scholarly journals Fast Atomic-Scale Elemental Mapping of Crystalline Materials by STEM Energy-Dispersive X-Ray Spectroscopy Achieved with Thin Specimens

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.

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

Abstract


Author(s):  
J. Bentley ◽  
E. A. Kenik

Instruments combining a 100 kV transmission electron microscope (TEM) with scanning transmission (STEM), secondary electron (SEM) and x-ray energy dispersive spectrometer (EDS) attachments to give analytical capabilities are becoming increasingly available and useful. Some typical applications in the field of materials science which make use of the small probe size and thin specimen geometry are the chemical analysis of small precipitates contained within a thin foil and the measurement of chemical concentration profiles near microstructural features such as grain boundaries, point defect clusters, dislocations, or precipitates. Quantitative x-ray analysis of bulk samples using EDS on a conventional SEM is reasonably well established, but much less work has been performed on thin metal foils using the higher accelerating voltages available in TEM based instruments.


2021 ◽  
Vol 27 (S1) ◽  
pp. 2602-2603
Author(s):  
Katherine MacArthur ◽  
Andrew Yankovich ◽  
Armand Béché ◽  
Martina Luysberg ◽  
Hamish Brown ◽  
...  
Keyword(s):  

2014 ◽  
Vol 20 (5) ◽  
pp. 1565-1575 ◽  
Author(s):  
Abdelhalim Zoukel ◽  
Lahcen Khouchaf ◽  
Jean Di Martino ◽  
David Ruch

AbstractA procedure has been developed to follow degradation of energy-dispersive spectroscopy (EDS) X-ray lateral resolution in a variable pressure scanning electron microscope. This procedure is based on evaluation of the EDS profile shape change for different experimental conditions. Some parameters affecting the X-ray resolution in high-vacuum mode have been taken into account. Good agreement between the simulated and experimental EDS profiles shows the reliability of the proposed procedure. A significant improvement in measurement of the EDS profile interfacial distance (DINT) has been achieved.


2013 ◽  
Vol 102 (17) ◽  
pp. 173111 ◽  
Author(s):  
Ping Lu ◽  
Jie Xiong ◽  
Mark Van Benthem ◽  
Quanxi Jia

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.


2013 ◽  
Vol 19 (S5) ◽  
pp. 157-161 ◽  
Author(s):  
Kyeongsoon Han ◽  
Sangjin Lee ◽  
Hwasoo Lee

AbstractDisputes on the painting methods of Goguryeo murals can mainly be categorized into whether the murals adapted eastern secco or western fresco; however, the murals have their own unique methods as well. There are different viewpoints among experts on interpreting the painting methods. This study involved the creation of research samples to discover the painting methods under dispute and may help discover the methods based on scanning electron microscopy energy-dispersive X-ray spectroscopy (SEM-EDX) studies. Goguryeo murals introduced pseudo-fresco rather than buon fresco methods. Unlike fresco techniques in the West, Goguryeo painters mixed traditional soft binders and adapted typical secco painting techniques for paintings, borders, and corrections after drying. The disputed issues may be resolved by these techniques, and samples may be produced based on the analyzed data. Therefore, many questions can finally be answered through SEM-EDX elemental mapping.


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