Single Atom Microscopy

2012 ◽  
Vol 18 (6) ◽  
pp. 1342-1354 ◽  
Author(s):  
Wu Zhou ◽  
Mark P. Oxley ◽  
Andrew R. Lupini ◽  
Ondrej L. Krivanek ◽  
Stephen J. Pennycook ◽  
...  

AbstractWe show that aberration-corrected scanning transmission electron microscopy operating at low accelerating voltages is able to analyze, simultaneously and with single atom resolution and sensitivity, the local atomic configuration, chemical identities, and optical response at point defect sites in monolayer graphene. Sequential fast-scan annular dark-field (ADF) imaging provides direct visualization of point defect diffusion within the graphene lattice, with all atoms clearly resolved and identified via quantitative image analysis. Summing multiple ADF frames of stationary defects produce images with minimized statistical noise and reduced distortions of atomic positions. Electron energy-loss spectrum imaging of single atoms allows the delocalization of inelastic scattering to be quantified, and full quantum mechanical calculations are able to describe the delocalization effect with good accuracy. These capabilities open new opportunities to probe the defect structure, defect dynamics, and local optical properties in 2D materials with single atom sensitivity.

Author(s):  
R. F. Loane

The multislice method has been adapted to simulate annular dark field (ADF) scanning transmission electron microscope (STEM) images. In the STEM image simulation, a highly focused electron probe is scanned across a specimen and the scattered intensity, accumulated over an annular detector, is recorded as a function of probe position. Each pixel in the STEM image is determined by an entire multislice calculation for a particular position of the incident probe. This N4 process is very computationally expensive and currently requires the use of a supercomputer to achieve runtimes of less than a day.The simulated specimen consisted of a (111) silicon crystal substrate, which was a multiple of 94 Å (30 slices) thick, followed by an additional slice containing a single gold atom. Slice potentials were 38.4 Å x 39.9 Å (256 x 256 pixels) in size, which set the maximum included scattering angle to 79 mrad.


Microscopy ◽  
2020 ◽  
Author(s):  
A Ishizuka ◽  
K Ishizuka ◽  
R Ishikawa ◽  
N Shibata ◽  
Y Ikuhara ◽  
...  

Abstract Although the possibility of locating single atom in three dimensions using the scanning transmission of electron microscope (STEM) has been discussed with the advent of aberration correction technology, it is still a big challenge. In this report we have developed deconvolution routines based on maximum entropy method (MEM) and Richardson-Lucy algorithm (RLA), which are applicable to the STEM annular dark-field (ADF) though-focus images to improve the depth resolution. The new 3D deconvolution routines require a limited defocus-range of STEM-ADF images that covers a whole sample and some vacuum regions. Since the STEM-ADF probe is infinitely elongated along the optical axis, a 3D convolution is performed with a 2D convolution over xy-plane using the 2D fast Fourier transform (FFT) in reciprocal space, and a 1D convolution along the z-direction in real space. Using our new deconvolution routines, we have processed simulated focal series of STEM-ADF images for single Ce dopants embedded in wurtzite-type AlN. Applying the MEM, the Ce peaks are clearly localized along the depth, and the peak width is reduced down to almost one half. We also applied the new deconvolution routines to experimental focal series of STEM-ADF images of a monolayer graphene. The RLA gives smooth and high-P/B ratio scattering distribution, and the graphene layer can be easily detected. Using our deconvolution algorithms, we can determine the depth locations of the heavy dopants and the graphene layer within the precision of 0.1 and 0.2 nm, respectively, Thus, the deconvolution must be extremely useful for the optical sectioning with 3D STEM-ADF images.


Author(s):  
Earl J. Kirkland ◽  
Robert J. Keyse

An ultra-high resolution pole piece with a coefficient of spherical aberration Cs=0.7mm. was previously designed for a Vacuum Generators HB-501A Scanning Transmission Electron Microscope (STEM). This lens was used to produce bright field (BF) and annular dark field (ADF) images of (111) silicon with a lattice spacing of 1.92 Å. In this microscope the specimen must be loaded into the lens through the top bore (or exit bore, electrons traveling from the bottom to the top). Thus the top bore must be rather large to accommodate the specimen holder. Unfortunately, a large bore is not ideal for producing low aberrations. The old lens was thus highly asymmetrical, with an upper bore of 8.0mm. Even with this large upper bore it has not been possible to produce a tilting stage, which hampers high resolution microscopy.


2009 ◽  
Vol 24 (8) ◽  
pp. 2596-2604 ◽  
Author(s):  
Sašo Šturm ◽  
Makoto Shiojiri ◽  
Miran Čeh

The microstructure in AO-excess SrTiO3 (A = Sr2+, Ca2+, Ba2+) ceramics is strongly affected by the formation of Ruddlesden-Popper fault–rich (RP fault) lamellae, which are coherently intergrown with the matrix of the perovskite grains. We studied the structure and chemistry of RP faults by applying quantitative high-resolution transmission electron microscopy and high-angle annular dark-field scanning transmission electron microscopy analyses. We showed that the Sr2+ and Ca2+ dopant ions form RP faults during the initial stage of sintering. The final microstructure showed preferentially grown RP fault lamellae embedded in the central part of the anisotropic perovskite grains. In contrast, the dopant Ba2+ ions preferably substituted for Sr2+ in the SrTiO3 matrix by forming a BaxSr1−xTiO3 solid solution. The surplus of Sr2+ ions was compensated structurally in the later stages of sintering by the formation of SrO-rich RP faults. The resulting microstructure showed RP fault lamellae located at the surface of equiaxed BaxSr1-xTiO3 perovskite grains.


