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Updated: Oct 11, 2025

Quantitative Atomic-Site Analysis of Functional Dopants/Point Defects in Crystalline Materials by Electron-Channeling-Enhanced Microanalysis
Published on: May 10, 2021
Energy-dispersive X-ray spectroscopy and atom-probe tomography data quantifying component-ratios of multicomponent
Karen Kruska1, Weilin Jiang1, Xuemei Wang2
1Energy and Environment Directorate, Pacific Northwest National Laboratory, P.O. Box 999, Richland, WA, 99352, USA.
Abstract:
Samples of ∼1 µm films of CeO2 doped with 2 wt% Mo, 1.5 wt% Ru, 0.75 wt% Pd, 0.5 wt% Re and 0.25 wt% Rh grown with pulsed laser deposition were irradiated with I2+ ions (610 °C and 730 °C, 1016 and 5 × 1016 I2+/cm2). For selected samples post-irradiation heat treatment was conducted (900 °C, 1100 °C). The specimens were sectioned with focused ion beam milling and characterized in a transmission electron microscope with energy-dispersive x-ray spectroscopy, and with atom-probe tomography. Energy-dispersive x-ray spectroscopy was used to obtain elemental maps showing the distribution of dopants in the specimen after exposure. Some of these maps are discussed in detail in our companion article "Formation of multicomponent alloy particles in doped ceria under I2+ ion irradiation and thermal annealing" in the Journal of Nuclear Materials [1]. Advanced computational analysis could be used to more accurately quantify local compositions. Data is provided for additional regions of interest and one additional irradiation condition. The doped ceria film that was heat treated at 1100 °C delaminated from the substrate in most places. Samples were extracted from the underside of a delaminated piece and analyzed with atom-probe tomography. The resulting data show ceria and a Mo-rich particle and demonstrate that this approach is feasable in principle to study local compositions in a sample exposed to such extreme conditions.
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