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The microanalysis of nonconductive specimen in a scanning electron
microscope is limited by charging effects. Using a charge density model
for the electric field buildup in a nonconductive specimen irradiated
by electrons, a Monte Carlo simulation method has been applied to
alumina (Al2O3). The results show a change in the
depth distribution for characteristic and bremsstrahlung X-ray,
φ(ρz) curves, and ψ(ρz) curves
(with absorption) for both elements' Kα lines. The
influence of the electric field on the measured X-ray intensity is
shown. The dependency of this influence by the three parameters,
electron energy, X-ray energy, and charge density, is clarified.
Following is a list of microscopy-related meetings and courses. The
editors would greatly appreciate input to this list via the electronic
submission form found in the MSA World-Wide Web page at
http://www.msa.microscopy.com. We will gladly add hypertext
links to the notice on the web and insert a listing of the meeting in
the next issue of the Journal. Send comments and questions to JoAn
Hudson, hudson@uoneuro.uoregon.edu or Nestor Zaluzec,
zaluzec@aaem.amc.anl.gov.
This work describes the application and usefulness of the focused ion
beam (FIB) technique for the preparation of transmission electron
microscopy (TEM) samples from metal matrix composite materials. Results
on an Al/diamond composite, manufactured by the squeeze casting
infiltration process, were chosen for demonstration. It is almost
impossible to prepare TEM specimens of this material by any other
conventional method owing to the presence of highly inhomogeneous
phases and reinforcement diamond particles. The present article gives a
detailed account of the salient features of the FIB technique and its
operation. One of the big advantages is the possibility to prepare
site-specific TEM specimens with high spatial resolution. The artifacts
occurring during the specimen preparation, for example, Ga-ion
implantation, curtain effects, amorphous layers, bending of the
lamella, or different milling behaviors of the materials have been
discussed. Furthermore, TEM examination of the specimens prepared
revealed an ultrafine amorphous layer of graphite formed at the
interface between the Al and diamond particles that may affect the
interfacial properties of the composite materials. This may not have
been feasible without the successful application of the FIB technique
for production of good quality site-specific TEM specimens.
Nanostructure and Dynamics of Molecular Assemblies: Biomembranes, Proteins, Surfactants, Polymers and Liquid-Crystals
Specimen charging may be one of the most significant factors that
contribute to the high variability and generally low quality of images
in cryo-electron microscopy. Understanding the nature of specimen
charging can help in devising methods to reduce or even avoid its
effects and thus improve the rate of data collection as well as the
quality of the data. We describe a series of experiments that help to
characterize the charging phenomenon, which has been termed the
Berriman effect. The pattern of buildup and disappearance of the charge
pattern has led to several suggestions for how to alleviate the effect.
Experiments are described that demonstrate the feasibility of such
charge mitigation.
It is shown that room-temperature diffraction pattern spots and
diffuse scatter can appear to change their size and appearance relative
to reciprocal-space sublattice reflections when the scattering material
corresponds in structure to a critical phase. Under such a condition,
the material is considered to be continually on the verge of a phase
transition and the diffraction spot will have no definite width, its
apparent size in reciprocal space dependent on the strength of the
scattering into the diffracted beam. It is thought that the materials
described in the experiments—niobia-zirconia ceramic
alloys—are capable of entering such a critical phase because of
their recently suggested planar XY spin character. After first
describing how the seemingly crystalline ceramic alloy can display
XY-like behavior, we analyze the intensity dependence of the
critical scattering from the alloy's oxygen superlattice using
information-theoretic methods.
Extended abstract of a paper presented at the Pre-Meeting Congress: Materials Research in an Aberration-Free Environment, at Microscopy and Microanalysis 2004 in Savannah, Georgia, USA, July 31 and August 1, 2004.
Extended abstract of a paper presented at the Pre-Meeting Congress: Materials Research in an Aberration-Free Environment, at Microscopy and Microanalysis 2004 in Savannah, Georgia, USA, July 31 and August 1, 2004.
Although the most familiar consequences of specimen charging in
transmission electron microscopy can be eliminated by evaporating a
thin conducting film (such as a carbon film) onto an insulating
specimen or by preparing samples directly on such a conducting film to
begin with, a more subtle charging effect still remains. We argue here
that specimen charging is in this case likely to produce a dipole sheet
rather than a layer of positive charge at the surface of the specimen.
A simple model of the factors that control the kinetics of specimen
charging, and its neutralization, is discussed as a guide for
experiments that attempt to minimize the amount of specimen charging.
Believable estimates of the electrostatic forces and the electron
optical disturbances that are likely to occur suggest that specimen
bending and warping may have the biggest impact on degrading the image
quality at high resolution. Electron optical effects are likely to be
negligible except in the case of a specimen that is tilted to high
angle. A model is proposed to explain how both the mechanical and
electron-optical effects of forming a dipole layer would have much
greater impact on the image resolution in a direction perpendicular to
the tilt axis, a well-known effect in electron microscopy of
two-dimensional crystals.
The microstructure and magnetic domain structure of a Co-CoO
obliquely evaporated tape for magnetic recording are studied by
analytical electron microscopy and electron holography, respectively.
While the existence of Co and CoO crystallites is confirmed by
energy-filtered electron diffraction, columnar structure of the Co
crystallites surrounded by the densely packed CoO crystallites is
visualized by an elemental mapping method with electron energy loss
spectroscopy, and the crystal orientation relation among the Co
crystallites is clarified by high-resolution electron microscopy. It is
found that the neighboring Co crystallites have close crystal
orientations. On the other hand, electron holography reveals the
magnetic flux distribution in a thin section of the tape. Although
there exists the background resulting from the effect of inner
potential with thickness variation, the distribution of lines of
magnetic flux is found to correspond well to the recorded pattern.
The structure of Xe precipitates with sizes in several nanometers
embedded in Al is known to be stable and its structure is well
confirmed. But knowledge about the structure of Xe precipitates with
nanometer sizes is very limited. There are difficulties in observing
such small structures embedded in a crystalline matrix. An off-Bragg
condition is used to observe diffraction patterns, dark-field, and
high-resolution transmission electron microscopy images. The structure
of Xe precipitates with sizes of about 2 nm and smaller is observed and
confirmed. They are in an fcc structure and their orientation
relationship with the Al matrix is similar to that of larger
crystalline Xe precipitates or in an undefined structure. The lattice
spacing or atomic distance in such nanometer-sized Xe precipitates is
smaller than those of larger Xe precipitates embedded in Al matrix.
There is a trend that as the size becomes smaller, the precipitates are
more likely to have an undefined structure.
Extended abstract of a paper presented at the Pre-Meeting Congress: Materials Research in an Aberration-Free Environment, at Microscopy and Microanalysis 2004 in Savannah, Georgia, USA, July 31 and August 1, 2004.
Kelvin probe microscopy (KPM) is a specialized atomic force
microscopy technique in which long-range Coulomb forces between a
conductive atomic force probe and a specimen enable the electrical
potential at the surface of a specimen to be characterized with high
spatial resolution. KPM has been used to characterize nonconductive
materials following their exposure to stationary electron beam
irradiation in a scanning electron microscope (SEM). Charged beam
irradiation of poorly conducting materials results in the trapping of
charge at either preexisting or irradiation-induced defects. The
reproducible characteristic surface potentials associated with the
trapped charge have been mapped using KPM. Potential profiles are
calculated and compared with observed potential profiles giving insight
into the charging processes and residual trapped charge
distributions.