Decagonal single quasicrystals of the composition Al70Ni15Co15 have been deformed in situ in a high-voltage transmission electron microscope at 730 °C along the 10-fold periodic axis to directly observe the dislocation motion. The deformation is carried by stress-assisted climb of dislocations with periodic Burgers vectors. These dislocations may also glide and move by a combination of glide and climb. Dislocations with Burgers vectors with components in the periodic and quasiperiodic directions probably move under the action of a chemical force. The observations are interpreted by a model established by P. Schall et al. under consideration of the activation parameters of macroscopic deformation and by analogies with the behavior of icosahedral quasicrystals.

Crystallization of amorphous thin films composed of doped SbxTe with x = 3.0, 3.6, and 4.2 and constant dopant level was studied by in situ heating in a transmission electron microscopy. Magnetron sputtering was used to deposit 20-nm-thick films sandwiched between two types of 3-nm-thick dielectric layers on 25-nm-thick silicon-nitride membranes. One type of dielectric layer consists of ZnS–SiO2 (ZSO), the other of GeCrN (GCN). Crystallization was studied for temperatures in-between 150 and 190 °C. The type of dielectric layer turned out to strongly influence the crystallization process. Not only did the nucleation rate appear to depend sensitively on the dielectric layer type, but also the growth rate. The velocity of the crystalline/amorphous interface is about 5 times higher for the x = 4.2 film than for the x = 3.0 film if ZSO is used. In case of GCN, the interface velocity is about 2 times higher for the x = 4.2 film than for the x = 3.0 film. The activation energy for crystal growth is not significantly dependent on the Sb/Te ratio but is clearly different for ZSO and GCN—2.9 eV and 2.0 eV, respectively. The incubation time for the crystal nuclei formation is longer for ZSO than for GCN. Although the effects of the Sb/Te ratio and the dielectric layer type on the growth rates are strong, their effects on the nucleation rate are even more pronounced. A higher Sb/Te ratio results in a lower nucleation rate and the use of GCN instead of ZSO leads to higher nucleation rates.

In a specially equipped transmission electron microscope (TEM), Ni particles were vapor deposited onto thin films of amorphous carbon (a-C), and subsequent reactions with the carbon support were observed at elevated temperatures. Particles deposited at temperatures around 370 °C developed a graphite shell at above 600 °C and subsequently spread and graphitized the substrate. This activity was enhanced by hydrogen. The speed of graphitization significantly increased during spreading of the metal, which is attributed to the concomitant increase of the length of the reaction front, as well as to a purifying effect of hydrogen. It is concluded that the driving force for spreading of the Ni is the interdiffusion and catalytic conversion of carbonto graphite at the reaction front. Particles deposited at 500 °C remained inactive at670 °C. This is probably due to the formation of a rather stable carbidic or graphitic interlayer during deposition.

Nanoparticulate materials are promising objects for studying the processes that triggermelting of solids. On a pyrolytic route, we successfully encapsulated 20–60 nm diameter Cu nanocrystals within multilayer graphitic carbon spheres. In situ electron microscope observations of the melting and displacement of the encapsulated Cu nanocrystals at temperatures up to 1175 K have provided clear evidence of the process of surface melting and its dependence on the quality of the metal/carbon interface. Detection of crystal defects inside the Cu particles during melting and vaporization has proved that the metal phase maintains its solid crystalline state in the particle center. Indications of the influence of surface anisotropy on the melting behavior were obtained. The carbon cages as a whole remained unchanged during the observations.

In situ local measurement of sub-threshold strains generated during the electromigration of a 0.3-μm-wide Al interconnect was performed for the first time using convergent-beam electron diffraction (CBED) in a transmission electron microscope (TEM). Thermal strains were also analyzed and provided verification for the electromigration analysis. Spatially averaged strains resulting from thermal cycling and electromigration quantitatively agree with models and data from previous studies. However, the local strains exhibited variations as large as 2 × 10−3. After eliminating other possible mechanisms, the strain inhomogeneity is attributed to local plasticity through source-limited dislocation activity.

Yttria-stabilized zirconia (YSZ)-Au composite coatings have great potential as solid film lubricants for aerospace applications over a wide range of environmental conditions. They were grown on steel disks or silicon wafers by pulsed laser ablation of YSZ and simultaneous magnetron sputtering of a Au target. Such a combination of ceramics with soft metals improved the toughness of the composite coating and increased its ability to lubricate at high temperature. Information on the time-dependent response of these microstructures to changes in temperature is essential to tribological investigations of high temperature performance. In situ transmission electron microscopy was used to directly measure the dynamic change of YSZ-Au coating structure at elevated temperatures. High-resolution electron microscopy and electron diffraction showed that amorphous YSZ-5 at.% Au coatings proceeded to crystallize under the irradiation of electron beams. Time varying x-ray energy dispersive spectra measured a loss of oxygen in the sample during about 10 min of irradiation with subsequent slight oxygen recovery. This behavior was related to the activation of oxygen diffusion under electron irradiation. X-ray diffraction patterns from vacuum annealed samples verified crystallization of the coatings at 500 °C. Real-time growth of Au nanograins in the sample was observed as the temperature was increased to 500 °C in a TEM specimen holder that could be heated. The grain growth process was recorded using a charge-coupled device camera installed on the transmission electron microscope. The crystallization and growth of zirconia and Au nanograins resulted in low friction during tribological tests. The nucleation of Au islands on heated ball-on-flat specimens was responsible for lowering friction.

