Lavorato, Gabriel C. (2016) Nanopartículas magnéticas multicomponentes : diseño, fabricación y propiedades. / Multicomponent magnetic nanoparticles : desing, fabrication an properties. Tesis Doctoral en Ciencias de la Ingeniería, Universidad Nacional de Cuyo, Instituto Balseiro.
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Resumen en español
Las propiedades de las nanopartículas magnéticas están definidas por la elevada relación superficie/volumen y se manifiestan en fenómenos como superparamagnetismo, anisotropía de superficie, desorden magnético superficial y exchange-bias. La síntesis de nanoestructuras multicomponentes con un grado creciente de complejidad permite un mayor control sobre sus propiedades que, guiadas por el impulso de la miniaturización de dispositivos electrónicos y el avance de las energías limpias y la nanomedicina, pueden optimizar el rendimiento de materiales para almacenamiento magnético de datos, imanes permanentes, aplicaciones biomédicas o catálisis. El superparamagnetismo impone un límite a la reducción del tamaño debido a la uctuación térmica del momento magnético cuando su energía de anisotropía resulta comparable a la energía térmica. Frente a ello, estudios previos demostraron que el acoplamiento en la interfaz de nanopartículas bimagnéticas antiferromagneto/ferrimagneto de estructura core/shell permite incrementar la anisotropía efectiva y manipular el exchange-bias, de acuerdo a la relación entre la energía de anisotropía del antiferromagneto y la intensidad de la interacción de intercambio en la interfaz. Esta tesis se enfoca en el diseño, la fabricación y el estudio de nuevos materiales nanoestructurados basados en nanopartículas core/shell, orientados a sintonizar las propiedades físicas gracias a la comprensión de los mecanismos microscópicos que los gobiernan. Se emplearon óxidos de metales de transición, materiales abundantes y relativamente económicos que ofrecen una variedad de propiedades, incluyendo ferrimagnetos como ferritas de elevada anisotropía magnetocristalina (CoFe_2O_4), ferritas de anisotropía ajustable según su composición (ferritas mixtas de Zn-Co o Ni-Co) o biocompatibles (Fe_3O_4), monóxidos antiferromagnéticos de elevada anisotropía (CoO) y semiconductores diamagnéticos fotoluminiscentes (ZnO). Distintas familias de nanopartículas multicomponentes se sintentizaron mediante métodos químicos basados en la descomposición de organometálicos en solventes orgánicos, asistida por surfactantes. Los materiales desarrollados se estudiaron mediante técnicas de caracterización estructural (microscopía electrónica de transmisión, difracción y reectometría de rayos X, termogravimetría), magnética (distintos magnetómetros DC y AC) y óptica (espectrometría UV-visible y de fotoluminiscencia). En primer lugar se diseñaron distintos sistemas de nanopartículas core/shell de composición CoO/CoFe_2O_4 y se estudiaron los efectos de tamaño con el objetivo de controlar la anisotropía efectiva. A diferencia de lo que se observa en nanopartículas monofásicas, al reducir el tamaño se registró un notable incremento de la anisotropía, a expensas de una menor estabilidad térmica por el menor volumen total. En nanopartículas de 5 nm de diámetro, se demostró que el campo coercitivo medido a 5 K puede incrementarse hasta 30.8 kOe, valor un 50% mayor que el máximo reportado para nanopartículas monofásicas de CoFe_2O_4. A su vez, la estabilidad del momento magnético puede aumentarse hasta la temperatura de Néel del CoO, cerca de temperatura ambiente. Se encontró que la cristalinidad del núcleo de CoO y la eficacia de la interacción de intercambio en la interfaz se pueden controlar mediante un tratamiento térmico gracias al recubrimiento que protege al núcleo. Además, la comparación con un sistema de tamaño y morfología análogos pero formado por un núcleo diamagnético (ZnO/CoFe_2O_4) permitió identificar los diferentes roles de los efectos de superficie, de interacciones y de interfaz, los últimos responsables de un mayor campo coercitivo, mayor temperatura de bloqueo y menor volumen de activación en nanopartículas bimagnéticas. Luego, se propuso manipular el campo de exchange-bias y la anisotropía efectiva introduciendo Zn"2+ y Ni"2+ en la ferrita de Co, para lo que se diseñaron nuevos sistemas de nanopartículas core/shell CoO/ferrita. Se encontró que al incorporar Zn"2+, un ión 3d10 no magnético, se debilita el acoplamiento en la interfaz lo que lleva a maximizar el exchange-bias para concentraciones intermedias de Zn en la ferrita mixta. Los resultados se interpretaron de acuerdo a la competencia entre la energía de anisotropía del CoO y la energía de acoplamiento en la