STEM-EDX tomography of bimetallic nanoparticles: A methodological investigation

Thomas Slater; Arne Janssen; Pedro H C Camargo; Grace Burke; Nestor J. Zaluzec; Sarah Haigh

doi:10.1016/j.ultramic.2015.10.007

STEM-EDX tomography of bimetallic nanoparticles: A methodological investigation

Thomas Slater, Arne Janssen, Pedro H C Camargo, Grace Burke, Nestor J. Zaluzec, Sarah Haigh^*

^*Corresponding author for this work

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Abstract

This paper presents an investigation of the limitations and optimisation of energy dispersive X-ray (EDX) tomography within the scanning transmission electron microscope, focussing on application of the technique to characterising the 3D elemental distribution of bimetallic AgAu nanoparticles. The detector collection efficiency when using a standard tomography holder is characterised using a tomographic data set from a single nanoparticle and compared to a standard low background double tilt holder. Optical depth profiling is used to investigate the angles and origin of detector shadowing as a function of specimen field of view. A novel time-varied acquisition scheme is described to compensate for variations in the intensity of spectrum images at each sample tilt. Finally, the ability of EDX spectrum images to satisfy the projection requirement for nanoparticle samples is discussed, with consideration of the effect of absorption and shadowing variations.

Original language	English
Pages (from-to)	61-73
Number of pages	13
Journal	Ultramicroscopy
Volume	162
Early online date	22 Oct 2015
DOIs	https://doi.org/10.1016/j.ultramic.2015.10.007
Publication status	Published - 1 Mar 2016

Keywords

Bimetallic nanoparticles
Electron tomography
Energy dispersive X-ray spectroscopy

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POST-PEER-REVIEW-NON-PUBLISHERS.PDFAccepted author manuscript, 2.37 MBLicence: CC BY

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title = "STEM-EDX tomography of bimetallic nanoparticles: A methodological investigation",

abstract = "This paper presents an investigation of the limitations and optimisation of energy dispersive X-ray (EDX) tomography within the scanning transmission electron microscope, focussing on application of the technique to characterising the 3D elemental distribution of bimetallic AgAu nanoparticles. The detector collection efficiency when using a standard tomography holder is characterised using a tomographic data set from a single nanoparticle and compared to a standard low background double tilt holder. Optical depth profiling is used to investigate the angles and origin of detector shadowing as a function of specimen field of view. A novel time-varied acquisition scheme is described to compensate for variations in the intensity of spectrum images at each sample tilt. Finally, the ability of EDX spectrum images to satisfy the projection requirement for nanoparticle samples is discussed, with consideration of the effect of absorption and shadowing variations.",

keywords = "Bimetallic nanoparticles, Electron tomography, Energy dispersive X-ray spectroscopy",

author = "Thomas Slater and Arne Janssen and Camargo, {Pedro H C} and Grace Burke and Zaluzec, {Nestor J.} and Sarah Haigh",

note = "Raw data can be obtained by contacting the corresponding author or is downloadable from the University of Manchester's escholar database.",

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doi = "10.1016/j.ultramic.2015.10.007",

language = "English",

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pages = "61--73",

journal = "Ultramicroscopy",

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T2 - A methodological investigation

AU - Slater, Thomas

AU - Janssen, Arne

AU - Camargo, Pedro H C

AU - Burke, Grace

AU - Zaluzec, Nestor J.

AU - Haigh, Sarah

N1 - Raw data can be obtained by contacting the corresponding author or is downloadable from the University of Manchester's escholar database.

PY - 2016/3/1

Y1 - 2016/3/1

N2 - This paper presents an investigation of the limitations and optimisation of energy dispersive X-ray (EDX) tomography within the scanning transmission electron microscope, focussing on application of the technique to characterising the 3D elemental distribution of bimetallic AgAu nanoparticles. The detector collection efficiency when using a standard tomography holder is characterised using a tomographic data set from a single nanoparticle and compared to a standard low background double tilt holder. Optical depth profiling is used to investigate the angles and origin of detector shadowing as a function of specimen field of view. A novel time-varied acquisition scheme is described to compensate for variations in the intensity of spectrum images at each sample tilt. Finally, the ability of EDX spectrum images to satisfy the projection requirement for nanoparticle samples is discussed, with consideration of the effect of absorption and shadowing variations.

AB - This paper presents an investigation of the limitations and optimisation of energy dispersive X-ray (EDX) tomography within the scanning transmission electron microscope, focussing on application of the technique to characterising the 3D elemental distribution of bimetallic AgAu nanoparticles. The detector collection efficiency when using a standard tomography holder is characterised using a tomographic data set from a single nanoparticle and compared to a standard low background double tilt holder. Optical depth profiling is used to investigate the angles and origin of detector shadowing as a function of specimen field of view. A novel time-varied acquisition scheme is described to compensate for variations in the intensity of spectrum images at each sample tilt. Finally, the ability of EDX spectrum images to satisfy the projection requirement for nanoparticle samples is discussed, with consideration of the effect of absorption and shadowing variations.

KW - Bimetallic nanoparticles

KW - Electron tomography

KW - Energy dispersive X-ray spectroscopy

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DO - 10.1016/j.ultramic.2015.10.007

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VL - 162

SP - 61

EP - 73

JO - Ultramicroscopy

JF - Ultramicroscopy

ER -

STEM-EDX tomography of bimetallic nanoparticles: A methodological investigation

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STEM-EDX tomography of bimetallic nanoparticles: A methodological investigation

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XRADIA : High Resolution of 4D Imaging of Degradation and Self-repair Processes

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