A unique straining device, fabricated using microlithographic techniques, has been developed to permit real-time investigation in the transmission electron microscope (TEM) of the deformation and failure mechanisms in ultrafine-grained aluminum. The tensile specimen is a freestanding thin film with a columnar microstructure that has a uniform cross-section (100 × 0.125 μm) and a gauge length of 300 μm. In situ TEM straining experiments show the fracture mode is intergranular with no accompanying general plasticity. Propagating cracks were halted at large grains, and crack blunting occurred through grain-boundary-mediated processes. The blunting process was accompanied by dislocation emission and deformation twinning in the grain responsible for arresting the crack. Voids or microcracks nucleated and grew on grain boundaries ahead of the arrested crack, and crack advance occurred through linkage of the microcracks and the primary crack.

The crystallization process of yttria-stabilized zirconia (YSZ) gate dielectrics deposited on p-Si (001) and SiOx/p-Si(001) substrates and the growth process of SiOx has been investigated directly using high-temperature in situ cross-sectional view transmission electron microscopy (TEM) method and high-temperature plan-view in-situ TEM method. The YSZ layer is crystallized by the nucleation and growth mechanism at temperatures greater than 573 K. Nucleation originates from the film surface. Nucleation occurs randomly in the YSZ layer. Subsequently, the crystallized YSZ area strains the Si surface. Finally, it grows in the in-plane direction with the strain, whereas, if a SiOx layer of 1.4 nm exists, it absorbs the crystallization strain. Thereby, an ultrathin SiOx layer can relax the strain generated in the Si substrate in thin film crystallization process.

To understand the role of boundaries in the deformation behavior of TiAl, in situ straining experiments in transmission electron microscopy have been performed on thin foils of polysynthetically twinned (PST) crystal of Ti–49.3 at.% Al. The deformation behavior of PST TiAl is anisotropic, depending on the angle between the lamellar boundaries and the straining axes. For L-orientation, deformation twins and ordinary dislocations transmit across the true-twin (TT) boundaries but are reflected at the pseudo-twin (PT) and rotational order-fault (RO) boundaries. For transverse (T) orientation, deformation twins are transmitted across all TT, PT, and RO boundaries. For I-orientation, shear deformation occurs parallel to the lamellar boundaries. There is a transmission of deformation across the interphase (IP) boundary in longitudinal orientation, but deformation is blocked and reflected at the IP boundary in T-orientation. The role of the various types of boundaries in localized deformation behavior was evaluated by considering Schmid factors and geometric compatibility factors.

The initial oxidation behaviors of Cu–50 at.% Au (001) single-crystal thin film were studied by in situ ultra-high-vacuum transmission electron microscopy to model nano-oxidation of alloys with one oxidizing component and one inert component. The oxidation behaviors such as incubation time, oxide nucleation rate, oxide growth kinetics as well as nucleation activation energy were greatly changed by the addition of nonoxidizing Au. The reasons for these changes, such as Au segregation to the top surface, a decrease in Cu activity, and reduced lattice mismatch due to the addition of Au, were discussed, and a qualitative analysis of nucleation energetics was given.

The nucleation and growth of Cu2O islands due to Cu(100) oxidation at temperatures from 200 to 350 °C have been observed by in situ ultra-high-vacuum transmission electron microscopy. For this temperature range, epitaxial Cu2O islands form a triangular shape with rounded edges when Cu(100) is exposed to dry oxygen at 5 × 10−4 Torr in situ. Our initial analysis on the nucleation and growth of these three-dimensional Cu2O islands agrees well with the heteroepitaxial model of surface diffusion of oxygen.

An iron nitride sample was irradiated by 2-MeV electrons intermittently for 2100 s with a dose rate of 6.3 × 1024 e.m.−2 s−1 inside a 3-MV high-voltage transmission electron microscope. The electron-stimulated oxidation of Fe4N and Fe2–3N was investigated in situ and ex situ using conventional transmission electron microscopy and high-resolution electron microscopy. It was found that both Fe4N and Fe2–3N nitrides were oxidized by the residual gas in the vacuum chamber to form Fe3O4 oxides. The orientation relationship between Fe4N (γ′) and Fe3O4 (o) was (110)γ′//(220)o, [001]γ′//[001]o, and that between Fe2–3N (ϵ) and Fe3O4 (o) was (110)ϵ//(−220)o, [1–11]ϵ//[001]o. Crystal lattice deformation from iron nitride to iron oxide took place during the dynamic oxidation process. Structural models were proposed to understand the oxide formation, and the models were confirmed by experimental observations. The irradiation effects of Fe4N and Fe2–3N crystals were compared. The results show that Fe4N is more sensitive than Fe2–3N to electron irradiation. These results are important not only for the fabrication of insulating iron oxide film, but also in the field of the surface modification of iron nitride to improve its mechanical properties.