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Origen, propiedades y efectos del avejentamiento en la superficie de monocristales del superconductor ꞵ-FeSe / Origin, properties and effects of ageing at the surface of single crystals of the ꞵ-FeSe superconductor

Lanoël, , Lucio (2023) Origen, propiedades y efectos del avejentamiento en la superficie de monocristales del superconductor ꞵ-FeSe / Origin, properties and effects of ageing at the surface of single crystals of the ꞵ-FeSe superconductor. Tesis Doctoral en Física, Universidad Nacional de Cuyo, Instituto Balseiro.

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Resumen en español

El compuesto binario superconductor β-FeSe es un sistema laminar de hierros unidos con selenios en el plano mediante uniones de tipo covalentes, formando capas que están unidas por fuerzas de Van der Waals a lo largo del eje-c. Este sistema posee una estructura tetragonal simple, de tipo anti-PbO (grupo espacial P4_nmm) el cual posee una transición electrónica-estructural a una temperatura de ∼90 K, donde la estructura pasa a ser ortorrómbica y la transición de fase electrónica, llamada transición hemática, se caracteriza por la aparición de magnetoresistencia positiva cuando se aplica campo paralelo al eje-c. Este sistema, a diferencia de otros de su mismo tipo, no muestra transición de orden magnético hasta la temperatura de transición de fase superconductora que suele estar en Tc=8 K. Durante el proceso de caracterización de este sistema, observamos mediante espectroscopia Raman, la aparición de un modo vibracional en ≈250 cm"−1, el cual no es esperado para el sistema de bulto de este compuesto. En este trabajo se realizó un estudio exhaustivo mediante variadas técnicas en la búsqueda de entender este fenómeno que era promovido por el paso del tiempo. Se tomaron espectros Raman en un amplio rango de temperaturas, 5-773 K. Se hicieron ajustes Lorentzianos de todos los espectros tomados con los que se determinó la dependencia en temperatura tanto de la energía como de la sección eficaz Raman. Se estudió la composición química, en perfil de profundidad utilizando la técnica de comido iónico en un equipo de espectroscopia por fotoemisión de electrones, de muestras donde se observaba y otras donde no se observaba la nueva señal Raman. Se tomaron mediciones de transporte eléctrico en función de la temperatura en muestras que tenían esta característica propia del paso del tiempo, donde se observaron mejoras en las propiedades superconductoras, obteniendo una temperatura de inicio de la transición superconductora, TO_nset = 14K, y una temperatura crítica (temperatura a la que la resistencia de la muestra es cero), Tc=10 K. Se propuso un modelo para explicar el fenómeno, y se resolvieron mediante teoría de grupos los modos vibracionales esperados para una sola lámina de β-FeSe. Del modelo se desprende la aparición de un nuevo pico, que se debe a que en el nuevo grupo de simetría un modo que no es Raman activo en el bulto, si lo es para el sistema bidimensional. El ajuste teórico-experimental fue muy bueno (R"2 > 0.99) y las dependencias en polarización que se esperan están de acuerdo con las observadas. Además la energía de unión covalente que se obtiene del ajuste, es consistente con lo calculado en simulaciones de este compuesto. Además se observaron modos vibracionales interlaminares predichos en este sistema, pero que no fueron reportados al momento de escritura de este trabajo. A partir de la energía de este modo, mediante un modelo simple unidimensional, podemos calcular la constante de acoplamiento del sistema y la misma es razonable en relación a las que se obtienen en otros compuestos laminares. Finalmente, se tomaron espectros Raman en una muestra del compuesto β-FeTe, el cual tiene una estructura cristalina análoga al β-FeSe, en busca de un fenómeno similar al observado, y basándonos en trabajos presentes en la literatura, se determinó que en estas familias de compuestos calcogenuros y dicalcogenuros de metales de transición, se forman alótropos del calcógeno correspondiente en la superficie del mismo. En este trabajo se logró determinar cual es el proceso que da lugar al envejecimiento de este compuesto. ´Este, es un proceso de degradación de la superficie poco convencional en el que se observa un estadio intermedio formado por varios compuestos. La superficie avejentada está compuesta por una mezcla de ´oxido de hierro, selenio amorfo, FeSe en estado iónico y el compuesto original β-FeSe. El remanente de β-FeSe en esta capa avejentada resultaría desacoplado del bulto, lo que produciría la aparición de un nuevo modo Raman prohibido para el bulto, pero esperado para una sola lámina de β-FeSe, es decir, para β-FeSe bidimensional. Este resultado se deprende de resolver cuales serían los modos vibracionales esperados y sus energías, para β-FeSe bidimensional. La energía, actividad Raman y dependencia en polarización del nuevo pico en 250 cm"−1 se encuentra de acuerdo con lo observado mediante espectroscopia Raman y este desacoplamiento de las primeras capas superficiales explicaría además las mejoras en las propiedades superconductoras observadas en mediciones de transporte eléctrico. Además se observaron modos interlaminares de baja energía. Éstos, fueron predichos pero aun no reportados para este compuesto al momento de escritura de esta tesis. Estos resultados necesitan de más experimentos y modelos mas complejos para ser entendidos mejor. Por último observamos en experimentos Raman en cristales de β-FeTe el mismo fenómeno de avejentamiento, que en este caso, da lugar a señal de teluro amorfo en la superficie de cristales avejentados que al clivar se recupera la señal del compuesto original. Este resultado, junto con reportes de aparición de un pico en 250 cm"−1 en distintos seleniuros, como ser: Bi_2Se_3, MoSe_2, TiSe_2 y TaSe_2 sugiere que el proceso de envejecimiento y degradación de la superficie que resulta en señal Raman del calcógeno del que este formado el compuesto en estado amorfo en la superficie es ubicuo a todos los compuestos calcogenuros.

