Chemical 3D tomography of 28nm high K metal gate transistor: STEM XEDS experimental method and results

Lepinay, K; Lorut, F.; Pantel, R.; Épicier, Thierry

doi:10.1016/j.micron.2013.01.004

Cited by 57 publications

(34 citation statements)

References 11 publications

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“…In this reaction, a solution of AuCl 4 -is added to Ag nanoparticle seeds. Au is reduced on the surface of the nanoparticles as Ag is oxidized, resulting in a bimetallic composition and hollowing of the initial seed.…”

Section: Representative Resultsmentioning

confidence: 99%

“…Specifically these traditional detector designs had relatively low collection efficiencies and measured no signal at a large range of tilt angles due shadowing from the sample holder 2,3 . The introduction of new geometrical designs of X-ray detectors within the (scanning) transmission electron microscope has made energy dispersive X-ray tomography a viable technique and has led to a number of recent studies [4][5][6] . HAADF STEM imaging is a widely used electron tomography imaging mode and is able to provide compositional information in specific situations based on the atomic number sensitivity of the HAADF signal intensity.…”

Section: Introductionmentioning

confidence: 99%

“…The disadvantage of EELS is that multiple scattering considerations impose stringent limits on the specimen thickness, and in several situations analysis is complicated by the presence of delayed onset edges or overlapping spectral features. Thus, EDX spectroscopy is often better suited to studying heavy elements such as those often associated with catalytic or plasmonic nanoparticle systems 9 The ideal sample geometry for EDX tomography consists of a needle shaped sample suspended in a vacuum and oriented along the tomographic tilt axis 4 . This situation ensures that there is no shadowing of the EDX detectors at any tilt angle by either the sample or the specimen holder.…”

Section: Introductionmentioning

confidence: 99%

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Energy Dispersive X-ray Tomography for 3D Elemental Mapping of Individual Nanoparticles

Slater

Lewis

Haigh

2016

JoVE

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Energy dispersive X-ray spectroscopy within the scanning transmission electron microscope (STEM) provides accurate elemental analysis with high spatial resolution, and is even capable of providing atomically resolved elemental maps. In this technique, a highly focused electron beam is incident upon a thin sample and the energy of emitted X-rays is measured in order to determine the atomic species of material within the beam path. This elementally sensitive spectroscopy technique can be extended to three dimensional tomographic imaging by acquiring multiple spectrum images with the sample tilted along an axis perpendicular to the electron beam direction.Elemental distributions within single nanoparticles are often important for determining their optical, catalytic and magnetic properties. Techniques such as X-ray tomography and slice and view energy dispersive X-ray mapping in the scanning electron microscope provide elementally sensitive three dimensional imaging but are typically limited to spatial resolutions of > 20 nm. Atom probe tomography provides near atomic resolution but preparing nanoparticle samples for atom probe analysis is often challenging. Thus, elementally sensitive techniques applied within the scanning transmission electron microscope are uniquely placed to study elemental distributions within nanoparticles of dimensions 10-100 nm.Here, energy dispersive X-ray (EDX) spectroscopy within the STEM is applied to investigate the distribution of elements in single AgAu nanoparticles. The surface segregation of both Ag and Au, at different nanoparticle compositions, has been observed.

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Section: Representative Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Energy Dispersive X-ray Tomography for 3D Elemental Mapping of Individual Nanoparticles

Slater

Lewis

Haigh

2016

JoVE

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show abstract

“…Extension of these methods to 3D spectroscopic imaging using TEM or STEM requires the sample to be beam-resistant (e.g. [9]) and/or a sacrifice of the image resolution by reducing the size of the spectrum-images. Using state-of-the art TEMs, voxel spectroscopy by simultaneous EELS and EDX tomography was demonstrated by Haberfehlner et al in [10], after generating 2,920 spectral volumes individually.…”

Section: Introductionmentioning

confidence: 99%

Reduced-dose and high-speed acquisition strategies for multi-dimensional electron microscopy

Saghi

Benning

Leary

et al. 2015

Adv Struct Chem Imag

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Multi-dimensional electron microscopy has recently gained considerable interest thanks to the advent of microscopes with unprecedented analytical and in situ capabilities. These information-rich imaging modes, though, are often subject to long acquisition times and large data generation. In this paper, we explore novel acquisition strategies and reconstruction algorithms to retrieve reliable reconstructions from datasets that are limited in terms of both per image and tilt series angular sampling. We show that inpainting techniques are capable of restoring scanning transmission electron microscopy images in which a very restricted number of pixels are scanned, while compressed sensing tomographic reconstruction is capable of minimising artefacts due to angular subsampling. An example of robust reconstruction from data constituting a dose reduction of 10× is presented, using an organic/inorganic core-shell nanowire as a test sample. The combination of these novel acquisition schemes and image recovery strategies provides new avenues to reduced-dose and high-speed imaging.

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“…EDX spectrum-imaging can yield 2D compositional maps in minutes and, by using prior information in the reconstruction process, high fidelity 3D tomograms may be possible with only 10 spectrum-images. From such rich 4D data sets, 3D compositional maps can be extracted [7] and more sophisticated PCA/ICA/NMF techniques used in a more routine fashion. A rather different 4D data set is available through time-resolved electron tomography.…”

mentioning

confidence: 99%

Electron Tomography of Nanoscale Materials - Opportunities and Challenges Ahead

Midgley¹

2013

Microsc Microanal

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Chemical 3D tomography of 28nm high K metal gate transistor: STEM XEDS experimental method and results

Cited by 57 publications

References 11 publications

Energy Dispersive X-ray Tomography for 3D Elemental Mapping of Individual Nanoparticles

Energy Dispersive X-ray Tomography for 3D Elemental Mapping of Individual Nanoparticles

Reduced-dose and high-speed acquisition strategies for multi-dimensional electron microscopy

Electron Tomography of Nanoscale Materials - Opportunities and Challenges Ahead

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