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Author |
MacArthur, K.E.; Yankovich, A.B.; Béché, A.; Luysberg, M.; Brown, H.G.; Findlay, S.D.; Heggen, M.; Allen, L.J. |
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Title |
Optimizing Experimental Conditions for Accurate Quantitative Energy-Dispersive X-ray Analysis of Interfaces at the Atomic Scale |
Type |
A1 Journal article |
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Year  |
2021 |
Publication |
Microscopy And Microanalysis |
Abbreviated Journal |
Microsc Microanal |
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Volume |
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Issue |
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Pages |
1-15 |
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Keywords |
A1 Journal article; Electron microscopy for materials research (EMAT) |
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Abstract |
The invention of silicon drift detectors has resulted in an unprecedented improvement in detection efficiency for energy-dispersive X-ray (EDX) spectroscopy in the scanning transmission electron microscope. The result is numerous beautiful atomic-scale maps, which provide insights into the internal structure of a variety of materials. However, the task still remains to understand exactly where the X-ray signal comes from and how accurately it can be quantified. Unfortunately, when crystals are aligned with a low-order zone axis parallel to the incident beam direction, as is necessary for atomic-resolution imaging, the electron beam channels. When the beam becomes localized in this way, the relationship between the concentration of a particular element and its spectroscopic X-ray signal is generally nonlinear. Here, we discuss the combined effect of both spatial integration and sample tilt for ameliorating the effects of channeling and improving the accuracy of EDX quantification. Both simulations and experimental results will be presented for a perovskite-based oxide interface. We examine how the scattering and spreading of the electron beam can lead to erroneous interpretation of interface compositions, and what approaches can be made to improve our understanding of the underlying atomic structure. |
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Wos |
000664532400007 |
Publication Date |
2021-04-12 |
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Series Issue |
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Edition |
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ISSN |
1431-9276 |
ISBN |
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Additional Links |
UA library record; WoS full record; WoS citing articles |
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Impact Factor |
1.891 |
Times cited |
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Open Access |
OpenAccess |
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Notes |
The authors would like to thank Jürgen Schubert for helping to supply the sample and valuable discussions on the topic. K. E. MacArthur and M. Heggen acknowledge the Helmholtz Funding agency and the DFG (grant number HE 7192/1-2) for their financial support of this work. L. J. Allen acknowledges the support of the Alexander von Humboldt Foundation. This research was supported under the Discovery Projects funding scheme of the Australian Research Council (Projects DP140102538 and FT190100619). K.E. MacArthur, A.B. Yankovich and A. Béché acknowledge support from the European Union’s Horizon 2020 research innovation program under grant agreement No. 823717 – ESTEEM3. A.B. Yankovich also acknowledges support from the Materials Science Area of Advance at Chalmers and the Swedish Research Council (VR, under grant No: 2020-04986).; esteem3TA; esteem3reported |
Approved |
Most recent IF: 1.891 |
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Call Number |
EMAT @ emat @c:irua:178129 |
Serial |
6760 |
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Author |
De Backer, A.; De Wael, A.; Gonnissen, J.; Martinez, G.T.; Béché, A.; MacArthur, K.E.; Jones, L.; Nellist, P.D.; Van Aert, S. |
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Title |
Quantitative annular dark field scanning transmission electron microscopy for nanoparticle atom-counting: What are the limits? |
Type |
P1 Proceeding |
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Year |
2015 |
Publication |
Journal of physics : conference series |
Abbreviated Journal |
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Volume |
644 |
Issue |
644 |
Pages |
012034 |
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Keywords |
P1 Proceeding; Electron microscopy for materials research (EMAT) |
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Abstract |
Quantitative atomic resolution annular dark field scanning transmission electron microscopy (ADF STEM) has become a powerful technique for nanoparticle atom-counting. However, a lot of nanoparticles provide a severe characterisation challenge because of their limited size and beam sensitivity. Therefore, quantitative ADF STEM may greatly benefit from statistical detection theory in order to optimise the instrumental microscope settings such that the incoming electron dose can be kept as low as possible whilst still retaining single-atom precision. The principles of detection theory are used to quantify the probability of error for atom-counting. This enables us to decide between different image performance measures and to optimise the experimental detector settings for atom-counting in ADF STEM in an objective manner. To demonstrate this, ADF STEM imaging of an industrial catalyst has been conducted using the near-optimal detector settings. For this experiment, we discussed the limits for atom-counting diagnosed by combining a thorough statistical method and detailed image simulations. |
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Wos |
000366826200034 |
Publication Date |
2015-10-13 |
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Abbreviated Series Title |
Electron Microscopy and Analysis Group Conference (EMAG), JUN 02-JUL 02, 2015, Manchester, ENGLAND |
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Series Volume |
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Series Issue |
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Edition |
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ISSN |
