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Nanometer-scale crystallographic structure and orientation of a NbTiN/AlN/NbTiN device stack grown via plasma-assisted molecular beam epitaxy on c-plane sapphire are reported. Structure, orientation, interface roughness, and thickness are investigated using correlative four-dimensional scanning transmission electron microscopy and atom probe tomography (APT). This work finds NbTiN that is rock salt structured and highly oriented toward ⟨111⟩ with rotations about that axis corresponding to step edges in the c-plane sapphire with a myriad of twin boundaries that exhibit nanoscale spacing. The wurtzite (0001) AlN film grown on (111) NbTiN exhibits nm-scale changes in the thickness resulting in pinhole shorts across the barrier junction. The NbTiN overlayer grown on AlN is polycrystalline, randomly oriented, and highly strained. APT was also used to determine local changes in chemistry within the superconductor and dielectric. Deviation from both intended cation:cation and cation:anion ratios are observed. The results from conventional and nanoscale metrology highlight the challenges of engineering nitride trilayer heterostructures in material systems with complicated and understudied phase space.
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Atom Probe Tomography Analysis of Mica
Abstract Laser-assisted atom probe tomography (APT) is a relatively new, powerful technique for sub-nanometric mineral and biomineral analysis. However, the laser-assisted APT analysis of highly anisotropic and chemically diverse minerals, such as phyllosilicates, may prove especially challenging due to the complex interaction between the crystal structure and the laser pulse upon applying a high electric field. Micas are a representative group of nonswelling clay minerals of relevance to a number of scientific and technological fields. In this study, a Mg-rich biotite was analyzed by APT to generate preliminary data on nonisotropic minerals and to investigate the effect of the crystallographic orientation on mica chemical composition and structure estimation. The difference in results obtained for specimens extracted from the (001) and (hk0) mica surfaces indicate the importance of both experimental parameters and the crystallography. Anisotropy of mica has a strong influence on the physicochemical properties of the mineral during field evaporation and the interpretation of APT data. The promising results obtained in the present study open the way to future innovative APT applications on mica and clay minerals and contribute to the general discussion on the challenges for the analysis of geomaterials by atom probe tomography.
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- Award ID(s):
- 2019870
- PAR ID:
- 10392476
- Publisher / Repository:
- Oxford University Press
- Date Published:
- Journal Name:
- Microscopy and Microanalysis
- Volume:
- 28
- Issue:
- 4
- ISSN:
- 1431-9276
- Format(s):
- Medium: X Size: p. 1207-1220
- Size(s):
- p. 1207-1220
- Sponsoring Org:
- National Science Foundation
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