A Novel Optical Method for Estimating the Dispersion of Carbon Black in Rubbers

1981 ◽  
Vol 54 (4) ◽  
pp. 698-717 ◽  
Author(s):  
P. C. Ebell ◽  
D. A. Hemsley
Keyword(s):  
Carbon Black ◽  
Dark Field Image ◽  
Dark Field ◽  
Specimen Preparation ◽  
Additional Advantage ◽  
Internal Mixing ◽  
Reflected Light ◽  
Large Program ◽  
Wide Range ◽  
Mixing Behavior

Abstract The work reported is part of a large program aimed at examining the internal mixing of rubbers and its effect on properties. The dispersion of carbon black in the compound is of primary importance. Standard microscopical methods used industrially to measure this parameter are either subjective or lack discrimination at the higher levels of dispersion. To study mixing behavior effectively it is necessary to be able to assess the property over a wide range of degrees of dispersion. A technique based on the analysis of the dark field image produced by a reflected light microscope has been developed. The specimen preparation is simple, and analysis is carried out using a standard T.V. system. The technique gives results which are sufficiently discriminating to allow correlation of black dispersion with processing and mechanical properties, even at extremely high levels of mixing. An additional advantage of the method is that unvulcanized samples may be used.

Observation of Atom Rows in Thorium Pyromellitate Using a Field Emission STEM

1977 ◽  
Vol 35 ◽  
pp. 80-81
Author(s):  
H. Todokoro ◽  
S. Nomura ◽  
T. Komoda
Keyword(s):  
Field Emission ◽  
Amorphous Carbon ◽  
Carbon Film ◽  
Dark Field Image ◽  
Dark Field ◽  
Amorphous Carbon Film ◽  
Atomic Size ◽  
Wide Range ◽  
A Chain

It is interesting to observe polymers at atomic size resolution. Some works have been reported for thorium pyromellitate by using a STEM (1), or a CTEM (2,3). The results showed that this polymer forms a chain in which thorium atoms are arranged. However, the distance between adjacent thorium atoms varies over a wide range (0.4-1.3nm) according to the different authors.The present authors have also observed thorium pyromellitate specimens by means of a field emission STEM, described in reference 4. The specimen was prepared by placing a drop of thorium pyromellitate in 10-3 CH3OH solution onto an amorphous carbon film about 2nm thick. The dark field image is shown in Fig. 1A. Thorium atoms are clearly observed as regular atom rows having a spacing of 0.85nm. This lattice gradually deteriorated by successive observations. The image changed to granular structures, as shown in Fig. 1B, which was taken after four scanning frames.

Direct STEM ADF imaging of gold on silicon (111)

1989 ◽  
Vol 47 ◽  
pp. 472-473
Author(s):  
P. Xu ◽  
E. J. Kirkland ◽  
J. Silcox
Keyword(s):  
Film Growth ◽  
Heavy Atom ◽  
High Vacuum ◽  
Dark Field ◽  
Thin Metal Film ◽  
Base Pressure ◽  
Ultra High Vacuum ◽  
Specimen Preparation ◽  
Dark Field Imaging ◽  
Wide Range

Many studies of thin metal film growth and the formation of metal-semiconductor contacts have been performed using a wide range of experimental methods. STEM annular dark field imaging could be an important complement since it may allow direct imaging of a single heavy atom on a thin silicon substrate. This would enable studies of the local atomic arrangements and defects in the initial stage of metal silicide formation.Preliminary experiments were performed in an ultra-high vacuum VG HB501A STEM with a base pressure of 1 × 10-10 mbar. An antechamber directly attached to the microscope for specimen preparation has a base pressure of 2×l0-10 mbar. A thin single crystal membrane was fabricated by anodic etching and subsequent reactive etching. The specimen was cleaned by the Shiraki method and had a very thin oxide layer left on the surface. 5 Å of gold was deposited on the specimen at room temperature from a tungsten filament coil monitored by a quartz crystal monitor.

A Preparation of High Resolution Standards for Electron Microscopy. Part II

1971 ◽  
Vol 29 ◽  
pp. 160-161
Author(s):  
Akira Tanaka ◽  
David F. Harling
Keyword(s):  
Electron Microscopy ◽  
High Resolution ◽  
Carbon Black ◽  
Single Crystal ◽  
Dark Field ◽  
Graphitized Carbon Black ◽  
Graphitized Carbon ◽  
Dark Field Imaging ◽  
Crystal Films ◽  
Micro Holes

In the previous paper, the author reported on a technique for preparing vapor-deposited single crystal films as high resolution standards for electron microscopy. The present paper is intended to describe the preparation of several high resolution standards for dark field microscopy and also to mention some results obtained from these studies. Three preparations were used initially: 1.) Graphitized carbon black, 2.) Epitaxially grown particles of different metals prepared by vapor deposition, and 3.) Particles grown epitaxially on the edge of micro-holes formed in a gold single crystal film.The authors successfully obtained dark field micrographs demonstrating the 3.4Å lattice spacing of graphitized carbon black and the Au single crystal (111) lattice of 2.35Å. The latter spacing is especially suitable for dark field imaging because of its preparation, as in 3.), above. After the deposited film of Au (001) orientation is prepared at 400°C the substrate temperature is raised, resulting in the formation of many square micro-holes caused by partial evaporation of the Au film.