2018 ◽  
Vol 2018 ◽  
pp. 1-12
Author(s):  
N. Baladés ◽  
D. L. Sales ◽  
M. Herrera ◽  
A. M. Raya ◽  
J. C. Hernández-Garrido ◽  
...  

This paper explores the capability of scanning transmission electron microscopy (STEM) techniques in determining the dispersion degree of graphene layers within the carbon matrix by using simulated high-angle annular dark-field (HAADF) images. Results ensure that unmarked graphene layers are only detectable if their orientation is parallel to the microscope beam. Additionally, gold-marked graphene layers allow evaluating the dispersion degree in structural composites. Moreover, electron tomography has been demonstrated to provide truthfully 3D distribution of the graphene sheets inside the matrix when an appropriate reconstruction algorithm and 2D projections including channelling effect are used.


Materials ◽  
2021 ◽  
Vol 14 (16) ◽  
pp. 4531
Author(s):  
Maria Meledina ◽  
Geert Watson ◽  
Alexander Meledin ◽  
Pascal Van Der Voort ◽  
Joachim Mayer ◽  
...  

Ru catalyst nanoparticles were encapsulated into the pores of a Cr-based metal-organic framework (MOF)—MIL-101. The obtained material, as well as the non-loaded MIL-101, were investigated down to the atomic scale by annular dark-field scanning transmission electron microscopy using low dose conditions and fast image acquisition. The results directly show that the used wet chemistry loading approach is well-fitted for the accurate embedding of the individual catalyst nanoparticles into the cages of the MIL-101. The MIL-101 host material remains crystalline after the loading procedure, and the encapsulated Ru nanoparticles have a metallic nature. Annular dark field scanning transmission electron microscopy, combined with EDX mapping, is a perfect tool to directly characterize both the embedded nanoparticles and the loaded nanoscale MOFs. The resulting nanostructure of the material is promising because the Ru nanoparticles hosted in the MIL-101 pores are prevented from agglomeration—the stability and lifetime of the catalyst could be improved.


2019 ◽  
Vol 10 ◽  
pp. 1754-1767
Author(s):  
Ilka Simon ◽  
Julius Hornung ◽  
Juri Barthel ◽  
Jörg Thomas ◽  
Maik Finze ◽  
...  

NiGa is a catalyst for the semihydrogenation of alkynes. Here we show the influence of different dispersion times before microwave-induced decomposition of the precursors on the phase purity, as well as the influence of the time of microwave-induced decomposition on the crystallinity of the NiGa nanoparticles. Microwave-induced co-decomposition of all-hydrocarbon precursors [Ni(COD)2] (COD = 1,5-cyclooctadiene) and GaCp* (Cp* = pentamethylcyclopentadienyl) in the ionic liquid [BMIm][NTf2] selectively yields small intermetallic Ni/Ga nanocrystals of 5 ± 1 nm as derived from transmission electron microscopy (TEM) and high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) and supported by energy-dispersive X-ray spectrometry (EDX), selected-area energy diffraction (SAED) and X-ray photoelectron spectroscopy (XPS). NiGa@[BMIm][NTf2] catalyze the semihydrogenation of 4-octyne to 4-octene with 100% selectivity towards (E)-4-octene over five runs, but with poor conversion values. IL-free, precipitated NiGa nanoparticles achieve conversion values of over 90% and selectivity of 100% towards alkene over three runs.


1999 ◽  
Vol 589 ◽  
Author(s):  
Y Kotaka ◽  
T. Yamazaki ◽  
Y Kikuchi ◽  
K. Watanabe

AbstractThe high-angle annular dark-field (HAADF) technique in a dedicated scanning transmission electron microscope (STEM) provides strong compositional sensitivity dependent on atomic number (Z-contrast image). Furthermore, a high spatial resolution image is comparable to that of conventional coherent imaging (HRTEM). However, it is difficult to obtain a clear atomic structure HAADF image using a hybrid TEM/STEM. In this work, HAADF images were obtained with a JEOL JEM-2010F (with a thermal-Schottky field-emission) gun in probe-forming mode at 200 kV. We performed experiments using Si and GaAs in the [110] orientation. The electron-optical conditions were optimized. As a result, the dumbbell structure was observed in an image of [110] Si. Intensity profiles for GaAs along [001] showed differences for the two atomic sites. The experimental images were analyzed and compared with the calculated atomic positions and intensities obtained from Bethe's eigen-value method, which was modified to simulate HAADF-STEM based on Allen and Rossouw's method for convergent-beam electron diffraction (CBED). The experimental results showed a good agreement with the simulation results.


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