Electron spectroscopic imaging (ESI) on multiphase polymer materials

Author(s):  
H.-J. Cantow ◽  
M. Kunz ◽  
M. Möller

In transmission electron microscopy the natural contrast of polymers is very low. Thus the contrast has to be enhanced by staining with heavy metals. The resolution is limited by the size of the staining particles and by the fact that electrons with different energy are focused in different image planes due to the chromatic aberration of the magnetic lenses. The integration of an electron energy loss spectrometer into the optical coloumn of a transmission electron microscope offers the possibility to use monoenergetic electrons and to select electrons with a certain energy for imaging. Thus contrast and resolution are enhanced. By imaging only electrons with an element specific energy loss the element distribution in the sample can be obtained. In addition, elastic bright field images and diffraction patterns yield excellent resolution. Some applications of the method on multicomponent polymer materials are discussed.Bulk polymer samples were prepared by ultramicrotoming at room temperature or well below the glass transition temperature. Very thin films for the direct observation of the structure in semicrystalline polymers were obtained by melt-spinning. Specimens were examined with a ZEISS CEM 902 operated at 80 kV.

Author(s):  
William Krakow

An electronic device has been constructed which manipulates the primary beam in the conventional transmission microscope to illuminate a specimen under a variety of virtual condenser aperture conditions. The device uses the existing tilt coils of the microscope, and modulates the D.C. signals to both x and y tilt directions simultaneously with various waveforms to produce Lissajous figures in the back-focal plane of the objective lens. Electron diffraction patterns can be recorded which reflect the manner in which the direct beam is tilted during exposure of a micrograph. The device has been utilized mainly for the hollow cone imaging mode where the device provides a microscope transfer function without zeros in all spatial directions and has produced high resolution images which are also free from the effect of chromatic aberration. A standard second condenser aperture is employed and the width of the cone annulus is readily controlled by defocusing the second condenser lens.


Author(s):  
A. Bakenfelder ◽  
L. Reimer ◽  
R. Rennekamp

One advantage of energy-filtering electron microscopy (EFEM) is to avoid the chromatic aberration of conventional transmission electron microscopy (CTEM) by the mode of electron spectroscopic imaging (ESI) using either zero-loss filtering of unscattered and elastically scattered electrons or a narrow selected energy window at the most probable loss of the electron-energy-loss spectrum (EELS). Chromatic aberration can also be reduced by high-voltage electron microscopy (HVEM). Comparisons of ESI at 80 keV and CTEM at 200 keV have already been reported for biological tissues. In this contribution we compare the imaging of evaporated crystalline films with ESI at 80 keV in a ZEISS EM902 and with CTEM at 200 keV in a Hitachi H800/NA.Zero-loss filtering at 80 keV can be applied for maximum mass-thicknesses of x=ρt≃150 μg/cm2 where the zero-loss transmission falls below 0.001 and an energy window at the most-probable energy loss can be used below ≃300 μg/cm2. Inelastic scattering preserves the Bragg contrast.


Author(s):  
J. Mayer

With imaging energy filters becoming commercially available in transmission electron microscopy many of the limitations of conventional TEM instruments can be overcome. Energy filtered images of diffraction patterns can now be recorded without scanning using efficient parallel (2-dimensional detection. We have evaluated a prototype of the Zeiss EM 912 Omega, the first commercially available electron microscope with integrated imaging Omega energy filter. Combining the capabilities of the imaging spectrometer with the principal operation modes of a TEM gives access to many new qualitative and quantitative techniques in electron microscopy. The basis for all of them is that the filter selecte electrons within a certain energy loss range ΔE1 <ΔE < ΔE2 and images their contribution to an image (electron spectroscopic imaging, ESI) or a diffraction pattern (electron spectroscopic diffraction, ESD) In many applications the filter is only used to remove the inelastically scattered electrons (elastic or zero loss filtering). Furthermore, the electron energy loss spectrum can be magnified and recorded with serial or parallel detection.


1998 ◽  
Vol 13 (6) ◽  
pp. 1679-1687
Author(s):  
R. J. Gonzalez ◽  
A. L. Ritter

Small titania particles, prepared by hydrolysis and condensation using in situ steric stabilization, have been studied by high-energy, transmission, electron energy-loss spectroscopy. Electron diffraction patterns and energy-loss spectra as a function of momentum transfer were measured for as-prepared particles (amorphous titania), particles annealed at 600 °C (primarily anatase), and particles annealed at 1000 °C (primarily rutile). The energy-loss spectra at low momentum disagreed with the loss function calculated from optical data (rutile) and disagreed with theory (rutile and anatase). The data was fit by an Elliot-like model for a resonant exciton interacting with a continuum of levels. The translational effective mass of the exciton derived from the fitting was quite large, indicating that it was self-trapped.


