Diffraction Imaging in a He+ Ion Beam Scanning Transmission Microscope

2010 ◽  
Vol 16 (5) ◽  
pp. 599-603 ◽  
Author(s):  
John Notte IV ◽  
Raymond Hill ◽  
Sean M. McVey ◽  
Ranjan Ramachandra ◽  
Brendan Griffin ◽  
...  

AbstractThe scanning helium ion microscope has been used in transmission mode to investigate both the feasibility of this approach and the utility of the signal content and the image information available. Operating at 40 keV the penetration of the ion beam, and the imaging resolution achieved, in MgO crystals was found to be in good agreement with values predicted by Monte Carlo modeling. The bright-field and annular dark-field signals displayed the anticipated contrasts associated with beam absorption and scattering. In addition, the diffraction of the He ion beam within the sample gave rise to crystallographic contrast effects in the form of thickness fringes and dislocation images. Scanning transmission He ion microscopy thus achieves useful sample penetration and provides nanometer scale resolution, high contrast images of crystalline materials and crystal defects even at modest beam energies.

Author(s):  
J. Liu ◽  
J. M. Cowley

High-angle annular dark-field (HAADF) scanning transmission electron microscopy (STEM) has been recently the subject of active research because of its successful applications to the characterization of supported catalysts, interface problems in MBE grown semiconductors, superconductors and X-ray multilayers. The characteristics of HAADF images are different from those of the TEM images. For perfect single crystals the HAADF signal is mainly generated from thermal diffuse scattering. HAADF technique has also been used to study dopant contrast effects in semiconductors and dislocations have also been observed with an ADF detector. In this paper we report a study of dislocation contrasts and their dependence on the inner collection angle of the ADF detector.The STEM instrument used for the observations was the HB5 from VG Microscopes, Ld., modified by the addition of an ultra-high resolution pole piece (Cs = 0.8 mm) and a two-dimensional detector system. Post specimen lenses and various beam stops were used to change the inner (α) and outer (β) collection angles of the ADF detector.


Author(s):  
Kannan M. Krishnan

Transmission electron microscopy provides information on all aspects of the microstructure — structural, atomic, chemical, electronic, magnetic, etc. — at the highest spatial resolution in physical and biological materials, with applications ranging from fundamental studies to process metrology in the semiconductor industry. Developments in correcting electron-optical aberrations have improved TEM resolution to sub-Å levels. Coherent Bragg scattering (diffraction), incoherent Rutherford scattering (atomic mass), and interference (phase) are some contrast mechanisms in TEM. For phase contrast, optimum imaging is observed at the Scherzer defocus. Magnetic domains are imaged in Fresnel, Foucault, or differential phase contrast (DPC) modes. Off-axis electron holography measures phase shifts of the electron wave, and is affected by magnetic and electrostatic fields of the specimen. In scanning-transmission (STEM) mode, a focused electron beam is scanned across the specimen to sequentially form an image; a high-angle annular dark field detector gives Z-contrast images with elemental specificity and atomic resolution. Series of (S)TEM images, recorded every one or two degrees about a tilt axis, over as large a tilt-range as possible, are back-projected to reconstruct a 3D tomographic image. Inelastically scattered electrons, collected in the forward direction, form the energy-loss spectrum (EELS), and reveal the unoccupied local density of states, partitioned by site symmetry, nature of the chemical species, and the angular momentum of the final state. Energy-lost electrons are imaged by recording them, pixel-by-pixel, as a sequence of spectra (spectrum imaging), or by choosing electrons that have lost a specific energy (energy-filtered TEM). De-excitation processes (characteristic X-ray emission) are detected by energy dispersive methods, providing compositional microanalysis, including chemical maps. Overall, specimen preparation methods, even with many recent developments, including focused ion beam milling, truly limit applications of TEM.


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.


