Quantification of atomic-scale grain boundary parameters by high-resolution electron microscopy

1992 ◽  
Vol 40 (3) ◽  
pp. 281-290 ◽  
Author(s):  
Karl L. Merkle
Author(s):  
M. I. Buckett ◽  
K. L. Merkle

With the advances in instrumentation and the capability of point-to-point resolution better than 0.2 nm, high resolution electron microscopy (HREM) is becoming more widely used for the quantitative study of both surfaces and internal interfaces. The elegance of the technique lies in its ability to deduce atomic-scale information on a localized scale. Without the proper analysis, however, HREM images can easily be misinterpreted. We investigate the considerations necessary for quantification of HREM images, using the measurement of the grain boundary volume expansion via the lattice fringe displacement technique as an example. The volume expansion, a parameter directly related to the grain boundary energy, is measured (in length units on the order of tenths of Å) as a rigid body translation normal to the boundary. It can be determined experimentally using statistical techniques which locate and fit the peak and valley positions in an experimental HREM image such that a direct measurement of the lattice fringe displacements is made.


2000 ◽  
Vol 652 ◽  
Author(s):  
K. L. Merkle ◽  
L. J. Thompson ◽  
Fritz Phillipp

ABSTRACTAtomic-scale grain boundary (GB) migration has been directly observed by high-resolution transmission electron microscopy (HREM). Atomic-scale motion of high-angle tilt GBs as well as twist and general GBs at gold island grains with a number of planar facets has been studied at ambient and elevated temperatures. GB migration mechanisms depend on GB structure and geometry. Strong indications for cooperative effects has been found. In this case, as has been proposed before, atoms may undergo small shifts in their lattice positions to be incorporated into the growing grain in a collective mode. At high temperature and in the absence of a strong driving force such small lattice regions are observed to fluctuate back and forth between the two grains. Faceted GBs typically move in spurts. This appears to be inherent to GB migration, whenever the motion is controlled by different structural entities. For some GB geometries the motion was found to proceed by the lateral propagation of atomic-scale steps.


Author(s):  
Jean-Luc Rouvière ◽  
Alain Bourret

The possible structural transformations during the sample preparations and the sample observations are important issues in electron microscopy. Several publications of High Resolution Electron Microscopy (HREM) have reported that structural transformations and evaporation of the thin parts of a specimen could happen in the microscope. Diffusion and preferential etchings could also occur during the sample preparation.Here we report a structural transformation of a germanium Σ=13 (510) [001] tilt grain boundary that occurred in a medium-voltage electron microscopy (JEOL 400KV).Among the different (001) tilt grain boundaries whose atomic structures were entirely determined by High Resolution Electron Microscopy (Σ = 5(310), Σ = 13 (320), Σ = 13 (510), Σ = 65 (1130), Σ = 25 (710) and Σ = 41 (910), the Σ = 13 (510) interface is the most interesting. It exhibits two kinds of structures. One of them, the M-structure, has tetracoordinated covalent bonds and is periodic (fig. 1). The other, the U-structure, is also tetracoordinated but is not strictly periodic (fig. 2). It is composed of a periodically repeated constant part that separates variable cores where some atoms can have several stable positions. The M-structure has a mirror glide symmetry. At Scherzer defocus, its HREM images have characteristic groups of three big white dots that are distributed on alternatively facing right and left arcs (fig. 1). The (001) projection of the U-structure has an apparent mirror symmetry, the portions of good coincidence zones (“perfect crystal structure”) regularly separate the variable cores regions (fig. 2).


1986 ◽  
Vol 77 ◽  
Author(s):  
Mary Beth Stearns ◽  
Amanda K. Petford-Long ◽  
C.-H. Chang ◽  
D. G. Stearns ◽  
N. M. Ceglio ◽  
...  

ABSTRACTThe technique of high resolution electron microscopy has been used to examine the structure of several multilayer systems (MLS) on an atomic scale. Mo/Si multilayers, in use in a number of x-ray optical element applications, and Mo/Si multilayers, of interest because of their magnetic properties, have been imaged in cross-section. Layer thicknesses, flatness and smoothness have been analysed: the layer width can vary by up to 0.6nm from the average value, and the layer flatness depends on the quality of the substrate surface for amorphous MLS, and on the details of the crystalline growth for the crystalline materials. The degree of crystallinity and the crystal orientation within the layers have also been investigated. In both cases, the high-Z layers are predominantly crystalline and the Si layers appear amorphous. Amorphous interfacial regions are visible between the Mo and Si layers, and crystalline cobalt suicide interfacial regions between the Co and Si layers. Using the structural measurements obtained from the HREM results, theoretical x-ray reflectivity behaviour has been calculated. It fits the experimental data very well.