Author(s):  
K. Shibatomi ◽  
T. Yamanoto ◽  
H. Koike

In the observation of a thick specimen by means of a transmission electron microscope, the intensity of electrons passing through the objective lens aperture is greatly reduced. So that the image is almost invisible. In addition to this fact, it have been reported that a chromatic aberration causes the deterioration of the image contrast rather than that of the resolution. The scanning electron microscope is, however, capable of electrically amplifying the signal of the decreasing intensity, and also free from a chromatic aberration so that the deterioration of the image contrast due to the aberration can be prevented. The electrical improvement of the image quality can be carried out by using the fascionating features of the SEM, that is, the amplification of a weak in-put signal forming the image and the descriminating action of the heigh level signal of the background. This paper reports some of the experimental results about the thickness dependence of the observability and quality of the image in the case of the transmission SEM.


Author(s):  
S. Takashima ◽  
H. Hashimoto ◽  
S. Kimoto

The resolution of a conventional transmission electron microscope (TEM) deteriorates as the specimen thickness increases, because chromatic aberration of the objective lens is caused by the energy loss of electrons). In the case of a scanning electron microscope (SEM), chromatic aberration does not exist as the restrictive factor for the resolution of the transmitted electron image, for the SEM has no imageforming lens. It is not sure, however, that the equal resolution to the probe diameter can be obtained in the case of a thick specimen. To study the relation between the specimen thickness and the resolution of the trans-mitted electron image obtained by the SEM, the following experiment was carried out.


Author(s):  
D.T. Grubb

Diffraction studies in polymeric and other beam sensitive materials may bring to mind the many experiments where diffracted intensity has been used as a measure of the electron dose required to destroy fine structure in the TEM. But this paper is concerned with a range of cases where the diffraction pattern itself contains the important information.In the first case, electron diffraction from paraffins, degraded polyethylene and polyethylene single crystals, all the samples are highly ordered, and their crystallographic structure is well known. The diffraction patterns fade on irradiation and may also change considerably in a-spacing, increasing the unit cell volume on irradiation. The effect is large and continuous far C94H190 paraffin and for PE, while for shorter chains to C 28H58 the change is less, levelling off at high dose, Fig.l. It is also found that the change in a-spacing increases at higher dose rates and at higher irradiation temperatures.


Author(s):  
David A. Ansley

The coherence of the electron flux of a transmission electron microscope (TEM) limits the direct application of deconvolution techniques which have been used successfully on unmanned spacecraft programs. The theory assumes noncoherent illumination. Deconvolution of a TEM micrograph will, therefore, in general produce spurious detail rather than improved resolution.A primary goal of our research is to study the performance of several types of linear spatial filters as a function of specimen contrast, phase, and coherence. We have, therefore, developed a one-dimensional analysis and plotting program to simulate a wide 'range of operating conditions of the TEM, including adjustment of the:(1) Specimen amplitude, phase, and separation(2) Illumination wavelength, half-angle, and tilt(3) Objective lens focal length and aperture width(4) Spherical aberration, defocus, and chromatic aberration focus shift(5) Detector gamma, additive, and multiplicative noise constants(6) Type of spatial filter: linear cosine, linear sine, or deterministic


Author(s):  
Atul S. Ramani ◽  
Earle R. Ryba ◽  
Paul R. Howell

The “decagonal” phase in the Al-Co-Cu system of nominal composition Al65CO15Cu20 first discovered by He et al. is especially suitable as a topic of investigation since it has been claimed that it is thermodynamically stable and is reported to be periodic in the dimension perpendicular to the plane of quasiperiodic 10-fold symmetry. It can thus be expected that it is an important link between fully periodic and fully quasiperiodic phases. In the present paper, we report important findings of our transmission electron microscope (TEM) study that concern deviations from ideal decagonal symmetry of selected area diffraction patterns (SADPs) obtained from several “decagonal” phase crystals and also observation of a lattice of main reflections on the 10-fold and 2-fold SADPs that implies complete 3-dimensional lattice periodicity and the fundamentally incommensurate nature of the “decagonal” phase. We also present diffraction evidence for a new transition phase that can be classified as being one-dimensionally quasiperiodic if the lattice of main reflections is ignored.


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