Buitrago Montañez, Nayibe L. (2019) Radiografía neutrónica avanzada de componentes nucleares base circonio / Advanced neutron radiography of nuclear components-zirconium base. Tesis Doctoral en Ciencias de la Ingeniería, Universidad Nacional de Cuyo, Instituto Balseiro.
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Resumen en español
Las aleaciones base circonio (Zr) utilizadas en los componentes de los reactores nucleares se encuentran en contacto con el refrigerante, por lo que incorporan hidrógeno (H) o deuterio (D) como resultado de un moderado proceso de corrosión, produciendo la fragilización del material debido a la precipitación de hidruros. En presencia de campos de tensiones, aparece el proceso conocido como fractura asistida por hidruros (Delayed Hydride Cracking-DHC), que involucra la migración de H a zonas de altas tensiones, y el crecimiento de fisuras por precipitación y ruptura de hidruros. Por esto, el contenido de H en estas aleaciones está directamente relacionado con su vida útil. El desarrollo de técnicas no destructivas para el estudio de la difusión de H en aleaciones base Zr posibilitará la visualización de la redistribución de H, ayudando a una interpretación más clara del proceso de DHC, muy difícil de alcanzar por métodos destructivos de caracterización. La radiografía de neutrones es equivalente a la radiografía con rayos X, pero con un contraste diferente y muchas veces complementario, ya que presenta una atenuación importante para muchos elementos livianos (H, B, Li). Así, el coeficiente de atenuación de neutrones del hidruro de circonio es ~25 veces mayor que el del Zr metálico, lo cual posibilita cuántica pequeños contenidos de H en forma no destructiva. En la presente tesis hemos utilizado la radiografía de neutrones para cuantificar la distribución espacial de bajos contenidos de H en muestras de aleaciones de Zr. Losexperimentos para explorar la factibilidad de la técnica fueron realizados sobre un conjunto de muestras de Zircaloy-2 y Zr-2.5Nb con contenidos conocidos de H en cuatro instrumentos de neutrones de características diferentes. Todos estos instrumentos pudieron resolver satisfactoriamente muy bajos contenidos de hidrogeno (0-300 wt ppm) en las aleaciones estudiadas, aunque con una resolución espacial y tiempo de medición dependientes de la colimacion, el flujo y el sistema de detección disponibles en cada caso. Además, se demostró que usando el protocolo de medición y la metodología de análisis de imágenes propuestos, es posible cuantificar el contenido de H con una resolución de ~5 wt ppm, una precisión de ~10 wt ppm y una resolución espacial de ~25μmx5mmx10mm para una línea de imágenes de neutrones fríos, de características similares a la que se instalará en el Laboratorio de Haces de Neutrones del reactor RA-10. Los estudios de difusión de H en aleaciones base Zr presentan gran variabilidad en los coeficientes de difusión reportados, debido en parte a diferencias entre las técnicas experimentales utilizadas, y en parte por diferencias intrínsecas en los posibles caminos para la difusión de H que aparecen en distintas microestructuras. En particular, existe evidencia que la solubilidad total de H y el coeficiente de difusión de H en las distintas fases cristalinas son muy diferentes, por lo que la difusión en una aleación de H compuesta de varias fases dependerá del volumen y la morfología de las fases presentes. Partiendo de la técnica de determinación de H desarrollada, hemos optimizado un método pre-existente para la determinación del coeficiente de difusión de H, que permite realizar estudios en forma no-destructiva en muestras de pequeñas dimensiones (10x10x4mm3) en el rango de temperaturas en las que trabajan estas aleaciones en reactores nucleares de potencia. Con este método se estudió la difusión de H a lo largo de distintas direcciones de chapas laminadas de Zircaloy-2 y Zr-2.5Nb para temperaturas entre 250°C y 350°C; la primera compuesta casi exclusivamente por β-Zr y la segunda conteniendo ~10% de fase βZr. Se encontró que la difusión de H en Zircaloy-2 laminado en frío, compuesto principalmente de granos α-Zr redondeados, es casi isotrópica y no varía significativamente cuando el material es relevado de tensiones y/o recristalizado. Los valores obtenidos ((D=6.80 ± 0.80)x10-¹¹1 m²/s a 300°C) coinciden con medidos por otras técnicas, reportados en la literatura. Como contrapartida,en chapas de Zr-2.5Nb compuestas de granos α-Zr alargados separados por delgadas láminas de fase β-Zr, la difusión es claramente anisotropía y presenta valores considerablemente mayores a los del Zircaloy-2 (D = (2.16± 0.43) x10-¹° m2/s en la dirección normal y D = (5.67± 1.9) x10-¹° m²/s en la dirección de laminado a 300ºC). Más aun, tras un tratamiento térmico a 860ºC durante 3h, la anisotropía observada en la difusión de H se invierte (D= (3.9± 0.4)x10-¹° m²/s en la dirección normal y D= (1.44 ±0.14) x10-¹° m²/s en la dirección de laminado a T=300°C). Esto puede ser explicado por cambios en la conectividad de la fase β-Zr producto de la doble transformación de fase que ocurre durante el tratamiento. Estos resultados demuestran la potencialidad de la técnica desarrollada y prevén su extensión al estudio de la difusión de H en otros materiales. Por ultimo, con el objeto de mejorar la exactitud de la técnica de determinación de H y prescindir del uso de patrones de calibración, se estudió el coeficiente de atenuación de las aleaciones Zircaloy-2 y Zr-2.5Nb con distintas cantidades de H en función de la longitud de onda y se lo comparó con cálculos teóricos. Se encontró que utilizando neutrones con longitudes de onda mayores a 5.7 ºA permitirán determinar contenidos de H en el rango de 1-300 wt ppm H sin la necesidad de muestras de calibración y alcanzar una exactitud mejor que 5 wt ppm H.