2000 ◽  
Vol 15 (7) ◽  
pp. 1551-1555 ◽  
Author(s):  
Guo-Dong Zhan ◽  
Mamoru Mitomo ◽  
Yuichi Ikuhara ◽  
Taketo Sakuma

The thickness distribution of grain-boundary films during the superplastic deformation of fine-grained β–silicon nitride was investigated by high-resolution electron microscopy. In particular, grain-boundary thickness was considered with respect to the stress axis in two orientations; namely, parallel and perpendicular to the direction of applied stress. The results showed that the thickness distribution in boundaries perpendicular to the direction of applied stress was unimodal, whereas in parallel boundaries it was bimodal. Moreover, it was found that the majority of film-free boundaries were parallel to the direction of applied stress in the extremely deformed sample. The variation in spacing reflects distribution of stresses within the material due to irregular shape of the grains and the existence of percolating load-bearing paths through the microstructure.


1989 ◽  
Vol 159 ◽  
Author(s):  
A. Catana ◽  
M. Heintze ◽  
P.E. Schmid ◽  
P. Stadelmann

ABSTRACTHigh Resolution Electron Microscopy (HREM) was used to study microstructural changes related to the CoSi/Si-CoSi/CoSi2/Si-CoSi2/Si transformations. CoSi is found to grow epitaxially on Si with [111]Si // [111]CoSi and < 110 >Si // < 112 >CoSi. Two CoSi non-equivalent orientations (rotated by 180° around the substrate normal) can occur in this plane. They can be clearly distinguished by HRTEM on cross-sections ( electron beam along [110]Si). At about 500°C CoSi transforms to CoSi2. Experimental results show that the type B orientation relationship satisfying [110]Si // [112]CoSi is preserved after the initial stage of CoSi2 formation. At this stage an epitaxial CoSi/CoSi2/Si(111) system is obtained. The atomic scale investigation of the CoSi2/Si interface shows that a 7-fold coordination of the cobalt atoms is observed in both type A and type B epitaxies.


1990 ◽  
Vol 202 ◽  
Author(s):  
A. Catana ◽  
P.E. Schmid

ABSTRACTHigh Resolution Electron Microscopy (HREM) and image calculations are combined to study microstructural changes related to the CoSi/Si-CoSi/CoSi2/Si-CoSi2/Si transformations. The samples are prepared by UHV e-beam evaporation of Co layers (2 nm) followed by annealing at 300°C or 400°C. Cross-sectional observations at an atomic scale show that the silicidation of Co at the lower temperature yields epitaxial CoSi/Si domains such that [111]Si // [111]CoSi and <110>Si // <112>CoSi. At about 400°C CoSi2 nucleates at the CoSi/Si interface. During the early stages of this chemical reaction, an epitaxial CoSi/CoSi2/Si system is observed. The predominant orientation is such that (021) CoSi planes are parallel to (220) CoSi2 planes, the CoSi2/Si interface being of type B. The growth of CoSi2 is shown to proceed at the expense of both CoSi and Si.


1992 ◽  
Vol 287 ◽  
Author(s):  
H.-J. Kleebe ◽  
M. K. Cinibulk ◽  
I. Tanaka ◽  
J. Bruley ◽  
R. M. Cannon ◽  
...  

ABSTRACTCharacterization of silicon nitride ceramics by transmission electron microscopy (TEM) provides structural and compositional information on intergranular phases necessary to elucidate the factors that can influence the presence and thickness of grain-boundary films. Different TEM techniques can be used for the detection and determination of intergranular-film thickness, however, the most accurate results are obtained by high-resolution electron microscopy (HREM). HREM studies were applied, in conjunction with analytical electron microscopy, to investigate the correlation between intergranular-phase composition and film thickness. Statistical analyses of a number of grain-boundary films provided experimental verification of a theoretical equilibrium film thickness. Model experiments on a high-purity Si3N4 material, doped with low amounts of Ca, suggest the presence of two repulsive forces, a steric force and a force produced by an electrical double layer, that may act to balance the attractive van der Waals force necessary to establish an equilibrium film thickness.


Sign in / Sign up

Export Citation Format

Share Document