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      Isothermal Oxidation of Ti 3Al 0.6Ga 0.4C 2 MAX Phase Solid Solution in Air at 1000 °C to 1300 °C

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          Abstract

          The atomically laminated Ti 2AlC, Ti 3AlC 2 and Cr 2AlC MAX phases, with A = Al, form adherent, passivating α-alumina, Al 2O 3, oxide scales when heated in air. The effect of solid solutions on the A layers in affecting the oxidation kinetics remains a subject of open research. Herein we synthesize a dense bulk polycrystalline Ti 3Al 1−xGa xC 2 (x ≈ 0.4) solid-solution and investigate its isothermal oxidation in ambient air, in the 1000 °C–1300 °C temperature range, for times varying between 15 and 300 h. At 1000 °C, a passivating dense Al 2O 3 layer ( ≈ 1–2.6 μm thick) with near cubic kinetics and an overall weight gain that is slightly less than either Ti 3AlC 2 or Ti 2AlC is formed. At 1200 °C, the Al 2O 3 layer thickens (3.5–12 μm thick) with some scale delamination on the corners initiating at 15 h. At 1300 °C, the Al 2O 3 layer (7.6–20.7 μm thick) wrinkles and Al 2TiO 5 forms. Though the Al 2O 3 grains coarsen at 1200 °C and 1300 °C, the weight gain is higher than that for Ti 3AlC 2 or Ti 2AlC. At around 7 at. %, this is one of the lowest, if not lowest, Al mole fraction in a Ti-based alloy/compound that forms an Al 2O 3 passivating layer. We further provide compelling microstructural evidence, in the form of a duplex oxide, that at 1000 °C, the outward Al flux, J Al, and the inward O flux, J O, are related such that 2 J Al = 3 J O. A fraction of these fluxes combine, at the duplex oxide interface, to nucleate small grains

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              In situ site-specific specimen preparation for atom probe tomography.

              Techniques for the rapid preparation of atom-probe samples extracted directly from a Si wafer are presented and discussed. A systematic mounting process to a standardized microtip array allows approximately 12 samples to be extracted from a near-surface region and mounted for subsequent focused-ion-beam sharpening in a short period of time, about 2h. In addition, site-specific annular mill extraction techniques are demonstrated that allow specific devices or structures to be removed from a Si wafer and analyzed in the atom-probe. The challenges presented by Ga-induced implantation and damage, particularly at a standard ion-beam accelerating voltage of 30 keV, are shown and discussed. A significant reduction in the extent of the damaged regions through the application of a low-energy "clean-up" ion beam is confirmed by atom-probe analysis of the damaged regions. The Ga+ penetration depth into {100} Si at 30 keV is approximately 40 nm. Clean-up with either a 5 or 2 keV beam reduces the depth of damaged Si to approximately 5 nm and <1 nm, respectively. Finally, a NiSi sample was extracted from a Si wafer, mounted to a microtip array, sharpened, cleaned up with a 5 keV beam and analyzed in the atom probe. The current results demonstrate that specific regions of interest can be accessed and preserved throughout the sample-preparation process and that this preparation method leads to high-quality atom probe analysis of such nano-structures.
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                Author and article information

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                Journal
                Journal of The Electrochemical Society
                J. Electrochem. Soc.
                The Electrochemical Society
                0013-4651
                1945-7111
                March 23 2022
                March 01 2022
                March 23 2022
                March 01 2022
                : 169
                : 3
                : 031510
                Article
                10.1149/1945-7111/ac58c1
                95ba6e55-fa9b-446b-afb4-4be6b3657807
                © 2022

                https://iopscience.iop.org/page/copyright

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