Shot-noise simulations of HREM images of polymer crystals

Author(s):  
Philippe Pradère ◽  
Edwin L. Thomas

High Resolution Electron Microscopy (HREM) is a very powerful technique for the study of crystal defects at the molecular level. Unfortunately polymer crystals are beam sensitive and are destroyed almost instantly under the typical HREM imaging conditions used for inorganic materials. Recent developments of low dose imaging at low magnification have nevertheless permitted the attainment of lattice images of very radiation sensitive polymers such as poly-4-methylpentene-1 and enabled molecular level studies of crystal defects in somewhat more resistant ones such as polyparaxylylene (PPX) [2].With low dose conditions the images obtained are very noisy. Noise arises from the support film, photographic emulsion granularity and in particular, the statistical distribution of electrons at the typical doses of only few electrons per unit resolution area. Figure 1 shows the shapes of electron distribution, according to the Poisson formula :

Author(s):  
J. A. Hugo ◽  
V. A. Phillips

A continuing problem in high resolution electron microscopy is that the level of detail visible to the microscopist while he is taking a picture is inferior to that obtainable by the microscope, readily readable on a photographic emulsion and visible in an enlargement made from the plate. Line resolutions, of 2Å or better are now achievable with top of the line 100kv microscopes. Taking the resolution of the human eye as 0.2mm, this indicates a need for a direct viewing magnification of at least one million. However, 0.2mm refers to optimum viewing conditions in daylight or the equivalent, and certainly does not apply to a (colored) image of low contrast and illumination level viewed on a fluorescent screen through a glass window by the dark-adapted eye. Experience indicates that an additional factor of 5 to 10 magnification is needed in order to view lattice images with line spacings of 2 to 4Å. Fortunately this is provided by the normal viewing telescope supplied with most electron microscopes.


Author(s):  
W. H. Wu ◽  
R. M. Glaeser

Spirillum serpens possesses a surface layer protein which exhibits a regular hexagonal packing of the morphological subunits. A morphological model of the structure of the protein has been proposed at a resolution of about 25 Å, in which the morphological unit might be described as having the appearance of a flared-out, hollow cylinder with six ÅspokesÅ at the flared end. In order to understand the detailed association of the macromolecules, it is necessary to do a high resolution structural analysis. Large, single layered arrays of the surface layer protein have been obtained for this purpose by means of extensive heating in high CaCl2, a procedure derived from that of Buckmire and Murray. Low dose, low temperature electron microscopy has been applied to the large arrays.As a first step, the samples were negatively stained with neutralized phosphotungstic acid, and the specimens were imaged at 40,000 magnification by use of a high resolution cold stage on a JE0L 100B. Low dose images were recorded with exposures of 7-9 electrons/Å2. The micrographs obtained (Fig. 1) were examined by use of optical diffraction (Fig. 2) to tell what areas were especially well ordered.


Author(s):  
J.M. Cowley

By extrapolation of past experience, it would seem that the future of ultra-high resolution electron microscopy rests with the advances of electron optical engineering that are improving the instrumental stability of high voltage microscopes to achieve the theoretical resolutions of 1Å or better at 1MeV or higher energies. While these high voltage instruments will undoubtedly produce valuable results on chosen specimens, their general applicability has been questioned on the basis of the excessive radiation damage effects which may significantly modify the detailed structures of crystal defects within even the most radiation resistant materials in a period of a few seconds. Other considerations such as those of cost and convenience of use add to the inducement to consider seriously the possibilities for alternative approaches to the achievement of comparable resolutions.


Author(s):  
David J. Smith

The era of atomic-resolution electron microscopy has finally arrived. In virtually all inorganic materials, including oxides, metals, semiconductors and ceramics, it is possible to image individual atomic columns in low-index zone-axis projections. A whole host of important materials’ problems involving defects and departures from nonstoichiometry on the atomic scale are waiting to be tackled by the new generation of intermediate voltage (300-400keV) electron microscopes. In this review, some existing problems and limitations associated with imaging inorganic materials are briefly discussed. The more immediate problems encountered with organic and biological materials are considered elsewhere.Microscope resolution. It is less than a decade since the state-of-the-art, commercially available TEM was a 200kV instrument with a spherical aberration coefficient of 1.2mm, and an interpretable resolution limit (ie. first zero crossover of the contrast transfer function) of 2.5A.


