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Protocols for conducting in situ transmission electron microscopy (TEM) reactions using an environmental TEM with dry gases have been well established. However, many important reactions that are relevant to catalysis or high-temperature oxidation occur at atmospheric pressure and are influenced by the presence of water vapor. These experiments necessitate using a closed-cell gas reaction TEM holder. We have developed protocols for introducing and controlling water vapor concentrations in experimental gases from 2% at a full atmosphere to 100% at ~17 Torr, while measuring the gas composition using a residual gas analyzer (RGA) on the return side of the in situ gas reactor holder. Initially, as a model system, cube-shaped MgO crystals were used to help develop the protocols for handling the water vapor injection process and confirming that we could successfully inject water vapor into the gas cell. The interaction of water vapor with MgO triggered surface morphological and chemical changes as a result of the formation of Mg(OH)2, later validated with mass spectra obtained with our RGA system with and without water vapor. Integrating an RGA with an in situ scanning/TEM closed-cell gas reaction system can thus provide critical measurements correlating gas composition with dynamic surface restructuring of materials during reactions.
This study applies atom probe tomography (APT) to analyze the oxide scales formed on model NiAlCr alloys doped with Hf, Y, Ti, and B. Due to its ability to measure small amounts of alloying elements in the oxide matrix and its ability to quantify segregation, the technique offers a possibility for detailed studies of the dopant’s fate during high-temperature oxidation. Three model NiAlCr alloys with different additions of Hf, Y, Ti, and B were prepared and oxidized in O2 at 1,100°C for 100 h. All specimens showed an outer region consisting of different spinel oxides with relatively small grains and the protective Al2O3-oxide layer below. APT analyses focused mainly on this protective oxide layer. In all the investigated samples segregation of both Hf and Y to the oxide grain boundaries was observed and quantified. Neither B nor Ti were observed in the alumina grains or at the analyzed interfaces. The processes of formation of oxide scales and segregation of the alloying elements are discussed. The experimental challenges of the oxide analyses by APT are also addressed.
Ni-based fcc alloys are frequently used as critical structural materials in nuclear energy applications. Despite extensive studies, fundamental questions remain regarding point defect migration and solute segregation as a function of grain boundary character after irradiation. In this study, a coupled experimental and modeling approach is used to understand the response of grain boundary character in a model Ni–5Cr alloy after high temperature heavy-ion irradiation. Radiation-induced segregation and void denuded zones were experimentally examined as a function of grain boundary character, while a kinetic rate theory model with grain boundary character boundary conditions was used to theoretically model Cr depletion in the alloy system. The results highlight major variations in the radiation response between the coherent and incoherent twin grain boundaries, but show limited disparity in defect sink strength between random low- and high-angle grain boundary regimes.