1742-6588 |
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Additional Links |
UA library record; WoS full record |
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Notes |
The authors acknowledge financial support from the Research Foundation Flanders (FWO, Belgium) through project funding (G.0368.15N, G.0369.15N, and G.0374.15N) and a PhD research grant to A De Backer. The research leading to these results has received funding from the European Union Seventh Framework Programme under Grant Agreement 312483 – ESTEEM2 (Integrated Infrastructure Initiative-I3), ERC Starting Grant 278510 Vortex, and the UK Engineering and Physical Sciences Research Council (EP/K032518/1). The authors acknowledge Johnson-Matthey for providing the sample and PhD funding to K E MacArthur. A Rosenauer is acknowledged for providing the STEMsim program.; esteem2jra2; ECASJO; |
Approved |
Most recent IF: NA |
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Call Number |
c:irua:130314 c:irua:130314 |
Serial |
4050 |
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Author |
de Backer, A.; Martinez, G.T.; MacArthur, K.E.; Jones, L.; Béché, A.; Nellist, P.D.; Van Aert, S. |
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Title |
Dose limited reliability of quantitative annular dark field scanning transmission electron microscopy for nano-particle atom-counting |
Type |
A1 Journal article |
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Year |
2015 |
Publication |
Ultramicroscopy |
Abbreviated Journal |
Ultramicroscopy |
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Volume |
151 |
Issue |
151 |
Pages |
56-61 |
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Keywords |
A1 Journal article; Electron microscopy for materials research (EMAT) |
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Abstract |
Quantitative annular dark field scanning transmission electron microscopy (ADF STEM) has become a powerful technique to characterise nano-particles on an atomic scale. Because of their limited size and beam sensitivity, the atomic structure of such particles may become extremely challenging to determine. Therefore keeping the incoming electron dose to a minimum is important. However, this may reduce the reliability of quantitative ADF STEM which will here be demonstrated for nano-particle atom-counting. Based on experimental ADF STEM images of a real industrial catalyst, we discuss the limits for counting the number of atoms in a projected atomic column with single atom sensitivity. We diagnose these limits by combining a thorough statistical method and detailed image simulations. |
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Place of Publication |
Amsterdam |
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Wos |
000351237800008 |
Publication Date |
2014-12-03 |
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ISSN |
0304-3991; |
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Additional Links |
UA library record; WoS full record; WoS citing articles |
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Impact Factor |
2.843 |
Times cited |
29 |
Open Access |
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Notes |
312483 Esteem2; 278510 Vortex; Fwo G039311; G006410; G037413; esteem2ta; ECASJO; |
Approved |
Most recent IF: 2.843; 2015 IF: 2.436 |
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Call Number |
c:irua:123927 c:irua:123927 |
Serial |
753 |
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Author |
de Backer, A.; De wael, A.; Gonnissen, J.; Martinez, G.T.; Béché, A.; MacArthur, K.E.; Jones, L.; Nellist, P.D.; Van Aert, S. |
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Title |
Quantitative annular dark field scanning transmission electron microscopy for nanoparticle atom-counting : what are the limits? |
Type |
A1 Journal article |
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Year |
2015 |
Publication |
Journal of physics : conference series |
Abbreviated Journal |
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Volume |
644 |
Issue |
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Pages |
012034-4 |
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Keywords |
A1 Journal article; Electron microscopy for materials research (EMAT) |
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Abstract |
Quantitative atomic resolution annular dark field scanning transmission electron microscopy (ADF STEM) has become a powerful technique for nanoparticle atom-counting. However, a lot of nanoparticles provide a severe characterisation challenge because of their limited size and beam sensitivity. Therefore, quantitative ADF STEM may greatly benefit from statistical detection theory in order to optimise the instrumental microscope settings such that the incoming electron dose can be kept as low as possible whilst still retaining single-atom precision. The principles of detection theory are used to quantify the probability of error for atom-counting. This enables us to decide between different image performance measures and to optimise the experimental detector settings for atom-counting in ADF STEM in an objective manner. To demonstrate this, ADF STEM imaging of an industrial catalyst has been conducted using the near-optimal detector settings. For this experiment, we discussed the limits for atomcounting diagnosed by combining a thorough statistical method and detailed image simulations. |
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Corporate Author |
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Publisher |
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Place of Publication |
Bristol |
Editor |
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Wos |
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ISSN |
1742-6588; 1742-6596 |
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Additional Links |
UA library record |
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Impact Factor |
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Times cited |
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Open Access |
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Notes |
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Approved |
Most recent IF: NA |
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Call Number |
UA @ lucian @ c:irua:129198 |
Serial |
4506 |
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