Factors Affecting Spatial Resolution for Compositional Analysis in Stem

1984 ◽  
Vol 41 ◽  
Author(s):  
John B. Vander Sande ◽  
Anthony J. Garratt-Reed

AbstractThis paper discusses the application of the scanning transmission electron microscope (STEM) to the detection of segregation at interfaces via the monitoring of X-rays generated when the incident electrons interact with the segregant. Issues of spatial resolution and minimum detectable concentration are discussed. Specific examples, emphasizing the importance of probe size, sample thickness, and sample orientation, are presented.

Author(s):  
Ernest L. Hall ◽  
John B. Vander Sande

The scanning transmission electron microscope has afforded a dramatic improvement in the spatial resolution of X-ray microanalysis of thin specimens, allowing the investigation of extremely localized compositional variations in materials systems. In this paper, the results of high resolution composition profile analysis in several materials are presented. The materials were analyzed in a 100 kV field emission STEM manufactured by VG Microscopes, Ltd., and fitted with an energy dispersive X-ray spectrometer. The specimens were held in a double-tilt graphite cartridge which allowed X-ray detection in the tilt range 0°-20° about each axis. The vacuum in the specimen chamber was ∿ 2 x 10-9 torr during analysis. Electron probe spot sizes of 5-10 Å were used, corresponding to probe currents in the range of 10-10-10-9 amps.For a given specimen composition, the spatial resolution of X-ray microanalysis in thin specimens is a function of probe size, accelerating voltage, specimen atomic number, and thickness.


Author(s):  
John B. Vander Sande ◽  
Thomas F. Kelly ◽  
Douglas Imeson

In the scanning transmission electron microscope (STEM) a fine probe of electrons is scanned across the thin specimen, or the probe is stationarily placed on a volume of interest, and various products of the electron-specimen interaction are then collected and used for image formation or microanalysis. The microanalysis modes usually employed in STEM include, but are not restricted to, energy dispersive X-ray analysis, electron energy loss spectroscopy, and microdiffraction.


1997 ◽  
Vol 3 (S2) ◽  
pp. 1171-1172 ◽  
Author(s):  
Ondrej L. Krivanek ◽  
Niklas Dellby ◽  
Andrew J. Spence ◽  
Roger A. Camps ◽  
L. Michael Brown

Aberration correction in electron microscopy is a subject with a 60 year history dating back to the fundamental work of Scherzer. There have been several partial successes, such as Deltrap's spherical aberration (Cs) corrector which nulled Cs over 30 years ago. However, the practical goal of attaining better resolution than the best uncorrected microscope operating at the same voltage remains to be fulfilled. Combining well-known electron-optical principles with stable electronics, versatile computer control, and software able to diagnose and correct aberrations on-line is at last bringing this goal within reach.We are building a quadrupole-octupole Cs corrector with automated aberration diagnosis for a VG HB5 dedicated scanning transmission electron microscope (STEM). A STEM with no spherical aberration will produce a smaller probe size with a given beam current than an uncorrected STEM, and a larger beam current in a given size probe.


1989 ◽  
Vol 160 ◽  
Author(s):  
W. T. Pike

AbstractUsing the nanometer probe available in the dedicated scanning transmission electron microscope (STEM) local structural information can be obtained from individual layers in [100] grown Si-Si1-xGex multilayer structures. Furthermore the small probe size enables cleaved specimens with their very large wedge angles to be analyzed in cross-section. Diffraction patterns are shown from multilayers of varying periodicity. Analysis of the patterns concentrates on the higher order Laue zone (holz) reflections in the high angle excess ring . The behaviour of the excess holz reflections indicates the transition from a strained layer superiattice to a dislocated structure as the thickness of the layers increases for a given composition.


1981 ◽  
Vol 8 ◽  
Author(s):  
John B. Vander Sande

ABSTRACTThe techniques of scanning transmission electron microscopy and field iron microscopy/atom probe are briefly described. The advantages of these techniques for high spatial resolution compositional analysis are discussed and examples cited.


Science ◽  
2019 ◽  
Vol 363 (6426) ◽  
pp. 525-528 ◽  
Author(s):  
Jordan A. Hachtel ◽  
Jingsong Huang ◽  
Ilja Popovs ◽  
Santa Jansone-Popova ◽  
Jong K. Keum ◽  
...  

The identification of isotopic labels by conventional macroscopic techniques lacks spatial resolution and requires relatively large quantities of material for measurements. We recorded the vibrational spectra of an α amino acid, l-alanine, with damage-free “aloof” electron energy-loss spectroscopy in a scanning transmission electron microscope to directly resolve carbon-site–specific isotopic labels in real space with nanoscale spatial resolution. An isotopic red shift of 4.8 ± 0.4 milli–electron volts in C–O asymmetric stretching modes was observed for 13C-labeled l-alanine at the carboxylate carbon site, which was confirmed by macroscopic infrared spectroscopy and theoretical calculations. The accurate measurement of this shift opens the door to nondestructive, site-specific, spatially resolved identification of isotopically labeled molecules with the electron microscope.


Author(s):  
C. E. Lyman

Formation of 2-dimensional dot maps of x-ray intensity from various elements in a flat polished section was an early application of the scanning beam electron probe microanalyzer. The spatial resolution of those early maps was the same as the microprobe itself, about lpm. These maps were usually scanned in an analogue fashion, and there was generally enough x-ray signal to produce maps with good peak-to-background ratios. For analysis of individual catalyst particles, a scanning transmission electron microscope (STEM) must be used to obtain the required spatial resolution. However, the x-ray signal level is usually low and is collected with an energy-dispersive spectrometer which has a lower peak-to-background ratio than the wavelength-dispersive spectrometer used in the microprobe. To produce suitable high magnification x-ray maps of catalyst particles digital beam techniques were employed.


Author(s):  
A. N. Sreeram ◽  
L.-C. Qin ◽  
A. J. Garratt-Reed ◽  
L. W. Hobbs

There is significant current interest in understanding the structure of aperiodic solids, such as originally crystalline material amorphized by ion implantation, impact or application of massive pressures, or deposited amorphous thin films, which occupy small volumes. Radially-averaged real-space distribution functions can be derived from diffraction data, the best of which come from thermal neutron diffraction, which inconveniently requires large volumes. Neutron data are collectable in reciprocal space out to q ≡ 2sin(Θ/2)/λ = 70 nm-1, where Θ is the scattering angle and λ the wavelength, or about twice as far as for X-rays, which also require large diffracting volumes. Electron diffraction is the only recourse for very small volumes because of the much stronger interaction of the electron, but spectra must be energy filtered to remove the large inelastic scattering component. Recently, it has been shown that useful electron diffraction data can be collected conveniently to at least q = 16 nm-1 in the VG HB5 dedicated 100-kV field-emission STEM. This contribution details our experiences with improved collection in the VG HB603 instrument operating at 250 kV.


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