Resumen en inglés
Zr-based alloys are used in nuclear power plants because of a unique combination of very low neutron absorption and excellent mechanical properties and corrosion resistance at operating conditions. However, Hydrogen (H) or Deuterium ingress due to waterside corrosion during operation can embrittle these materials. In particular, Zr alloys are affected by Delayed Hydride Cracking (DHC), a stress-corrosion cracking mechanism operating at very low H content (~100-300 wt ppm), which involves the diffusion of H to the crack tip, followed by crack growth through precipitation and rupture of hydrides. Hence, H content in Zr alloy specimen may have a profound impact on its service life. Development of non-destructive techniques to directly visualize H diffusion in Zr alloys would greatly contribute to a better understanding of the DHC process, very difficult to achieve by destructive techniques. Neutron radiography is a technique similar and complementary to conventional X-ray radiography, with no clear dependence on Z, and a particularly large attenuation for several light elements (H, B. Li). So the neutron attenuation coefficient in zirconium hydride is ~25 times larger than in metal Zr, which opens the possibility to quantify very low content H profiles in Zr alloys by non-destructive tests. In this work, we have used neutron imaging to non-destructively quantify the spatial distribution of H in Zr alloys specimens. Feasibility experiments were performed in a set of Zircaloy-2 and Zr-2.5Nb samples with calibrated H contents in four neutron instruments worldwide. All beamlines were able to resolve very low H contents (0-300 wt ppm H) in those alloys, yet with differences on spatial resolution and counting times, depending on the neutron beam collimation, neutron ux and detection system available at each instrument. This showed that by following the proposed measurement protocol and image analysis procedure, it is possible to quantify H contents with a resolution of ~5 wt ppm, an accuracy of ~10 wt ppm and a spatial resolution of ~ 25μmx5mm x10 mm in a cold neutron imaging beamline, similar to the one to be installed at the Argentinean Neutron Beam Laboratory (LAHN) of the RA-10 reactor. Diffusion coefficients of H in Zr alloys found in the literature show large variability, partly due to the different techniques used in each work, and partly due to real differences in the diffusion paths that are available to H in different microstructures. In particular, it has been reported that H terminal solubility and diffusion coefficients in α-Zr and β-Zr are very different, so the actual diffusion coefficient in an alloy composed by both phases will depend on the volume and morphology of the two phases. Here, we have combined a traditional technique used to determine diffusion coefficients with the previously developed neutron imaging technique to non-destructively determine diffusion coefficients within the operational range of Zr alloys in nuclear power plants, using relatively small specimens (4x10x10 mm3). Using this optimized method, we studied H diffusion along different directions of rolled Zircaloy-2 and Zr- 2.5Nb plates for temperatures between 250°C and 350°. The former alloy is almost exclusively composed by β-Zr, whilst the later typically contains 10% of β phase. We found that H diffusion in cold rolled Zircaloy-2, composed mainly by rounddigrains, is nearly isotropic an does not change significantly upon common thermal treatments (stress relief, recrystallization). Measured values ((6.80± 0.80)x10-¹¹ m²/s at 300°C) agree well with those found by other techniques. On the other hand, H diffusion in Zr-2.5Nb plates composed by elongated _ grains surrounded by filaments of β phase is clearly anisotropic, and much larger than in Zircaloy-2 (D = (2.16±0.43)x10-¹° m²/s along the normal direction and D = (5.67 ±1.9)x10-¹° m²/s along the rolling direction, both at 300°C). Moreover, the diffusion anisotropy inverts after a thermal treatment of 3h at 860°C (D=(3.9 ±0.4)x10-¹° m²/s along the normal diffrection and D= (1.44±0.14)x10-¹° m²/s along the rolling direction, both at 300°C). These results can qualitatively be explained by changes in the connectivity of the β phase induced by the thermal treatment, as a result of the double phase transformation α-β-α. These results illustrate the capability of the technique and envisage its future application to the study of H diffusion in other materials. Finally, with the goal of improving the accuracy of the technique for H determination and to allow its application without calibrated standards, we measured the dependence of neutron wavelength on the attenuation coefficient of Zircaloy-2 and Zr-2.5Nb specimens with different H contents, and compared it with theoretical calculations. We found that calibrated standards can be avoided by taking images with neutrons having wavelengths longer than 5.7 °A, with an expected accuracy better than 5 wt ppm H.
| Tipo de objeto: | Tesis (Tesis Doctoral en Ciencias de la Ingeniería) |
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| Palabras Clave: | Zirconium alloys; Aleaciones de circonio; [Neutron imaging; Radiografía de neutrones; Hydrogen diffusion; Difusión de hidrógeno] |
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| Materias: | Ingeniería > Neutrografía Ingeniería > Degradación de Hidrógeno por Circonio |
| Divisiones: | Energía nuclear > Ingeniería nuclear > Física de neutrones |
| Código ID: | 866 |
| Depositado Por: | Tamara Cárcamo |
| Depositado En: | 22 Mar 2021 10:08 |
| Última Modificación: | 12 Abr 2021 12:32 |
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