Author(s):  
Z. L. Wang ◽  
J. Bentley

The success of obtaining atomic-number-sensitive (Z-contrast) images in scanning transmission electron microscopy (STEM) has shown the feasibility of imaging composition changes at the atomic level. This type of image is formed by collecting the electrons scattered through large angles when a small probe scans across the specimen. The image contrast is determined by two scattering processes. One is the high angle elastic scattering from the nuclear sites,where ϕNe is the electron probe function centered at bp = (Xp, yp) after penetrating through the crystal; F denotes a Fourier transform operation; D is the detection function of the annular-dark-field (ADF) detector in reciprocal space u. The other process is thermal diffuse scattering (TDS), which is more important than the elastic contribution for specimens thicker than about 10 nm, and thus dominates the Z-contrast image. The TDS is an average “elastic” scattering of the electrons from crystal lattices of different thermal vibrational configurations,


Author(s):  
R.D. Leapman ◽  
S.Q. Sun ◽  
S-L. Shi ◽  
R.A. Buchanan ◽  
S.B. Andrews

Recent advances in rapid-freezing and cryosectioning techniques coupled with use of the quantitative signals available in the scanning transmission electron microscope (STEM) can provide us with new methods for determining the water distributions of subcellular compartments. The water content is an important physiological quantity that reflects how fluid and electrolytes are regulated in the cell; it is also required to convert dry weight concentrations of ions obtained from x-ray microanalysis into the more relevant molar ionic concentrations. Here we compare the information about water concentrations from both elastic (annular dark-field) and inelastic (electron energy loss) scattering measurements.In order to utilize the elastic signal it is first necessary to increase contrast by removing the water from the cryosection. After dehydration the tissue can be digitally imaged under low-dose conditions, in the same way that STEM mass mapping of macromolecules is performed. The resulting pixel intensities are then converted into dry mass fractions by using an internal standard, e.g., the mean intensity of the whole image may be taken as representative of the bulk water content of the tissue.


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.


2018 ◽  
Vol 273 ◽  
pp. 95-100
Author(s):  
Wen Hui Yang ◽  
Tomokazu Yamamoto ◽  
Kazuhiro Nogita ◽  
Syo Matsumura

Cu6Sn5 is an important intermetallic compound in soldering and electronic packaging. It is formed at the interface between molten solder and substrate during the soldering process, and the evolution of microstructure and properties also occurs in service. Previous studies revealed that Au and Ni are stabilization alloying elements for hexagonal η-Cu6Sn5 intermetallic. For better understanding of stabilization mechanisms at atomic resolution level, in this work, we made an attempt atomic structure analysis on a stoichiometric (Cu, Au, Ni)6Sn5 intermetallic prepared by direct alloying. High-angle annular dark-field (HAADF) imaging and atomic-resolution chemical mapping were taken by the aberration-corrected (Cs-corrected) scanning transmission electron microscopy (STEM). It is found that Au and Ni doped Cu6Sn5 has hexagonal structure. The atom sites of Cu1 and Sn can be distinguished in atomic-resolution images after being observed from orientation [2110], which is also confirmed by atomic-resolution chemical mapping analysis. Importantly, atomic-resolution about distribution of alloying Au atom was directly observed, and Au atoms occupy the Cu1 sites in η-Cu6Sn5.


2020 ◽  
Vol 11 ◽  
pp. 1854-1864
Author(s):  
Eduardo Serralta ◽  
Nico Klingner ◽  
Olivier De Castro ◽  
Michael Mousley ◽  
Santhana Eswara ◽  
...  

A detection system based on a microchannel plate with a delay line readout structure has been developed to perform scanning transmission ion microscopy (STIM) in the helium ion microscope (HIM). This system is an improvement over other existing approaches since it combines the information of the scanning beam position on the sample with the position (scattering angle) and time of the transmission events. Various imaging modes, such as bright field and dark field or the direct image of the transmitted signal, can be created by post-processing the collected STIM data. Furthermore, the detector has high spatial and temporal resolution, is sensitive to both ions and neutral particles over a wide energy range, and shows robustness against ion beam-induced damage. A special in-vacuum movable support gives the possibility of moving the detector vertically, placing the detector closer to the sample for the detection of high-angle scattering events, or moving it down to increase the angular resolution and distance for time-of-flight measurements. With this new system, we show composition-dependent contrast for amorphous materials and the contrast difference between small-angle and high-angle scattering signals. We also detect channeling-related contrast on polycrystalline silicon, thallium chloride nanocrystals, and single-crystalline silicon by comparing the signal transmitted at different directions for the same data set.


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