High-resolution Electron Microscopy Observation of Grain-boundary Films in Superplastically Deformed Silicon Nitride

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.

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.


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).


Author(s):  
Hiroshi Kakibayashi ◽  
Fumio Nagata

Many kinds of ceramics have been developed providing enough insulation, heat conduction or shock resistance. For the characteristics of strong toughness of the ceramics, movements of cracks by applying a force are noteworthy, because most ceramics are hardly distorted.In the present works, behavior of cracks in ceramics is observed with high resolution electron microscopy. Silicon nitride (Si3N4) ceramics were made by sintering in nitrogen atmosphere at 1800°C. Some Y2O3 and AlN were added to assist the sintering. A piece of the ceramics was sliced and polished mechanically untill 20μm in thickness. The specimen was mounted on a single hole grid, and was thinned with an ion etching equipment to be thin enough to observe.


Author(s):  
T. Kizuka ◽  
N. Tanaka

Mechanical properties of polycrystalline materials become anomalous when the grain size and grain boundary length decrease to nanometer scale. For example, ductility and toughness increase significantly in nanometer-grained ceramics (nanocrystalline ceramics). Ductility increases due to appearance of fine-grained-superplastic deformation. Grain boundary migration and interface migration are fundamental processes of the superplastic deformation. Structural transformation of fine grains is a factor which limits the toughness in polycrystalline ceramics because the transformation relaxes internal strain. The behavior of grain boundaries and interfaces, such as diffusion bonding and Czochralski-type crystal growth at ambient temperature, can be analyzed by a time-resolved high-resolution electron microscopy (TRHREM) developed by Kizuka et al.,In the present study, grain boundary migration and successive transformation of crystal structure in nanocrystalline ZnO were investigated by TRHREM.Zinc oxide was vacuum-deposited on air-cleaved (001) surfaces of sodium chloride at 200°C. TRHREM was carried out at room temperature using a 200-kV electron microscope (JEOL, JEM2010) equipped with a high sensitive TV camera and a video tape recorder.


1999 ◽  
Vol 589 ◽  
Author(s):  
V. Potin ◽  
G. Nouet ◽  
P. Ruterana ◽  
R.C. Pond

AbstractThe studied GaN layers are made of mosaYc grains rotated around the c-axis by angles in the range 0-25°. Using high-resolution electron microscopy, anisotropic elasticity calculations and image simulation, we have analyzed the atomic structure of the edge threading dislocations. Here, we present an analysis of the Σ = 7 boundary using circuit mapping in order to define the Burgers vectors of the primary and secondary dislocations. The atomic structure of the primary ones was found to exhibit 5/7 and 8 atom cycles.


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