interfaz, considerando la densidad de espines magnéticos acoplados en la interfaz. En cambio, la introducción de Ni"2+ en la ferrita de Co demostró, además de la presencia de exchange-bias, importantes efectos de superficie y desorden magnético. Las dificultades para controlar con precisión los tamaños de las fases en las estructuras core/shell y la necesidad de un estudio sistemático de los efectos de los tamaños relativos sobre el acoplamiento en la interfaz motivó la fabricación y estudio de películas delgadas ferrita/ferrita. En bicapas de Fe_3O_4/CoFe_2O_4 fabricadas mediante depósito por láser pulsado donde el espesor de Fe_3O_4 se varío entre 0 y 25 nm, se identificó un espesor crítico de ~ 8 nm para la magnetita, por debajo del cual se observa un acople rígido entre ambas fases, mientras que mayores espesores promueven un comportamiento de tipo exchange-spring. Tales estudios pueden servir como sistema modelo para el diseño de nanopartículas bimagnéticas con propiedades óptimas. Por último, se diseñó y fabricó un sistema de nanopartículas core/shell bifuncionales de composición CoFe_2O_4/ZnO. La caracterización preliminar reveló que el material es capaz de generar calor frente a la aplicación de un campo magnético de radiofrecuencia y, al mismo tiempo, presenta una respuesta óptica fotoluminiscente. Los progresos registrados en los últimos años en el campo de la nanomedicina sugieren que las nanopartículas magnéticas pueden aportar soluciones a problemas biomédicos específicos. La combinación de ambas funcionalidades en un mismo material permitiría abordar nuevos estudios en el campo de la hipertermia de uido magnético donde la marcación óptica es fundamental, por ejemplo, para la evaluación de una aplicación sistémica de las nanopartículas en el organismo. La nanotecnología ofrece actualmente poderosas herramientas para el desarrollo de materiales magneticos avanzados, incluyendo nuevos metodos químicos de fabricación y la consolidación de técnicas de caracterización sensibles a la interfaz. El principal aporte de este trabajo es el diseño de nanoestructuras multicomponentes y el estudio de la compleja relación entre su estructura y propiedades físicas, que las distinguen de las nanopartículas monofasicas, con el fin de desarrollar nuevos materiales con propiedades sintonizables.
Resumen en inglés
The properties of magnetic nanoparticles are governed by the high surface-to-volume ratio and are manifested in dierent phenomena such as superparamangetism, exchangebias, surface magnetic disorder and surface anisotropy. The fabrication of complex multicomponent nanostructures enables a better control of their physical properties and, driven by the current needs for miniaturized devices and the growth of clean energy and nanomedicine, can improve the performance of materials for magnetic recording media, permanent magnets, biomedical applications or catalysis. Since the magnetic moments uctuates when its anisotropy energy is comparable to the thermal energy, the superparamagnetism imposes a limit to the size reduction. In this context, previous studies showed that the eective anisotropy and the exchange-bias eld can be increased as a result of the relationship between the antiferromagnetic anisotropy energy and the interface coupling energy in antiferromagnetic/ferrimagnetic core/shell bimagnetic nanoparticles. This thesis is focused on the design, fabrication and study of new nanostructured materials based on core/shell nanoparticles aiming at tuning the physical properties and understanding the microscopic mechanisms that rule them. Due to their abundance and relatively low costs, transition metal-oxides were employed. Such materials oer a variety of properties, including ferrimagnets with high magnetocrystalline anisotropy (CoFe_2O_4), with composition-dependent anisotropy (mixed Zn-Co or Ni-Co ferrites) or biocompatible (Fe_3O_4), antiferromagnetic monoxides with high anisotropy (CoO) and diamagnetic fotoluminiscent semiconductors (ZnO). Dierent families of multicomponent nanoparticles were synthesized by chemical methods based on the high temperature decomposition of organometallics assisted by surfactants. The materials were studied by means of structural (transmission electron microscopy, X-ray diraction and refl ectivity, thermogravimetry), magnetic (multiple DC and AC magnetometry) and optical (UV-visible and photoluminescence spectroscopy) characterization techniques. Firstly, dierent CoO/CoFe_2O_4 core/shell nanoparticle systems were designed and their size eects were analyzed with the aim of controlling the eective magnetic anisotropy. A remarkable increase of the anisotropy was found when the size