Mass Accuracy in the STEM

Author(s):  
J. S. Wall

The scanning transmission electron microscope (STEM) has a number of features which make it ideal for quantitative studies: 1) large acceptance angle scintillator-photomultiplier detectors for low dose dark field imaging with linear electron detection, 2) simple contrast transfer function with no oscillations, 3) cold stage for zero contamination and reduced mass loss, 4) digital scanning for accurate magnification and positioning and 5) serial readout of several signals simultaneously for direct interfacing to a computer.For the past 10 years the Brookhaven STEM has been used for mass measurements on isolated individual molecules in freeze dried biological specimens. Interpretation of dark field STEM images is straightforward because of the clean background and linearity of the entire imaging process. Mass measurements provide a quantitative link to biochemical studies. Tobacco mosaic virus (TMV) usually is included along with the specimen of interest as a measure of the quality of the freeze drying and as a check on the microscope calibration, but is not necessary for absolute mass measurements.

1999 ◽  
Vol 5 (S2) ◽  
pp. 670-671 ◽  
Author(s):  
O.L. Krivanek ◽  
N. Dellby ◽  
A.R. Lupini

Even though two generations of electron microscopists have come to accept that the resolution of their instruments is limited by spherical aberration, three different aberration correctors showing that the aberration can be overcome have recently been built [1-3]. One of these correctors was developed by us specifically for forming small electron probes in a dedicated scanning transmission electron microscope (STEM) [3, 4]. It promises to revolutionize the way STEM instruments are built and the types of problems that they are applied to.As was the case with the Berlin Wall, when a barrier that was once thought immovable finally crumbles, many of the consequences can be quite unexpected. For STEM, the removal of spherical aberration (Cs) as the main resolution limit is likely to lead to a new paradigm in which:1) The resolution at a given operating voltage will improve by about 3x relative to today's best. When Cs can be adjusted arbitrarily in a STEM being used for microanalysis or dark field imaging, defocus and Cs are set to values that optimally oppose the effect of the 5th-order spherical aberration C5.


2021 ◽  
Vol 106 (1) ◽  
pp. 82-96 ◽  
Author(s):  
Lei Jin ◽  
Dimitrios Koulialias ◽  
Michael Schnedler ◽  
Andreas U. Gehring ◽  
Mihály Pósfai ◽  
...  

Abstract Pyrrhotites, characterized by the chemical formula Fe1–δS (0 < δ ≤ 1/8), represent an extended group of minerals that are derived from the NiAs-type FeS aristotype. They contain layered arrangements of ordered Fe vacancies, which are at the origin of the various magnetic signals registered from certain natural rocks and can act as efficient electrocatalysts in oxygen evolution reactions in ultrathin form. Despite extensive studies over the past century, the local structural details of pyrrhotite superstructures formed by different arrangements of Fe vacancies remain unclear, in particular at the atomic scale. Here, atomic-resolution high-angle annular dark-field imaging and nanobeam electron diffraction in the scanning transmission electron microscope are used to study natural pyrrhotite samples that contain commensurate 4C and incommensurate 4.91 ± 0.02C constituents. Local measurements of both the intensities and the picometer-scale shifts of individual Fe atomic columns are shown to be consistent with a model for the structure of 4C pyrrhotite, which was derived using X-ray diffraction by Tokonami et al. (1972). In 4.91 ± 0.02C pyrrhotite, 5C-like unequally sized nano-regions are found to join at anti-phase-like boundaries, leading to the incommensurability observed in the present pyrrhotite sample. This conclusion is supported by computer simulations. The local magnetic properties of each phase are inferred from the measurements. A discussion of perspectives for the quantitative counting of Fe vacancies at the atomic scale is presented.


Author(s):  
Adam Amali ◽  
Peter Rez

The highly coherent probe in the scanning transmission electron microscope(STEM) equipped with a with high angle annular dark field (HAADF) detector has become an important tool for high resolution work in the study of crystals.with potential for providing chemically sensitive information.The results of Pennycook and Boatner and the calculations of Kirkland et al clearly demonstrated that lattice resolution was possible using HAADF imaging.There has been other contributions since then.The theoretical interpretation of these images however remains controversial and other contributions have focussed on whether the imaging is coherent or incoherent.In the present work we analyse the various mechanisms that contribute to the large angle signal obtained in the HAADF detector.Bloch waves are used to describe the elastic dynamical scattering; and in the abscence of any strong Bragg reflections.the amplitude observed in the detector plane in the STEM may be represented by a simple convolution between the scattering function of the object and the probe.