Enhancement of Contrast in the CEM and STEM Using Bumpy Specimens and Employing the “Dappled Field” Mode of Operation

1974 ◽  
Vol 32 ◽  
pp. 552-553 ◽  
Author(s):  
L. Gandolfi ◽  
J. Reiffel
Keyword(s):  
Operating Mode ◽  
Scanning Transmission Electron Microscope ◽  
Dark Field ◽  
Specimen Preparation ◽  
Field Mode ◽  
Preparation Methods ◽  
Scanning Transmission Electron ◽  
Transmission Electron ◽  
Mode Of Operation ◽  
Scanning Transmission

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.

Applications of Through-Focus Dark Field Image Shifts to Phase Identification

1975 ◽  
Vol 33 ◽  
pp. 178-179
Author(s):  
Prakash Rao
Keyword(s):  
Dark Field Image ◽  
Thin Foil ◽  
Dark Field ◽  
The Other ◽  
Stereo Image ◽  
Phase Identification ◽  
The Past ◽  
Field Electron Microscopy ◽  
Dark Field Electron ◽  
Recent Extension

Image shifts in out-of-focus dark field images have been used in the past to determine, for example, epitaxial relationships in thin films. A recent extension of the use of dark field image shifts has been to out-of-focus images in conjunction with stereoviewing to produce an artificial stereo image effect. The technique, called through-focus dark field electron microscopy or 2-1/2D microscopy, basically involves obtaining two beam-tilted dark field images such that one is slightly over-focus and the other slightly under-focus, followed by examination of the two images through a conventional stereoviewer. The elevation differences so produced are usually unrelated to object positions in the thin foil and no specimen tilting is required.In order to produce this artificial stereo effect for the purpose of phase separation and identification, it is first necessary to select a region of the diffraction pattern containing more than just one discrete spot, with the objective aperture.

Effets of surfaces on precipitate morphology in irradiated thin foils

1978 ◽  
Vol 36 (1) ◽  
pp. 654-655
Author(s):  
D.I. Potter ◽  
A. Taylor
Keyword(s):  
Ion Irradiation ◽  
Dark Field Image ◽  
Thin Foil ◽  
Dark Field ◽  
Al Alloy ◽  
Bright Field Image ◽  
Dislocation Loops ◽  
Precipitate Morphology ◽  
Thin Foils

Thermal aging of Ni-12.8 at. % A1 and Ni-12.7 at. % Si produces spatially homogeneous dispersions of cuboidal γ'-Ni3Al or Ni3Si precipitate particles arrayed in the Ni solid solution. We have used 3.5-MeV 58Ni+ ion irradiation to examine the effect of irradiation during precipitation on precipitate morphology and distribution. The nearness of free surfaces produced unusual morphologies in foils thinned prior to irradiation. These thin-foil effects will be important during in-situ investigations of precipitation in the HVEM. The thin foil results can be interpreted in terms of observations from bulk irradiations which are described first.Figure 1a is a dark field image of the γ' precipitate 5000 Å beneath the surface(∿1200 Å short of peak damage) of the Ni-Al alloy irradiated in bulk form. The inhomogeneous spatial distribution of γ' results from the presence of voids and dislocation loops which can be seen in the bright field image of the same area, Fig. 1b.

A Novel TEM Technique for Characterizing As-Grown CVD Diamond Films

1991 ◽  
Vol 49 ◽  
pp. 956-957 ◽  
Author(s):  
Z.L. Wang ◽  
J. Bentley ◽  
R.E. Clausing ◽  
L. Heatherly ◽  
L.L. Horton
Keyword(s):  
Diamond Films ◽  
Chemical Vapor ◽  
Growth Direction ◽  
Dark Field ◽  
Growth Surface ◽  
Specimen Preparation ◽  
Transmission Electron ◽  
Diffraction Patterns ◽  
First Time ◽  
Microstructural Studies

Microstructural studies by transmission electron microscopy (TEM) of diamond films grown by chemical vapor deposition (CVD) usually involve tedious specimen preparation. This process has been avoided with a technique that is described in this paper. For the first time, thick as-grown diamond films have been examined directly in a conventional TEM without thinning. With this technique, the important microstructures near the growth surface have been characterized. An as-grown diamond film was fractured on a plane containing the growth direction. It took about 5 min to prepare a sample. For TEM examination, the film was tilted about 30-45° (see Fig. 1). Microstructures of the diamond grains on the top edge of the growth face can be characterized directly by transmitted electron bright-field (BF) and dark-field (DF) images and diffraction patterns.

