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Desarrollo e implementación de la técnica de nanoindentación instrumentada por microscopía de fuerza atómica : aplicación en el estudio de las propiedades mecánicas de sistemas nanoestructurados / Development and implementation of the nanoindentation technique instrumented by atomic force microscopy: application in the study of the mechanical properties of nanostructured systems

Roa Díaz, Simón A. (2022) Desarrollo e implementación de la técnica de nanoindentación instrumentada por microscopía de fuerza atómica : aplicación en el estudio de las propiedades mecánicas de sistemas nanoestructurados / Development and implementation of the nanoindentation technique instrumented by atomic force microscopy: application in the study of the mechanical properties of nanostructured systems. Tesis Doctoral en Física, Universidad Nacional de Cuyo, Instituto Balseiro.

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Resumen en español

La industria nanotecnológica ha estado en continuo progreso debido al desarrollo acelerado de tecnologías de nano y micro fabricación, que han permitido fabricar diversos sistemas nanoestructurados para diferentes aplicaciones. El estudio de las propiedades mecánicas de estos sistemas, fundamentales para el desarrollo de nuevas tecnologías emergentes como sistemas electro-mecánicos a escala micro (MEMS) y nanométrica (NEMS), ha sido un tópico de alto impacto dentro de la física de materiales en los últimos años. Hoy en día, la técnica de nanoindentación es uno de los métodos más extendidos para la caracterización de estas propiedades en nanomateriales. El reciente interés por esta técnica se ha debido al desarrollo de equipos especializados en su implementación, siendo principalmente impulsado por la creciente demanda multidisciplinaria de este tipo de caracterización a escala nanométrica en diversas áreas de la nanotecnología. En virtud de la relevancia actual de la técnica de nanoindentación, los objetivos fundamentales de la tesis propuesta son el desarrollo e implementación de esta técnica utilizando el Microscopio de Fuerza Atómica (AFM) ubicado en las dependencias del Instituto de Nanociencia y Nanotecnología (INN – Nodo Bariloche). Más allá de ésto, el objetivo principal y el fin de esta tesis es proveer de nuevas e importantes perspectivas con respecto al rol que juegan distintos tipos de confinamiento u otros fenómenos no triviales en el comportamiento mecánico de diversos tipos de nanoestructuras. La fundamental y primera parte de esta tesis abarca un estudio sobre la instrumentación de la nanoindentación por AFM. El objetivo principal es la sistematización de distintos protocolos de calibración para la obtención de curvas de fuerza (𝑃)-desplazamiento (ℎ) (o curvas 𝑃(ℎ) por simplicidad) por AFM, las cuales son cruciales para el análisis cuantitativo de las propiedades mecánicas mediante modelos estándar de indentación. Además, con el objetivo de proveer una estimación cuantitativa de las tales propiedades, se presenta una nueva metodología indirecta para la calibración del perfil geométrico del nanoindentador basado en el estudio de deformación plástica. Los resultados derivados de esta primera fase de desarrollo han permitido dilucidar de forma exacta las limitaciones físicas asociadas a la implementación de esta técnica, y validarla para el futuro estudio de la mecánica de distintos tipos de nanomateriales. La segunda parte de esta tesis muestra los primeros estudios de factibilidad y validación de esta técnica para la caracterización mecánica. En este contexto, el objetivo es validar la técnica, a primer orden, mediante el estudio de las propiedades mecánicas de distintos materiales tipo bulk (Si, SiO2 e In), enfocándose en la estimación cuantitativa de propiedades tales como dureza y módulo de Young. Este estudio nos ha mostrado el buen acuerdo que existe entre los valores determinados para estas propiedades usando el AFM y los rangos típicos esperados, lo que nos ha permitido verificar la validez de esta técnica para la cuantificación precisa y exacta de las propiedades mecánicas. La parte principal y final de esta tesis tiene como objetivo la implementación de la técnica de nanoindentación por AFM para el estudio de fenómenos físicos interesantes en distintos sistemas nanoestructurados. Como objetivo específico se ha planteado el estudio de sistemas tales como películas delgadas de Cu y Ag y nanodiscos de Ag, los cuales fueron analizados con el fin de entender y cuantificar el efecto de distintos tipos de confinamiento en el comportamiento mecánico efectivo de los mismos. Para el caso de películas delgadas de Cu se ha estudiado particularmente la competencia entre efectos microestructurales y efectos de tamaño (inducidos por espesor) en las propiedades mecánicas de éstas, dándose nuevas perspectivas con respecto del rol de ambos factores en el comportamiento mecánico efectivo. En este caso, los resultados nos han mostrado que la sensibilidad instrumental es adecuada para estudiar y discriminar la influencia de efectos de tamaño y microestructurales en las propiedades mecánicas. Además, nos han nos han permitido plantear que tanto el espesor de la película como los efectos microestructurales son importantes a la hora de describir las propiedades mecánicas efectivas de películas delgadas policristalinas. Por otro lado, los estudios en películas delgadas y nanodiscos de Ag nos han demostrado que esta técnica es una herramienta eficiente para la caracterización del comportamiento nanomecánico tanto de películas delgadas como nanodiscos, evidenciando su potencial para la detección de efectos de substrato y confinamiento lateral. Los resultados han demostrado que en ciertos regímenes ambos efectos compiten, siendo el confinamiento lateral una contribución de segundo orden cuya magnitud parece no estar asociada a escalas de longitud absoluta, sino más bien con escalas de longitud relativa. Nuestros estudios han demostrado que los efectos de espesor y confinamiento lateral deberían tenerse en cuenta en el desarrollo de componentes metálicos a nanoescala para su uso en tecnologías emergentes como MEMS/NEMS, ya que su vida útil podría verse negativamente afectada en determinadas condiciones de tamaño. Los resultados provistos a lo largo de esta tesis proveen sólidos cimientos para la futura implementación de esta facilidad por parte de investigadores que requieran estudios complementarios de este tipo, tanto para investigación básica como aplicada. Se ha validado la factibilidad y utilidad de esta técnica para el estudio del comportamiento mecánico de sistemas tanto bulk como nanoestructurados, abriendo futuras perspectivas para el estudio de diversos materiales con alto impacto en la industria nanotecnológica.