is reduced, at the expense of a lower thermal stability for the magnetic moment. It was shown that the coercive eld of 5 nm nanoparticles can be increased up to 30.8 kOe at 5 K, 50 % larger than the maximum value reported up to now for single-phase CoFe_2O_4 nanoparticles; while the thermal stability of the magnetic moment can be increased up to the Neel temperature of CoO, close to room temperature. It was found that, since the CoO core is protected by the ferrite shell, its structural quality, and therefore the eciency of the interface exchange interaction, can be improved by a thermal treatment. In addition, the dierent roles played by surface eects, magnetic interactions and interface eects were identied by the comparison with ZnO/CoFe_2O_4 core/shell nanoparticles, synthesized with anologous size and morphology but a diamagnetic core. The results indicate that the interface interaction is responsible for the larger coercive eld and blocking temperature and the lower activation volume observed for bimagnetic nanoparticles. Next, the introduction of Zn"2+ or Ni"2+ into the ferrite was proposed in order to manipulate the exchange-bias eld and the eective anisotropy. To this extent, novel core/shell CoO/mixed-ferrite bimagnetic nanoparticles were designed and synthesized. It was found that the introduction of Zn"2+, a 3d"10 non-magnetic ion, reduces the interface exchange-coupling leading to a non-monotonic variation of the exchange-bias that results maximum for intermediate Zn concentrations. Such behavior was interpreted by taking into account the competition between the anisotropy energy of the CoO and the interface coupling energy, and by considering the density of coupled-spins a the interface. On the other hand, the introduction of Ni"2+ into the Co-ferrite revealed, in addition to the presence of exchange-bias, important surface and magnetic disorder eects. The diculties to adjust precisely the size of each phase in core/shell structures and the requierements of a systematic study of the size eects on the interface exchangecoupling motivated the fabrication and study of ferrite/ferrite thin lm bilayers. Therefore, high-quality Fe_3O_4/CoFe_2O_4 bilayers with a Fe_3O_4-thickness varying between 0 and 25 nm were produced by pulsed laser deposition and an 8 nm critical Fe_3O_4 thickness was identied: while thicknesses below such value lead to a rigid-coupling regime, larger values promote an exchange-spring behavior. The present study can be useful as a model system for the design of novel bimagnetic nanoparticles with improved properties. Finally, core/shell bifunctional CoFe_2O_4/ZnO nanoparticles were designed, fabricated and its preliminary characterization is reported. Such material is able to generate heat upon the application of a radiofrequency magnetic eld and shows, at the same time, a photoluminescent optical response. In the last years, the continuous progress of nanomedicine has suggested that magnetic nanoparticles can provide solutions to specic biomedical issues. The combination of both functionalities in a nanoparticle system could initiate new studies in the eld of magnetic uid hyperthermia where optical labeling is a key factor, for example, to the evaluation of a systemic delivery of nanoparticles into the body. Current nanotechnology oers powerful tools for the development of advanced magnetic materials, including new chemical synthesis methods and the consolidation of interface-sensitive characterization techniques. The main contribution of this thesis is the design of multicomponent nanoparticles, their study and the interpretation of the complex relationship between their structure and physical properties, which are clearly dierent than single-phase and bulk materials.
| Tipo de objeto: | Tesis (Tesis Doctoral en Ciencias de la Ingeniería) |
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| Palabras Clave: | Anisotropy; Anisotropía; Nanoparticles; Nanopartículas; [Magnetic nanoparticles; Nanopartículas magnéticas; Superparamagnetism; Superparamagnetismo; Nanomedicine; Nanomedicina; Chemical systhesis; Síntesis química ] |
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Monodisperse magneto uorescent nanoplatforms for local heating and temperature sensing. Nanoscale, 6 (22), 13463-13469, 2014. |
| Materias: | Física > Nanotecnología |
| Divisiones: | Gcia. de área de Investigación y aplicaciones no nucleares > Gcia. de Física > Ciencias de materiales > Resonancias magnéticas |
| Código ID: | 607 |
| Depositado Por: | Tamara Cárcamo |
| Depositado En: | 18 May 2017 10:17 |
| Última Modificación: | 18 May 2017 10:17 |
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