Nonconductive specimens for scanning electron microscopy or X-ray microanalysis are coated with conductive carbon in order to reduce charging. But carbon film absorbs X-ray fluxes causing errors in measuring chemical composition. Especially when the carbon content is measured, carbon coating not only blocks X-rays but also becomes a source of carbon X-rays. It is thus necessary to determine how much errors are induced by carbon coating, and how thick coating is allowed for the accurate measurement. In this study, quantitative analysis of carbon on silicon carbide with carbon coating films was attempted by electron probe microanalyzer. It was found that measured carbon content increased in a nonlinear manner up to 40% with a film thickness, whereas silicon content decreased slightly. Carbon X-ray intensity was determined by computer simulation, which increased in a linear manner with the thickness. The discrepancy was due to a nucleation and growth of islands and thus a change of density with a thickening of coating film.

In this study, bicrystals of silver (Ag) and aluminum (Al) were used to investigate the physical spatial resolution of the electron backscatter diffraction system combining a digital image correlation method. Furthermore, the effect of the accelerating voltage and probe current was investigated on the physical spatial resolution of the lateral and longitudinal resolutions for Ag and Al, respectively. The lateral and longitudinal resolutions show high dependency on the accelerating voltage for a low atomic mass material of Al, In addition, these are almost independent of the accelerating voltage for a high atomic mass material of Ag. Moreover, the probe current does not play any role on both the lateral and longitudinal resolutions. The best lateral resolutions for Al and Ag are 40.5 and 12.1 nm at 10 kV and 1 nA, respectively. The best longitudinal resolutions of 23.2 and 80 nm were obtained at 10 kV and 1 nA for Al and Ag, respectively.

ZK60 (Mg–Zn–Zr) alloys exhibited a variation in precipitates with aging, and their mechanical properties also changed. Microindentation tests were carried out on two types of ZK60 alloys of solid solution (T4) and peak aging (T6). Microstructure and texture evolution during indentation was investigated using electron backscatter diffraction. Twinning occurred near the indentation marks in most grains. It was found that tensile twinning was dominant, and two twin variants were usually observed. Texture and microstructure evolution by twinning and slip activation was further examined by uniaxial compression test with strain. The initial random orientation gradually changed into basal fibers with strain. Some grains with nonbasal orientations aligned with the loading direction easily underwent twinning followed by slip deformation. Other grains near basal orientations revealed only slip deformation.

A quantitative and automated phase analysis of dual-phase (DP) steel using electron backscatter diffraction (EBSD) was attempted. A ferrite–martensite DP microstructure was produced by intercritical annealing and quenching. An EBSD map of the microstructure was obtained and post-processed for phase discrimination. Band slope (BS), which was a measure of pattern quality, exhibited much stronger phase contrast than another conventional one, band contrast. Owing to high sensitivity to lattice defect and little orientation dependence, BS provided handiness in finding a threshold for phase discrimination. Its grain average gave a superior result on the discrimination and volume fraction measurement of the constituent phases in the DP steel.

In ferritic stainless steel (FSS), undesirable surface defects of ridging appear during deep drawing. The formation of these defects is attributed to the inhomogeneous distribution of orientations of individual grains. In the present work, a new electron backscattered diffraction R(α)-value map was introduced, and the dependence of the tensile directions on the formation of ridging in an FSS sheet was discussed using this map. The results showed that large grain colonies in the R(α)-value maps lead to the formation of severe ridging in an FSS sheet.

Cast AZ31B-H24 magnesium alloy, comprising Mg with 3.27 wt% Al and 0.96 wt% Zn, was cold rolled and subsequently annealed. Global texture evolutions in the specimens were observed by X-ray diffractometry after the thermomechanical processing. Image-based microstructure and texture for the deformed, recrystallized, and grown grains were observed by electron backscattered diffractometry. Recrystallized grains could be distinguished from deformed ones by analyzing grain orientation spread. Split basal texture of ca. ±10–15° in the rolling direction was observed in the cold-rolled sample. Recrystallized grains had widely spread basal poles at nucleation stage; strong {0001} basal texture developed with grain growth during annealing.

Two kinds of Sr2FeReO6 (SFRO) samples, pristine SFRO and Re-excess SFRO, were prepared and we visualized the local atomic structure in terms of cationic ordering in the prepared SFRO samples via high-angle annular dark-field (HAADF) scanning transmission electron microscopy (STEM). HAADF-STEM results demonstrated the high degree of cationic ordering maintains in both the pristine SFRO and Re-excess SFRO samples. On the other hand, defective structures such as antiphase boundary and Re-deficient phase were observed dominantly in the pristine SFRO, and thus the poor magnetic property in the pristine SFRO is attributed to those defective structures related with the frustrated Fe/Re ordering.

