Atomic-scale chemical quantification of oxide interfaces using energy-dispersive X-ray spectroscopy

2013 ◽  
Vol 102 (17) ◽  
pp. 173111 ◽  
Author(s):  
Ping Lu ◽  
Jie Xiong ◽  
Mark Van Benthem ◽  
Quanxi Jia
2021 ◽  
Vol 27 (S1) ◽  
pp. 2602-2603
Author(s):  
Katherine MacArthur ◽  
Andrew Yankovich ◽  
Armand Béché ◽  
Martina Luysberg ◽  
Hamish Brown ◽  
...  
Keyword(s):  

2014 ◽  
Vol 20 (6) ◽  
pp. 1782-1790 ◽  
Author(s):  
Ping Lu ◽  
Eric Romero ◽  
Shinbuhm Lee ◽  
Judith L. MacManus-Driscoll ◽  
Quanxi Jia

AbstractWe report our effort to quantify atomic-scale chemical maps obtained by collecting energy-dispersive X-ray spectra (EDS) using scanning transmission electron microscopy (STEM) (STEM-EDS). With thin specimen conditions and localized EDS scattering potential, the X-ray counts from atomic columns can be properly counted by fitting Gaussian peaks at the atomic columns, and can then be used for site-by-site chemical quantification. The effects of specimen thickness and X-ray energy on the Gaussian peak width are investigated using SrTiO3 (STO) as a model specimen. The relationship between the peak width and spatial resolution of an EDS map is also studied. Furthermore, the method developed by this work is applied to study cation occupancy in a Sm-doped STO thin film and antiphase boundaries (APBs) present within the STO film. We find that Sm atoms occupy both Sr and Ti sites but preferably the Sr sites, and Sm atoms are relatively depleted at the APBs likely owing to the effect of strain.


2021 ◽  
Vol 33 (1) ◽  
pp. 77-112
Author(s):  
Ruggero Vigliaturo ◽  
Sabrina M. Elkassas ◽  
Giancarlo Della Ventura ◽  
Günther J. Redhammer ◽  
Francisco Ruiz-Zepeda ◽  
...  

Abstract. In this paper, we present the results of a multi-analytical characterization of a glaucophane sample collected in the Piedmont region of northwestern Italy. Investigation methods included optical microscopy, powder X-ray diffraction, Fourier-transform infrared spectroscopy, µ-Raman spectroscopy, Mössbauer spectroscopy, electron probe microanalysis, environmental scanning electron microscopy and energy-dispersive X-ray spectroscopy, and scanning/transmission electron microscopy combined with energy-dispersive X-ray spectroscopy and electron energy-loss spectroscopy. In addition to the crystal–chemical characterization of the sample from the mesoscale to the near-atomic scale, we have also conducted an extended study on the morphology and dimensions of the mineral particles. The main finding is that studying the same particle population at different magnifications yields different results for mineral habit, dimensions, and dimensional distributions. As glaucophane may occur as an elongate mineral particle (e.g., asbestiform glaucophane occurrences in California and Nevada), the observed discrepancies therefore need to be considered when assessing potential breathability of such particles, with implications for future regulations on elongate mineral particles. While the sample preparation and particle counting methods are not directly investigated in this work, our findings suggest that different magnifications should be used when characterizing an elongate mineral particle population, irrespective of whether or not it contains asbestiform material. These results further reveal the need for developing improved regulation for elongate mineral particles. We thus propose a simple methodology to merge the datasets collected at different magnifications to provide a more complete description and a better risk evaluation of the studied particle population.