2002 ◽  
Vol 8 (6) ◽  
pp. 475-486 ◽  
Author(s):  
Robert F. Klie ◽  
Nigel D. Browning

This article presents a comprehensive investigation of (La, Sr)FeO3 by correlated atomic resolution annular dark field imaging and electron energy loss spectroscopy. Here, the ability of these techniques to characterize point defect formation and phase transitions under reducing conditions in situ in the scanning transmission electron microscope is evaluated and the influence of oxygen vacancies on the structure–property relationships is discussed. In particular, the evolution of the Ruddlesden–Popper, Brownmillerite, and Aurivillius phases can be associated directly with the ionic and electronic conductivity of the bulk material under different thermodynamic conditions. These results lead naturally to an atomistic defect chemistry model to explain the high temperature ionic and electronic conductivity in this and other perovskite materials.


Author(s):  
Max T. Otten ◽  
Marc J.C de Jong

With the rapid advances in new materials and production techniques in fields such as ceramics, semiconductors, metals, polymers and composites, the demands on analytical techniques for studying these materials are ever increasing. The TEM is ideally suited because of its spatial resolution and large number of different signals (bright-field and dark-field imaging, high-resolution imaging, convergent beam diffraction. X-ray and energy-loss analysis, scanning with bright-field, dark-field, backscattered and secondary electrons, etc). Many TEM’s suffer, however, from an unnecessary restrictiveness in the techniques provided, e.g. top-entry TEM’s without X-ray microanalysis or TEM systems without scanning. In order to provide the materials scientist with a powerful solution for current and future demands in materials research, the new Philips CM20 (Fig. 1) has been designed specifically to incorporate as many techniques as possible with the highest possible performance.In addition to its high electron-optical performance, the CM20’s MICROCONTROLLER, a microprocessor control system with ergonomic control-panel lay-out, ensures ease of use, greatly speeding up operation and enhancing the microscopist’s productivity.


Author(s):  
L. Gandolfi ◽  
J. Reiffel

Calculations have been performed on the contrast obtainable, using the Scanning Transmission Electron Microscope, in the observation of thick specimens. Recent research indicates a revival of an earlier interest in the observation of thin specimens with the view of comparing the attainable contrast using both types of specimens.Potential for biological applications of scanning transmission electron microscopy has led to a proliferation of the literature concerning specimen preparation methods and the controversy over “to stain or not to stain” in combination with the use of the dark field operating mode and the same choice of technique using bright field mode of operation has not yet been resolved.


Author(s):  
M. Boublik ◽  
G. Thornton ◽  
G. Oostergetel ◽  
J.F. Hainfeld ◽  
J.S. Wall

Understanding the structural complexity of ribosomes and their role in protein synthesis requires knowledge of the conformation of their components - rRNAs and proteins. Application of dedicated scanning transmission electron microscope (STEM), electrical discharge of the support carbon film in an atmosphere of pure nitrogen, and determination of the molecular weight of individual rRNAs enabled us to obtain high resolution electron microscopic images of unstained freeze-dried rRNA molecules from BHK cells in a form suitable for evaluation of their 3-D structure. Preliminary values for the molecular weight of 28S RNA from the large and 18S RNA from the small ribosomal subunits as obtained by mass measurement were 1.84 x 106 and 0.97 x 106, respectively. Conformation of rRNAs consists, in general, of alternating segments of intramolecular hairpin stems and single stranded loops in a proportion which depends on their ionic environment, the Mg++ concentration in particular. Molecules of 28S RNA (Fig. 1) and 18S RNA (not shown) obtained by freeze-drying from a solution of 60 mM NH+4 acetate and 2 mM Mg++ acetate, pH 7, appear as partially unfolded coils with compact cores suggesting a high degree of ordered secondary structure.


Sign in / Sign up

Export Citation Format

Share Document