As the presence of Sc2O3 and CeO2 is known to largely enhance the ionic conductivity in the temperature range of 600–800°C, compared with the conventional yttria-stabilized ZrO2, Sc2O3&CeO2-stabilized ZrO2 provide its applicability as electrolytes in solid oxide fuel cells. The current study introduces the methodology to synthesize Sc2O3&CeO2-stabilized ZrO2 powders by using co-precipitation technique or high-temperature hydrothermal reaction, and further describes the structural characterization of the zirconia powders synthesized by the above-mentioned two methods. The co-precipitation technique was found to allow obtaining powders of cubic phase, whereas high-temperature hydrothermal synthesis results in the presence of a monoclinic phase as well. The scanning transmission electron microscope observations also confirm that the size of the synthesized ZrO2 powders in this study is found to be much smaller than that of commercially available powders.

Focused ion beam (FIB) milling using high-energy gallium ions is widely used in the preparation of specimens for transmission electron microscopy (TEM). However, the energetic ion beam induces amorphization on the edge of specimens during milling, resulting in a mischievous influence on the clearness of high-quality transmission electron micrographs. In this work, the amorphization induced by the FIB milling was investigated by TEM for three kinds of materials, metallic materials in bulk shape, and semiconductive and electronic ceramic materials as a substrate for the deposition of thin films.

We report the direct visualization of point defect clustering in {113} planes of silicon crystal using a transmission electron microscope, which was supported by structural modeling and high-resolution electron microscope image simulations. In the initial stage an accumulation of nonbonded interstitial–vacancy (I–V) pairs stacked at a distance of 7.68 Å along neighboring atomic chains located on the {113} plane takes place. Further broadening of the {113} defect across its plane is due to the formation of planar fourfold coordinated defects (FFCDs) perpendicular to chains accumulating I–V pairs. Closely packed FFCDs create a sequence of eightfold rings in the {113} plane, providing sites for additional interstitials. As a result, the perfect interstitial chains are built on the {113} plane to create an equilibrium structure. Self-ordering of point defects driven by their nonisotropic strain fields is assumed to be the main force for point defect clustering in the {113} plane under the existence of an energy barrier for their recombination.

In situ transmission electron microscopy was performed on the electromigration in platinum (Pt) nanowires (14 nm thick, 200 nm wide, and 300 nm long) with and without feedback control. Using the feedback control mode, symmetric electrodes are obtained and the gap usually forms at the center of the Pt nanowire. Without feedback control, asymmetric electrodes are formed, and the gap can occur at any position along the wire. The three-dimensional gap geometries of the electrodes in the Pt nanowire were determined using high-angle annular dark-field scanning transmission electron microscopy; the thickness of the nanowire is reduced from 14 nm to only a few atoms at the edge with a gap of about 5–10 nm.

We investigated the microstructural evolution of Sn96.4Ag2.8Cu0.8 solder through in situ heating transmission electron microscopy observations. As-soldered bump consisted of seven layers, containing the nanoeutectic lamella structure of AuSn and Au5Sn phases, and the polygonal grains of AuSn2 and AuSn4, on Au-plated Cu bond pads. Here, we found that there are two nanoeutectic lamellar layers with lamella spacing of 40 and 250 nm. By in situ heating above 140°C, the nanoeutectic lamella of AuSn and Au5Sn was decomposed with structural degradation by sphering and coarsening processes of the lamellar interface. At the third layer neighboring to the lamella layer, on the other hand, Au5Sn particles with a zig-zag shape in AuSn matrix became spherical and were finally dissipated in order to minimize the interface energy between two phases. In the other layers except both lamella layers, polycrystal grains of AuSn2 and AuSn4 grew by normal grain growth during in situ heating. The high interface energy of nanoeutectic lamella and polygonal nanograins, which are formed by rapid solidification, acted as a principal driving force on the microstructural change during the in situ heating.

The charging effects of microfibrils of sciatic nerve tissues due to electron irradiation are investigated using electron holography. The phenomenon that the charging effects are enhanced with an increase of electron intensity is visualized through direct observations of the electric potential distribution around the specimen. The electric potential at the surface of the specimen could be quantitatively evaluated by simulation, which takes into account the reference wave modulation due to the long-range electric field.

Distribution of wax in laser printer toner was observed using an ultra-high-voltage (UHV) and a medium-voltage transmission electron microscope (TEM). As the radius of the wax spans a hundred to greater than a thousand nanometers, its three-dimensional recognition via TEM requires large depth of focus (DOF) for a volumetric specimen. A tomogram with a series of the captured images would allow the determination of their spatial distribution. In this study, bright-field (BF) images acquired with UHV-TEM at a high tilt angle prevented the construction of the tomogram. Conversely, the Z-contrast images acquired by the medium-voltage TEM produced a successful tomogram. The spatial resolution for both is discussed, illustrating that the image degradation was primarily caused by beam divergence of the Z-contrast image and the combination of DOF and chromatic aberration of the BF image from the UHV-TEM.