Author(s):  
M. Pan

It has been known for many years that materials such as zeolites, polymers, and biological specimens have crystalline structures that are vulnerable to electron beam irradiation. This radiation damage severely restrains the use of high resolution electron microscopy (HREM). As a result, structural characterization of these materials using HREM techniques becomes difficult and challenging. The emergence of slow-scan CCD cameras in recent years has made it possible to record high resolution (∽2Å) structural images with low beam intensity before any apparent structural damage occurs. Among the many ideal properties of slow-scan CCD cameras, the low readout noise and digital recording allow for low-dose HREM to be carried out in an efficient and quantitative way. For example, the image quality (or resolution) can be readily evaluated on-line at the microscope and this information can then be used to optimize the operating conditions, thus ensuring that high quality images are recorded. Since slow-scan CCD cameras output (undistorted) digital data within the large dynamic range (103-104), they are ideal for quantitative electron diffraction and microscopy.


Author(s):  
W. Coene ◽  
F. Hakkens ◽  
T.H. Jacobs ◽  
K.H.J. Buschow

Intermetallic compounds of the type RE2Fe17Cx (RE= rare earth element) are promising candidates for permanent magnets. In case of Y2Fe17Cx, the Curie temperature increases from 325 K for x =0 to 550 K for x = 1.6 . X ray and electron diffraction reveal a carbon - induced structural transformation in Y2Fe17Cx from the hexagonal Th2Ni17 - type (x < 0.6 ) to the rhombohedral Th2Zn17 - type ( x ≥ 0.6). Planar crystal defects introduce local sheets of different magnetic anisotropy as compared with the ordered structure, and therefore may have an important impact on the coercivivity mechanism .High resolution electron microscopy ( HREM ) on a Philips CM30 / Super Twin has been used to characterize planar crystal defects in rhombohedral Y2Fe17Cx ( x ≥ 0.6 ). The basal plane stacking sequences are imaged in the [100] - orientation, showing an ABC or ACB sequence of Y - atoms and Fe2 - dumbbells, for both coaxial twin variants, respectively . Compounds resulting from a 3 - week annealing treatment at high temperature ( Ta = 1000 - 1100°C ) contain a high density of planar defects.


1983 ◽  
Vol 219 (1215) ◽  
pp. 111-117 ◽  

The calcite coccoliths from the alga Emiliania huxleyi (Lohmann) Hay and Mohler have been studied by ultra-high resolution electron microscopy. This paper describes the two different types of structure observed, one in the upper elements, the other in the basal plate, or lower element. The former consisted of small, microdomain structures of 300-500 Å (1 Å = 10 -10 m) in length with no strong orientation. At places along these elements, and particularly in the junction between stem and head pieces, triangular patterns of lattice fringes were observed indicating multiple nucleation sites in the structure. In contrast, the lower element consisted of a very thin single crystalline sheet of calcite which could be resolved into a two dimensional lattice image, shown by a computer program that is capable of simulating electron diffraction patterns and lattice images to be a [421] zone of calcite. A possible mechanism for these growth patterns in the formation of coccoliths is discussed, together with the relevance of such mechanisms to biomineralization generally.


1996 ◽  
Vol 11 (7) ◽  
pp. 1783-1786 ◽  
Author(s):  
N. Jiang ◽  
A. Hatta ◽  
T. Ito ◽  
Z. Zhang ◽  
T. Sasaki ◽  
...  

We have investigated the near-interface characterization of diamond films grown on Si(100) substrates by means of a hot-filament chemical-vapor-deposition (HFCVD) method using high-resolution-electron microscopy (HREM). Atomic scale study of the diamond/Si interface reveals that on the top of the amorphous intermediate layer, there exists a precursor phase which seems to be a diamond-like structure, which provides a suitable site for subsequent diamond nucleation. High density crystal defects directly originate from the precursor phase. HREM images also reveal that during the deposition Si recrystallizes in some damaged areas left by pretreatment, such as scratching grooves. In the recrystallization process twins and microtwins can be formed, and amorphous solid is left in the Si crystals.


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