Microscopy ◽  
2020 ◽  
Vol 69 (1) ◽  
pp. 26-30
Author(s):  
Shin Inamoto ◽  
Yuji Otsuka

Abstract The properties of core-shell nanoparticles, which are used for many catalytic processes as an alternative to platinum, depend on the size of both the particle and the shell. It is thus necessary to develop a quantitative method to determine the shell thickness. Pd–Pt core-shell particles were analyzed using scanning transmission electron microscopy (STEM) and energy-dispersive X-ray spectroscopy (EDX). Quantitative EDX line profiles acquired from the core-shell particle were compared to four core-shell models. The results indicate that the thickness of the Pt shell corresponds to two atomic layers. Meanwhile, high-angle annular dark-field STEM images from the same particle were analyzed and compared to simulated images. Again, this experiment demonstrates that the shell thickness was of two atomic layers. Our results indicate that, in small particles, it is possible to use EDX for a precise atomic-scale quantitative analysis.


2021 ◽  
pp. 1-15
Author(s):  
Katherine E. MacArthur ◽  
Andrew B. Yankovich ◽  
Armand Béché ◽  
Martina Luysberg ◽  
Hamish G. Brown ◽  
...  

Abstract


2015 ◽  
Vol 21 (S3) ◽  
pp. 819-820
Author(s):  
Zhen Chen ◽  
Scott D. Findlay ◽  
Matthew Weyland ◽  
Adrian J. D'Alfonso ◽  
Leslie J. Allen
Keyword(s):  

Nanomaterials ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 2117
Author(s):  
Thomas Walther

A procedure based on energy-dispersive X-ray spectroscopy in a scanning electron microscope (SEM-EDXS) is proposed to measure ultra-thin oxide layer thicknesses to atomic scale precision in top-down instead of cross-sectional geometry. The approach is based on modelling the variation of the electron beam penetration depth and hence the depth of X-ray generation in the sample as a function of the acceleration voltage. This has been tested for the simple case of silica on silicon (SiO2/Si) which can serve as a model system to study gate oxides in metal-on-semiconductor field-effect transistors (MOS-FETs). Two possible implementations exist both of which rely on pairs of measurements to be made: in method A, the wafer piece of interest and a reference sample (here: ultra-clean fused quartz glass for calibration of the effective k-factors of X-ray lines from elements O and Si) are analysed at the same acceleration voltage. In method B, two measurements of the apparent O/Si ratio of the same wafer sample need to be made at different acceleration voltages and from their comparison to simulations the SiO2 layer thickness of the sample can be inferred. The precision attainable is ultimately shown to be limited by surface contamination during the experiments, as very thin carbonaceous surface layers can alter the results at very low acceleration voltages, while the sensitivity to ultra-thin surface oxides is much reduced at higher acceleration voltages. The optimal operation voltage is estimated to lie in the range of 3–15 kV. Method A has been experimentally verified to work well for test structures of thin oxides on Si-Ge/Si.


2017 ◽  
Vol 23 (1) ◽  
pp. 145-154 ◽  
Author(s):  
Ping Lu ◽  
Renliang Yuan ◽  
Jian Min Zuo

AbstractElemental mapping at the atomic-scale by scanning transmission electron microscopy (STEM) using energy-dispersive X-ray spectroscopy (EDS) provides a powerful real-space approach to chemical characterization of crystal structures. However, applications of this powerful technique have been limited by inefficient X-ray emission and collection, which require long acquisition times. Recently, using a lattice-vector translation method, we have shown that rapid atomic-scale elemental mapping using STEM-EDS can be achieved. This method provides atomic-scale elemental maps averaged over crystal areas of ~few 10 nm2with the acquisition time of ~2 s or less. Here we report the details of this method, and, in particular, investigate the experimental conditions necessary for achieving it. It shows, that in addition to usual conditions required for atomic-scale imaging, a thin specimen is essential for the technique to be successful. Phenomenological modeling shows that the localization of X-ray signals to atomic columns is a key reason. The effect of specimen thickness on the signal delocalization is studied by multislice image simulations. The results show that the X-ray localization can be achieved by choosing a thin specimen, and the thickness of less than about 22 nm is preferred for SrTiO3in [001] projection for 200 keV electrons.


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