Precipitates in two X80 pipeline steels were studied by transmission electron microscopy equipped with an energy filtering system. The steels are microalloyed with niobium and niobium–vanadium (Nb–V), respectively, and produced by continuous hot rolling. Besides the precipitates TiN and (Ti, Nb) (C, N), which were 10–100 nm in size, a large number of precipitates smaller than 10 nm distributed in the two steels have been observed. In the Nb–V microalloyed steel, only a few titanium nitrides covered by vanadium compounds on the surface have been observed. It is inferred that the vanadium exists mainly in the matrix as a solid solution element. The fact has been accepted that there was no contribution to the precipitation strengthening of the X80 steel by adding 0.04–0.06% vanadium under the present production process. By contrast, the toughness of the Nb–V steel is deteriorated. Therefore, a better toughness property of the Nb microalloyed X80 results from the optimum microalloying composition design and the suitable accelerating cooling after hot rolling.

In this study, every effort was exerted to determine and accumulate data to correlate microstructural and compositional elements in ultra-low-carbon (ULC) steels to variation of carbon content (12–44 ppm), manganese (0.18–0.36%), and sulfur (0.0066–0.001%). Quantitative analysis of the ULC steel using optical microscope, scanning electron microscope, transmission electron microscope, and three-dimensional atom probe revealed the decrease of grain size and dislocation density with the increase of carbon contents and/or increase of the final delivery temperature. For a given carbon content, the grain interior carbon concentration increases as the grain size increases.

The technological development of all kinds of lightweight transportation devices including vehicles, aircraft, ships, etc. has progressed markedly with the demand for energy saving and environmental protection. Aluminum alloy is in the spotlight as it is a suitable environmentally friendly material. However, deformation is a major problem during the welding process because aluminum alloy has a large thermal expansion coefficient. In addition, it is known that its corrosion resistance is excellent; nevertheless, in practice, considerable corrosion is generated and this is a major problem. To solve this problem, the friction stir welding (FSW) technology is applied extensively at various industrial fields as a new welding technique. This method involves a process in which materials are joined by frictional heat and physical force. Therefore, we evaluated improvements in mechanical properties and corrosion resistance through annealing heat treatment after FSW. The electrochemical experiment did not show a significant difference. However, the microstructure observation showed defectless, fine crystal particles, indicating excellent properties at 200–225°C.

In this study, we replaced the expensive blade material with an aluminum–bronze alloy that has excellent corrosion resistance and cavitation characteristics and developed the corrosion protection method to improve durability using an electrochemical method. The objective of this study was to identify the electrochemical corrosion protection conditions to minimize cavitation damage due to generating hydrogen gas (2H2O + 2e− → 2OH− + H2) by means of hydrogen overvoltage before the impact pressure of the cavity is transferred to the surface. In the constant potential experiment under the cavitation environment, the energy was reflected or cancelled out by collision of the cavities with the hydrogen gas generated by the hydrogen overvoltage. As a result, the optimal corrosion prevention potential in the dynamic state is assumed to be the range of −1.4 to −1.7 V, which is the range at which active polarization took place.

Scale-bridging analysis on deformation behavior of high-nitrogen austenitic Fe–18Cr–10Mn–(0.39 and 0.69)N steels was performed by neutron diffraction, electron backscattered diffraction (EBSD), and transmission electron microscopy (TEM). Two important modes of deformation were identified depending on the nitrogen content: deformation twinning in the 0.69 N alloy and strain-induced martensitic transformation in the 0.39 N alloy. The phase fraction and deformation faulting probabilities were evaluated based on analyses of peak shift and asymmetry of neutron diffraction profiles. Semi in situ EBSD measurement was performed to investigate the orientation dependence of deformation microstructure and it showed that the variants of ε martensite as well as twin showed strong orientation dependence with respect to tensile axis. TEM observation showed that deformation twin with a {111}⟨112⟩ crystallographic component was predominant in the 0.69 N alloy whereas two types of strain-induced martensites (ε and α′ martensites) were observed in the 0.39 N alloy. It can be concluded that scale-bridging analysis using neutron diffraction, EBSD, and TEM can yield a comprehensive understanding of the deformation mechanism of nitrogen-alloyed austenitic steels.

Band contrast (BC) is a qualitative measure of electron back-scattered diffraction (EBSD), which is derived from the intensity of the Kikuchi bands. The BC is dependent upon several factors including scanning electron microscope measurement parameters, EBSD camera setup, and the specimen itself (lattice defect and grain orientation). In this study, the effective factors for BC variations and the feasibility of using BC variations for the quantification of microstructure evolutions have been investigated. In addition, the effects of the lattice defect and the grain orientation on the BC variations are studied. Next, a shear-deformed microstructure of 316L stainless steel, which contains nanosized grains and a large portion of twin boundaries, is revealed by BC map and histogram. Recovery and recrystallization of shear-deformed 316L stainless steel are displayed by BC variations during isothermal annealing at 700 and 800°C, respectively. It is observed that the BC turns bright as the shear-deformed crystal structure is recovered or recrystallized.