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Conventional studies of structure-property relationships for polycrystalline materials have focused either on descriptions of the morphological aspects of the microstructure, such as grain size and shape, or on the chemistry and structure of individual grain boundaries using transmission electron microscopy (TEM). TEM, while capable of determining the misorientation of adjacent grains, can provide information only for a small number of boundaries. A more complete description of a polycrystal requires the lattice orientations of a statistically significant number of grains, coupled with the morphological aspects, such as grain size and shape. This description can be obtained using a relatively new technique known as orientation imaging microscopy (OIM), which utilizes crystallographic orientation data obtained from Backscattered Electron Kikuchi patterns (BEKP) collected using a scanning electron microscope. This paper describes the OIM results for Al2O3. The results include image quality maps, grain boundary maps, pole figures, and lattice misorientations depicted on MacKenzie plots and in Rodrigues space. High quality BEKP were obtained and the images and data readily reveal the grain morphology, texture, and grain boundary misorientations, including those for cracked boundaries.
Oxide on a stress corrosion cracked region of TT Alloy 600 exposed to a nuclear power plant for over 20 years was analyzed using TEM-EDS for a sample prepared by an FIB. Pb above 10 wt% was observed in the oxide on the pulled TT Alloy 600 tubes presuming that Pb affects SCC to some extent. The oxide structure in the crack was fairly consistent with the laboratory grown oxide, indicating that the oxide grown in the real operational condition is formed in a similar way. The oxide property on TT Alloy 600 was investigated as a function of the immersion time in 0.1 M NaOH with 1000 ppm PbO at 315 C using SEM, TEM, TEM-EDS, and EIS in view of the passivity and chemical composition. Electrochemical impedance was increased to an almost saturation value with the immersion time in a leaded solution while the oxide was increased to a steady state thickness. However, electrochemical impedance was decreased to an almost constant value with the immersion time in un-leaded solution suggesting that the Pb mainly affects the oxide passivity on early days. Moreover the electrochemical behavior of TT Alloy 600 was understood by analyzing the potentiodynamic polarization curve in 0.1 M NaOH with/without PbO.
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