Time-resolved high-resolution electron microscopy of structural transformation in nanocrystalline ZnO films

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.

Author(s):  
T. Kizuka ◽  
M. Iijima ◽  
N. Tanaka

High-resolution electron microscopy (HREM) has been employed intensively to analyze the atomic structures of grain boundaries and interfaces having two dimensional structures inside polycrystalline and composite materials. Furthermore time-resolved HREM (TRHREM) is required to analyze the behavior of grain boundaries and interfaces at atomic scale. The grain boundary migration, which is a typical grain boundary behavior, is a fundamental process relating to structural stability of polycrystalline materials. The mechanism of the migration has been still unknown.In the present study, the variation of atomic arrangement at the grain boundary migration of a MgO [001]Σ5 boundary was analyzed by TRHREM.Magnesium oxide polycrystalline films were prepared by vacuum-deposition on air-cleaved (001) surfaces of sodium chloride at 300°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. The spatial resolution of the system was 0.2 nm at 200 kV and the time resolution was 1/60 s. Electron beam density was 30 A/cm2.


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).


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):  
T. Kizuka ◽  
N. Tanaka

Structure and stability of atomic clusters have been studied by time-resolved high-resolution electron microscopy (TRHREM). Typical examples are observations of structural fluctuation in gold (Au) clusters supported on silicon oxide films, graphtized carbon films and magnesium oxide (MgO) films. All the observations have been performed on the clusters consisted of single metal element. Structural stability of ceramics clusters, such as metal-oxide, metal-nitride and metal-carbide clusters, has not been observed by TRHREM although the clusters show anomalous structural and functional properties concerning to solid state physics and materials science.In the present study, the behavior of ceramic, magnesium oxide (MgO) clusters is for the first time observed by TRHREM at 1/60 s time resolution and at atomic resolution down to 0.2 nm.MgO and gold were subsequently deposited on sodium chloride (001) substrates. The specimens, single crystalline MgO films on which Au particles were dispersed were separated in distilled water and observed by using a 200-kV high-resolution electron microscope (JEOL, JEM2010) equipped with a high sensitive TV camera and a video tape recorder system.


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.


1996 ◽  
Vol 11 (8) ◽  
pp. 1880-1890 ◽  
Author(s):  
Zenji Horita ◽  
David J. Smith ◽  
Minoru Furukawa ◽  
Minoru Nemoto ◽  
Ruslan Z. Valiev ◽  
...  

High-resolution electron microscopy was used to examine the structural features of grain boundaries in Al–1.5% Mg and Al–3% Mg solid solution alloys produced with submicrometer grain sizes using an intense plastic straining technique. The grain boundaries were mostly curved or wavy along their length, and some portions were corrugated with regular or irregular arrangements of facets and steps. During exposure to high-energy electrons, grain boundary migration occurred to reduce the number of facets and thus to reduce the total boundary energy. The observed features demonstrate conclusively that the grain boundaries in these submicrometer-grained materials are in a high-energy nonequilibrium configuration.


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