows great potential in this area. This dissertation focuses on studying thin, porous, and nanostructured films by nanoindentation and LiSAW techniques in an effort to directly correlate the two methodologies and to test the limits and applicabilities of each technique on challenging media. The LiSAW technique is particularly useful for thin porous films because unlike indentation, the substrate is properly accounted for in the wave motion analysis and no plastic deformation is necessary. Additionally, the use of lasers for surface acoustic wave generation and detection allows the technique to be fully non-contact. This is desirable in the measurement of thin, delicate, and porous films where physical sample probing may not be feasible. The LiSAW technique is also valuable in overcoming nanoscale roughness, particularly for films that cannot be mechanically polished, since typical SAW wavelengths are micrometers in scale whereas indentation depths are usually confined to the nanometer scale. This dissertation demonstrates the effectiveness of LiSAW on both thin porous layers and rough surfaces and shows the challenges faced by nanoindentation on the same films. Zeolite thin films are studied extensively in this work as a model system because of their porous crystalline framework and enormous economic market. Many types of zeolite exist and their widely varying structures and levels of porosity present a unique opportunity for mechanical characterization. For a fully dense ZSM-5 type zeolite with wear and corrosion resistance properties, nanoindentation was used to compare its mechanical properties to industrial chromium and cadmium films. Through tribological and indentation tests, it was shown that the zeolite film possesses exceptional resilience and hardness therefore demonstrating superior wear resistance to chromium and cadmium. This also highlighted the quality of nanoindentation measurements on thick dense layers where traditional nanoindentation excels. Nanoindentation was then performed on porous and non-porous MFI zeolite films with low-k (low dielectric constant) properties. These films were softer and much thinner than the ZSM-5 coatings resulting in significant substrate effects, evidenced by inflation of the measurements from the hard silicon substrate, during indentation. Such effects were avoided with the LiSAW technique on the same films where properties were readily extracted without complications. An alternative indentation analysis method was demonstrated to produce accurate mechanical measurements in line with the LiSAW results, but the non-traditional technique requires substantial computational intensity. Thus LiSAW was proven to be an accurate and efficient means of mechanical characterization for thin porous layers. The case for LiSAW was further supported by utilizing the technique on a porous nanostructured V2O5 electrode film. The surface roughness, on the same scale as indentation depths, created difficulty in obtaining consistent nanoindentation results. Since the film was too delicate for mechanical polishing, the nanoindentation results possessed a high level of uncertainty. It was demonstrated that the LiSAW technique could extract the mechanical properties from such layers without substrate effects and with higher accuracy than nanoindentation. The research in this dissertation directly demonstrates the areas where nanoindentation excels and the areas where it encounters difficulty. It is shown how the LiSAW technique can be an efficient alternative in the challenging areas through its dependence on bulk dispersive wave motion rather than localized deformation. Thus, LiSAW opens up many avenues towards the mechanical characterization of thin, porous, soft, or rough films. Nanoindentation remains an extremely useful technique for thin film characterization, especially with the alternative analysis adaptation. However, as films continue trending towards smaller length scales, more complex porous morphologies, and engineered nanoscale surfaces, LiSAW may well become an equally valuable and indispensable technique.
- Mechanical engineering