Resumen en inglés

The nanotechnology industry has been in continuous progress due to the accelerated development of nano and micro fabrication technologies, which have allowed the fabrication of various nanostructured systems for different applications. The study of the mechanical properties of these systems, which are fundamental for the development of new emerging technologies such as electro-mechanical systems at micro (MEMS) and nano (NEMS) scales, has been a high-impact topic in materials physics in recent years. Nowadays, nanoindentation technique is one of the most extended methods for characterizing these properties in nanomaterials. The recent interest in this technique is due to the development of instruments specialized for its implementation, being mainly boosted by the increasing multidisciplinary demand for this type of characterization at the nanometric scale in various areas of nanotechnology. Due to the current relevance of the nanoindentation technique, the fundamental objectives of the proposed thesis are the development and implementation of this technique by using the Atomic Force Microscope (AFM) located in the Institute of Nanoscience y Nanotechnology (INN – Nodo Bariloche) facilities. Beyond these objectives, the main objective and purpose of this thesis is to provide new and relevant perspectives regarding the role of different types of confinement or other non-trivial phenomena on the mechanical behavior of various types of nanostructures. The fundamental and first part of this thesis encompasses a study on the instrumentation of nanoindentation by AFM. The main objective is the systematization of different calibration protocols for obtaining force (𝑃)-displacement (ℎ) curves (or 𝑃(ℎ) curves for simplicity) by AFM, which are crucial for the quantitative analysis of the mechanical properties by standard indentation models. In addition, to provide a quantitative estimation of such properties, a new indirect methodology is presented for the calibration of the nanoindenter geometric profile based on the study of plastic strain. The results obtained from this first development phase have enabled to elucidate the exact physical limitations associated with the implementation of this technique, and to validate it for the future study of the mechanics of different types of nanomaterials. The second part of this thesis shows the first feasibility and validation studies of this technique for mechanical characterization. In this context, the objective is to validate this technique, firstly, by studying the mechanical properties of different bulk materials (Si, SiO2 and In), focusing on the quantitative estimation of mechanical properties such as hardness and Young's modulus. This study has shown us the good agreement that exists between the values determined for these properties by using the AFM and the expected typical ranges, which has enabled us to verify the validity of this technique for a precise and accurate quantification of the mechanical properties. The main and final part of this thesis has the objective of implementing the AFM-assisted nanoindentation technique for the study of interesting physical phenomena in different nanostructured systems. As a specific objective, we have proposed the study of different systems such as Cu and Ag thin films and Ag nanodisks, which were analyzed to understand and quantify the effect of different types of confinement on their effective mechanical behavior. For the case of Cu thin films, the competition between microstructural effects and size effects (induced by thickness changes) on their mechanical properties has been particularly studied, giving new insights regarding the role of both factors on the effective mechanical behavior. In this case, the results have shown us that the instrumental sensitivity is adequate to study and discriminate the influence of size and microstructural effects on the films mechanical properties. Also, these have enabled us to state that both film thickness and microstructural effects are important to describe the effective mechanical properties of polycrystalline thin films. On the other hand, the studies on Ag thin films and nanodisks have shown us that this technique is an efficient tool for characterizing the nanomechanical behavior of both kinds of systems, evidencing its potential for the detection of substrate and lateral confinement effects. The results have shown that in certain regimes both effects compete, being lateral confinement a second-order contribution whose magnitude does not seem to be associated with absolute length scales, but rather with relative length scales. Our studies have shown that the effects of thickness and lateral confinement should be considered in the development of metallic components at nanoscale for their use in emerging technologies such as MEMS/NEMS, since their lifetime could be negatively affected under certain size conditions.

Tipo de objeto:	Tesis (Tesis Doctoral en Física)
Palabras Clave:	Mechanical properties; Propiedades mecánicas; Thin films; Capas finas; Atomic force microscopy; Microscopia de fuerza atómica [Nanoindentation; Nanoindentación; Confinement effect; Efectos de confinamiento; Microstucture effects; Efectos Microestructurales]
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Materias:	Física > Materia condensada
Divisiones:	Investigación y aplicaciones no nucleares > Física > Resonancias magnéticas
Código ID:	1092
Depositado Por:	Tamara Cárcamo
Depositado En:	25 Jul 2022 11:43
Última Modificación:	28 Jul 2022 14:38

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