Rada Vilela , Evilus (2022) Desarrollo de materiales avanzados con morfología controlada para electrodos de baterías de ion de litio / Development of advanced materials with controlled morphology for Li-ion battery electrodes. Tesis Doctoral en Ciencias de la Ingeniería, Universidad Nacional de Cuyo, Instituto Balseiro.
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Resumen en español
Las baterías de ion de litio dominan el mercado de almacenamiento energético tanto en dispositivos portátiles como en vehículos eléctricos, y su uso en aplicaciones estacionarias es cada vez más amplio. Además, se prevé un incremento acelerado en la demanda de almacenamiento durante las próximas décadas, debido principalmente a la electrificación total del transporte. Este escenario plantea la necesidad de desarrollar baterías que ofrezcan mayor rango de autonomía, mayor tiempo de vida útil y altas velocidades de carga, buscando reducir el impacto ambiental desde su fabricación hasta su disposición final, y precios competitivos frente a los vehículos de motor de combustión interna. Estos factores dependen sustancialmente de las propiedades de los materiales activos de los electrodos. El óxido de litio manganeso (LiMn_2O_4) es un material activo catódico que presenta buenas propiedades electroquímicas, toxicidad reducida y costos moderados de obtención. Sin embargo, el material en volumen sufre un acelerado decaimiento de la capacidad de carga debido a la degradación de su superficie por contacto con el electrolito, y un bajo coeficiente de difusión del Li+, lo cual limita la velocidad de carga. Una de las estrategias utilizadas para mejorar el desempeño electroquímico es el uso de materiales activos nanoestructurados, ya que estos presentan propiedades distintas en comparación con su contraparte en volumen (bulk). Debido a que estas propiedades están íntimamente relacionadas con las características morfológicas de las nanopartículas, la posibilidad de controlar la morfología permite ajustar las propiedades del material optimizando el funcionamiento del mismo. Esta tesis se enfocó en la síntesis con morfología controlada de nanopartículas de LiMn_2O_4 como estrategia para abordar los problemas que presenta el material en volumen. La síntesis se basó en el método de descomposición térmica de precursores organometálicos asistida por surfactantes, seguido de un tratamiento térmico en aire. El control de la morfología se realizó mediante el ajuste de parámetros de la síntesis. Las muestras se caracterizaron química, estructural y microestructuralmente mediante difracción de rayos X, difracción de electrones, espectroscopía de pérdida de energía de electrones y microscopía electrónica de transmisión. Las propiedades electroquímicas se evaluaron mediante técnicas de ciclado galvanostático, voltamperometría cíclica y espectroscopía de impedancia electroquímica. En primer lugar, se sintetizaron nanopartículas de LiMn_2O_4, cuya capacidad de carga y descarga inicial resultó comparable con los valores reportados en la bibliografía para este material. Sin embargo, esta capacidad decae rápidamente durante el ciclado, posiblemente debido a la degradación de la superficie por contacto con el electrolito. Para evaluar la capacidad de controlar la morfología, se sintetizaron nanopartículas core/shell de composición LiMn_2O_4/Li_2O, cuya cáscara podría proteger la superficie del material, además de proveer litio adicional para compensar posibles pérdidas. Esta muestra presentó mayor capacidad de carga inicial, sin embargo, se obtuvieron valores casi nulos en los ciclos siguientes. Esto puede atribuirse a la descomposición del electrolito por reacciones secundarias del material agregado como cáscara. Finalmente, se generaron nanoestructuras huecas de LiMn_2O_4. Si bien la capacidad de carga y descarga inicial fue ligeramente inferior en comparación con las muestras anteriores, esta muestra presentó una mejor estabilidad en condiciones de ciclado, lo cual está relacionado con las características morfológicas de las nanoestructuras. Se determinó además que, tanto las nanopartículas como las nanoestructuras huecas, presentan coeficientes de difusión de Li+ elevados en comparación con los valores reportados para el material en volumen, indicando que la cinética resultó favorecida debido a las dimensiones nanométricas del material.
Resumen en inglés
Lithium-ion batteries dominate the energy storage market in both portable devices and electric cars, and their use in stationary applications is growing fast. In addition, a rapid increase in storage demand is expected in the coming decades, mainly due to the total electrification of the transport sector. This scenario raises the need to develop batteries that offer a greater drive range, longer cycle life, and faster charge rates, also ensuring a low environmental impact from its manufacture to its final disposal, and competitive prices compared to combustion engine vehicles. These factors depend substantially on the properties of the active materials of the electrodes. Lithium manganese oxide (LiMn_2O_4) is a cathodic active material that exhibits good electrochemical properties, low toxicity, and moderate manufacturing costs. However, the bulk material suffers from fast capacity fading as a result of surface degradation due to contact with the electrolyte, and low Li+ diffusion coefficient which results in slow charge/discharge rates. One of the strategies used to improve electrochemical performance is using nanostructured active materials, due to their different properties compared to their bulk counterpart. Since these properties are closely related to the morphological characteristics of the nanoparticles, the possibility of controlling the morphology allows the properties of the material to be adjusted, optimizing its performance. This thesis is focused on the synthesis with controlled morphology of LiMn_2O_4 nanoparticles as a strategy to overcome the issues of the bulk material. The synthesis was based on the method of thermal decomposition of organometallic precursors assisted by surfactants, followed by a thermal treatment in air. The morphology was controlled by adjusting certain parameters of the synthesis. Chemical, structural, and microstructructural characterization of the samples were made by X-ray diffraction, electron diffraction, electron energy loss spectroscopy, and transmission electron microscopy. The electrochemical properties were analyzed by galvanostatic charge/discharge cycling, cyclic voltammetry, and electrochemical impedance spectroscopy. Initially, LiMn_2O_4 nanoparticles were obtained, whose initial charge and discharge capacity was favorable, however, this capacity rapidly decays during cycling, possibly due to surface degradation. In order to protect the surface of the material, we synthesized core/shell nanoparticles with LiMn_2O_4/Li_2O composition. The electrochemical evaluation revealed a higher initial charge capacity for this sample; however, the charging process was highly irreversible, obtaining almost null capacities in the following cycles, which was attributed to the accelerated decomposition of the electrolyte due Li_2O side reactions. Finally, hollow LiMn_2O_4 nanostructures were obtained. Although the initial charge and discharge capacity was slightly lower compared to previous samples, these nanostructures showed improved stability during cycling, which is related to the morphological characteristics of the nanostructures. It was also determined that both the nanoparticles and the hollow nanostructures exhibit high Li+ diffusion coefficients compared to the values reported for the bulk material, indicating that the kinetics were favored due to the nanoscale dimensions of the material.
| Tipo de objeto: | Tesis (Tesis Doctoral en Ciencias de la Ingeniería) |
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| Palabras Clave: | Nanoparticles; Nanopartículas; [Li ion batteries; Baterías de ion de litio; Controlled morphology; Morfología controlada; Hollow nanostructures; Nanoestructuras huecas; Core shell nanoparticles; Nanopartículas core shell] |
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| Materias: | Ingeniería mecánica > Ciencia de materiales |
| Divisiones: | Gcia. de área de Aplicaciones de la tecnología nuclear > Gcia. de Investigación aplicada > Materiales metálicos y nanoestructurados |
| Código ID: | 1167 |
| Depositado Por: | Tamara Cárcamo |
| Depositado En: | 13 Mar 2023 16:19 |
| Última Modificación: | 13 Mar 2023 16:19 |
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