Melone, Mauro (2023) Estudio de la influencia del proceso de conformado en las propiedades de cables superconductores de Ti/Mg(B1-xCx)2 / Study of the influence of the forming process on the properties of superconducting Ti/Mg(B1-xCx)2. Tesis Doctoral en Física, Universidad Nacional de Cuyo, Instituto Balseiro.
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Resumen en español
En esta tesis se estudió la influencia del proceso de conformado en la microestructura y propiedades superconductoras de cables compuestos de Ti/Mg(B_1–xC_x )_2 realizados por el método Powder In Tube. En primera instancia, se estudió la influencia del dopaje con carbono, la temperatura y el tiempo de sinterizado en la síntesis de pastillas de Mg(B_1–xC_x )_2. En segunda instancia, se estudió la influencia del proceso de conformado en la textura cristalográfica. Por ultimo, se estudió la influencia del conformado en la microestructura de la vaina de Ti. Para estudiar la influencia del nano-SiC y el uso del B dopado con carbono en la síntesis controlando su temperatura y tiempo, se realizaron síntesis a distintas temperaturas y períodos de tiempo, con distintos niveles de dopaje, para luego analizar su estructura y microestructura por difracción de rayos X y microscopía electrónica de transmisión; y sus temperaturas críticas y densidades de corriente crítica por magnetometría SQUID. Complementariamente, se estudiaron las reacciones que suceden durante la síntesis, para distintos niveles de dopaje mediante análisis térmico diferencial y termogravimetría simultáneos (DTA-TG) y se analizaron los difractogramas por refinamiento Rietveld. Se pudo encontrar una ruta de síntesis con dopaje en un paso que permite obtener un polvo precursor con buenas propiedades superconductoras para la formación de cables por el método Powder In Tube. Para estudiar la influencia del proceso de conformado en la textura cristalográfica se usaron cables Ti/Mg(B_1–xC_x )_2 realizados por el método Powder In Tube en dos configuraciones monofilamentarias distintas: una hexagonal y una circular. Se estudió la textura de ambos materiales generando figuras de polo incompletas por difracción de rayos X, para luego generar la función distribución de orientaciones. Además, se determinó la densidad de corriente crítica para distintas direcciones de la muestra con el uso del magnetómetro SQUID. Finalmente, se analizó la correlación entre ambas propiedades mediante la determinación de los factores de Kearns a partir de la función distribución de orientaciones y de la anisotropía en la densidad de corriente crítica. Se pudo determinar que, para ambas configuraciones de cables, la textura cristalográfica de la vaina de Ti no influye en la textura cristalográfica del núcleo de Mg(B_1–xC_x )_2. Así mismo, se pudo correlacionar la anisotropía en la densidad de corriente crítica con la anisotropía en el núcleo de Mg(B_1–xC_x )_2 mediante los factores de Kearns. Para estudiar la influencia del conformado en la microestructura de la vaina de cables Ti/Mg(B_1–xC_x )_2 realizados por el método Powder In Tube, se estudió la microestructura sobre la superficie tangencial de una muestra cortada y pulida, mediante mapas de Electron Backscater Difraction. Complementariamente, se obtuvo una lamela de la misma superficie mediante FIB-SEM para estudiarla por microscopía electrónica de transmisión. Se encontró, por ambas técnicas, la presencia de una fase delta, minoritaria y metaestable. Esta fase delta podría aumentar la dureza de la vaina, generando un aumento en la densidad del núcleo de Mg(B_1–xC_x )_2, que puede ser clave para mejoras en sus propiedades superconductoras. En síntesis, se lograron establecer condiciones que optimizan el proceso de preparación del MgB_2, tanto en bulk como en alambres powder in tube (PIT), tendientes a mejorar sus propiedades superconductoras. La comprensión de las condiciones del proceso son fundamentales para mejorar el proceso de conformado de cables PIT de Ti/MgB_2 para cualquiera de sus aplicaciones en cables o bobinas.
Resumen en inglés
’Study of the influence of the conformation process on the properties of superconducting Ti/Mg(B_1−xC_x)_2 wires’ In this thesis, we study the influence of the forming process on the microstructure and superconducting properties of Ti/Mg(B_1–xC_x )_2 composite wires made by the Powder In Tube method. Firstly, we study the influence of carbon doping, temperature, and sintering time on the synthesis of Mg(B_1–xC_x )_2 pellets. Secondly, we study the influence of the forming process on the crystallographic texture. Finally, we study the influence of manufacturing on the microstructure of the Ti sheath. To study the influence of nano-SiC and the use of carbon-doped B in the synthesis by controlling its temperature and time, syntheses were carried out at different temperatures and periods, with different doping levels, to then analyse its structure and microstructure by X-ray diffraction and transmission electron microscopy. Also, we determine its critical temperatures and critical current densities by SQUID magnetometry. The reactions occurring during the synthesis were studied for different doping levels by simultaneous differential thermal analysis and thermogravimetry (DTA-TG) and the diffractograms were analysed by Rietveld refinement. We found a one-step doped synthesis route to obtain a precursor powder with good superconducting properties for the formation of wires by the Powder In Tube method. To study the influence of the forming process on the crystallographic texture, we used Ti/Mg(B_1–xC_x )_2 wires made by the Powder In Tube method in two different monofilament configurations: a hexagonal and a circular one. The texture of both materials was studied by generating incomplete pole figures by X-ray diffraction, to generate the orientation distribution function. In addition, the critical current density was determined for different directions of the sample using the SQUID magnetometer. Finally, the correlation between both properties was analysed by determining the Kearns factors from the orientation distribution function and the anisotropy in the critical current density. We determined that, for both wire configurations, the crystallographic texture of the Ti sheath does not influence the crystallographic texture of the Mg(B_1–xC_x )_2 core. Likewise, it was possible to correlate the anisotropy in the critical current density with the anisotropy in the Mg(B_1–xC_x )_2 core employing Kearns factors. To study the influence of the forming on the microstructure of the Ti/Mg(B_1–xC_x )_2 sheath of wires made by the Powder In Tube method, we studied the microstructure on the tangential surface of a cut and polished sample by Electron Backscatter Diffraction mapping. Complementarily, a lamella of the same surface was obtained by FIB-SEM to study it by transmission electron microscopy. Both techniques showed the presence of a delta phase, a minor metastable phase. This delta phase could increase the hardness of the sheath, generating an increase in the density of the Mg(B_1–xC_x )_2 core, which could be key to eventually improving its superconducting properties. In summary, we were able to establish conditions that optimise the preparation process of MgB_2, both in bulk and PIT wires, tending to improve their superconducting properties. Understanding the process conditions are critical to improving the process of forming Ti/MgB_2 PIT wires for any of its cable or coil applications.
| Tipo de objeto: | Tesis (Tesis Doctoral en Física) |
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| Palabras Clave: | Superconductors; Superconductores; Microstructure; Microestructura; Crystallography; Cristalografía; [Magnesium diboride; Diboruro de magnesio Powder in tube] |
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| Materias: | Física > Física del estado sólido Física > Ciencias de materiales |
| Divisiones: | Aplicaciones de la energía nuclear > Tecnología de materiales y dispositivos > Caracterización de materiales |
| Código ID: | 1217 |
| Depositado Por: | Tamara Cárcamo |
| Depositado En: | 18 Oct 2023 10:37 |
| Última Modificación: | 18 Oct 2023 10:37 |
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