Density-based discrimination of protein and RNA in the ribosome

1992 ◽  
Vol 50 (1) ◽  
pp. 464-465
Author(s):  
Joachim Frank
Keyword(s):  
Transfer Function ◽  
Spatial Frequency ◽  
Three Dimensional ◽  
Wiener Filter ◽  
Dark Field Image ◽  
Dark Field ◽  
Frequency Range ◽  
Bright Field ◽  
Contrast Transfer Function ◽  
Pass Filter

Cryo-electron microscopy combined with single-particle reconstruction techniques has allowed us to form a three-dimensional image of the Escherichia coli ribosome.In the interior, we observe strong density variations which may be attributed to the difference in scattering density between ribosomal RNA (rRNA) and protein. This identification can only be tentative, and lacks quantitation at this stage, because of the nature of image formation by bright field phase contrast. Apart from limiting the resolution, the contrast transfer function acts as a high-pass filter which produces edge enhancement effects that can explain at least part of the observed variations. As a step toward a more quantitative analysis, it is necessary to correct the transfer function in the low-spatial-frequency range. Unfortunately, it is in that range where Fourier components unrelated to elastic bright-field imaging are found, and a Wiener-filter type restoration would lead to incorrect results. Depending upon the thickness of the ice layer, a varying contribution to the Fourier components in the low-spatial-frequency range originates from an “inelastic dark field” image. The only prospect to obtain quantitatively interpretable images (i.e., which would allow discrimination between rRNA and protein by application of a density threshold set to the average RNA scattering density may therefore lie in the use of energy-filtering microscopes.

EM of rapidly solidified permanent magnets

1992 ◽  
Vol 50 (1) ◽  
pp. 198-199
Author(s):  
Raja K. Mishra
Keyword(s):  
Melt Spinning ◽  
Permanent Magnets ◽  
Dark Field Image ◽  
Dark Field ◽  
Maximum Energy ◽  
Quench Rate ◽  
Maximum Energy Product ◽  
Energy Product ◽  
Annular Dark Field ◽  
Rapidly Solidified

The discovery of a new class of permanent magnets based on Nd2Fe14B phase in the last decade has led to intense research and development efforts aimed at commercial exploitation of the new alloy. The material can be prepared either by rapid solidification or by powder metallurgy techniques and the resulting microstructures are very different. This paper details the microstructure of Nd-Fe-B magnets produced by melt-spinning.In melt spinning, quench rate can be varied easily by changing the rate of rotation of the quench wheel. There is an optimum quench rate when the material shows maximum magnetic hardening. For faster or slower quench rates, both coercivity and maximum energy product of the material fall off. These results can be directly related to the changes in the microstructure of the melt-spun ribbon as a function of quench rate. Figure 1 shows the microstructure of (a) an overquenched and (b) an optimally quenched ribbon. In Fig. 1(a), the material is nearly amorphous, with small nuclei of Nd2Fe14B grains visible and in Fig. 1(b) the microstructure consists of equiaxed Nd2Fe14B grains surrounded by a thin noncrystalline Nd-rich phase. Fig. 1(c) shows an annular dark field image of the intergranular phase. Nd enrichment in this phase is shown in the EDX spectra in Fig. 2.

A New Detector System For The HB5 Stem Instrument

1985 ◽  
Vol 43 ◽  
pp. 134-135
Author(s):  
J.M. Cowley
Keyword(s):  
Dark Field ◽  
Detector System ◽  
Electron Holography ◽  
Small Specimen ◽  
Bright Field ◽  
Multiple Images ◽  
Practical Applications ◽  
Wide Range ◽  
Diffraction Patterns ◽  
Operational Modes

The HB5 STEM instrument at ASU has been modified previously to include an efficient two-dimensional detector incorporating an optical analyser device and also a digital system for the recording of multiple images. The detector system was built to explore a wide range of possibilities including in-line electron holography, the observation and recording of diffraction patterns from very small specimen regions (having diameters as small as 3Å) and the formation of both bright field and dark field images by detection of various portions of the diffraction pattern. Experience in the use of this system has shown that sane of its capabilities are unique and valuable. For other purposes it appears that, while the principles of the operational modes may be verified, the practical applications are limited by the details of the initial design.

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