Resumen en inglés

The superconducting β-FeSe binary compound is a layered system of irons bounded with selenium atoms by covalent unions, forming layers that are bounded to each other by Van der Waals forces along the c-axis. This system has a simple tetragonal structure, of anti-PbO (space group P4_nmm) which has a structural-electronic phase transition at T ∼90 K. Below this temperature, the structure becomes orthorhombic and the electronic phase transition, called nematic transition, is characterized by the appearance of positive magnetoresistance when field is applied parallel to the c-axis. Particularly, this system, unlike others of the same type, does not show a magnetic order transition down to the superconducting phase transition temperature, which is usually at Tc=8 K. During the characterization process of this system, the appearance of a vibrational mode at ≈250 cm"−1 was observed by Raman spectroscopy. This feature is not expected for the bulk system of this compound. In this work, a comprehensive study was carried out, using various techniques, to understand this phenomenon, which was promoted by aging. Raman spectra were taken over a wide range of temperatures, 5-773 K. Lorentzian fits were made to all the spectra taken, from which the energy and the Raman cross section as a function of temperature, were determined. The chemical composition of the samples, with and without the new Raman signal, was studied using Argon ion sputtering depth profiling technique in an X-ray Electron Photoemission Spectroscopy (XPS) equipment. Electrical transport measurements were taken on aged samples as a function of temperature. Improvements in superconducting properties were observed, obtaining a superconducting transition temperature of Tc=10 K. A model was proposed to explain the phenomenon. The expected vibrational modes for a single β-FeSe sheet (bidimensional system) were solved by group theory. The model shows the appearance of a new peak, which, in the new symmetry group, is Raman active, but can not be observed for the bulk system. The theoretical-experimental fit was good (R"2 > 0.99) and the expected polarization dependencies agree with the observed ones. In addition, the covalent bonding energy obtained from the fit is consistent with the one obtained in simulations for this compound. In addition, predicted interlaminar vibrational modes were observed in this system, which were not reported up to the time this thesis was written. From the energy of these modes, using a simple one-dimensional model, the coupling constant of the system was calculated. The result is reasonable, in comparison with those obtained in ther laminar compounds. Finally, Raman spectra were taken on a β-FeTe sample, which has an analogous crystal structure to the β-FeSe one, in the search for a similar phenomenon to the observed one. Based on works present in the literature, and our results, we determined that in these families of transition metal chalcogenides and dichalcogenides compounds, allotropes of the corresponding chalcogenides are formed on the surface of the compound. In this work it was possible to determine which is the process that gives rise to aging of this compound. This is an unconventional process of degradation of the surface in which an intermediate stage formed by several compounds is observed. The aged surface is composed of a mixture of iron oxide, amorphous selenium, FeSe in ionic state and the original compound β-FeSe. The remaining β-FeSe in this aged layer would become unbonded from the bulk, which would produce the appearance of a new Raman mode prohibited for the bulk, but expected for a single sheet of β-FeSe, that is, for two-dimensional β-FeSe. This result is derived from resolving the expected vibrational modes and their energies for bidimensional β-FeSe. The energy, Raman activity and polarization dependence of the new peak at 250 cm"−1 is in agreement with that observed by Raman spectroscopy and this unbonding of the first superficial sheets would also explain the improvements in the superconducting properties observed in electrical transport measurements. In addition, low energy interlaminar modes were observed. These were predicted but not yet reported for this compound at the time of writing this thesis. These results need more experiments and more complex models to be better understood. Lastly, we observed in Raman experiments on β-FeTe crystals the same aging phenomenon, which in this case, gives rise to an amorphous tellurium signal on the surface of aged crystals which, when cleaving, recovers the signal of the original compound. This result, along with reports of the appearance of a peak at 250 cm"−1 in different selenium compounds such as: Bi_2Se_3, MoSe_2, TiSe_2 and TaSe_2 suggests that the process of aging and degradation of the surface that results in Raman signal of the chalcogen from which the compound is formed in the amorphous state at the surface, is ubiquitous to all chalcogenide compounds.

Tipo de objeto:Tesis (Tesis Doctoral en Física)
Palabras Clave:Raman spectroscopy; Espectroscopia raman; Superconductivity; Superconductividad;[Iron based superconductors; Superconductores basados en hierro]
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Materias:Física > Superconductividad
Divisiones:Gcia. de área de Investigación y aplicaciones no nucleares > Gcia. de Física > Materia condensada > Bajas temperaturas
Código ID:1198
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