The recent development of electron-sensitive and pixelated detectors has attracted the use of four-dimensional scanning transmission electron microscopy (4D-STEM). Here, we present a precession electron diffraction-assisted 4D-STEM technique for automated orientation mapping using diffraction spot patterns directly captured by an in-column scintillator-based complementary metal-oxide-semiconductor (CMOS) detector. We compare the results to a conventional approach, which utilizes a fluorescent screen filmed by an external charge charge-coupled device camera. The high-dynamic range and signal-to-noise characteristics of the detector greatly improve the image quality of the diffraction patterns, especially the visibility of diffraction spots at high scattering angles. In the orientation maps reconstructed via the template matching process, the CMOS data yield a significant reduction of false indexing and higher reliability compared to the conventional approach. The angular resolution of misorientation measurement could also be improved by masking reflections close to the direct beam. This is because the orientation sensitive, weak, and small diffraction spots at high scattering angles are more significant. The results show that fine details, such as nanograins, nanotwins, and sub-grain boundaries, can be resolved with a sub-degree angular resolution which is comparable to orientation mapping using Kikuchi diffraction patterns.

Regarding the effect of composition on the mechanical properties of intermetallic phases such as Laves phases, there is conflicting information in the literature. Some authors observed defect hardening when deviating from stoichiometric Laves phase composition, whereas others find defect softening. Here, we present a systematic investigation of the defect state, hardness, and elastic modulus of cubic and hexagonal NbCo2 Laves phases as a function of crystal structure and composition. For this purpose, diffusion couples were prepared which exhibit diffusion layers of the cubic C15 and hexagonal C14 and C36 NbCo2 Laves phases, with concentration gradients covering their entire homogeneity ranges from 24 to 37 at.% Nb. Direct observations of dislocations and stacking faults in the diffusion layers as a function of composition were performed by electron channeling contrast imaging, and the hardness and elastic modulus were probed in the diffusion layers along the concentration gradients by nanoindentation.

In situ nanomechanical testing provides critical insight into the fundamental processes that lead to deformation phenomena in materials. Often, in situ tests are performed in relevant conditions such as high or low temperatures, tribological contact, gas environments, or under radiation exposure. Modern diffraction and imaging methods of materials under load provide high spatial resolution and enable extraction of quantitative mechanical data from local microstructure components or nano-sized objects. The articles in this issue cover recent advances in different types of in situ nanomechanical testing methods, spanning from dedicated nanomechanical testing platforms and microelectromechanical systems devices to deformation analyses via in situ diffraction and imaging methods. This includes scanning electron microscopy, advanced scanning transmission electron microscopy, electron diffraction, x-ray diffraction, and synchrotron techniques. Emerging areas such as in situ tribology enable novel insights into the origin of deformation mechanisms, while the evolution of microelectromechanical systems for controlled in situ testing provide opportunities for advanced control and loading strategies. Discussion on the current state of the art for in situ nanomechanical testing and future opportunities in imaging, strain sensing, and testing environments are also addressed.

Hydrogen exposure has been found to result in metal embrittlement. In this work, we use nanoindentation to study the mechanical properties of polycrystalline tungsten subjected to deuterium plasma exposure. For the purpose of comparison, nanoindentation tests on exposed and unexposed reference tungsten were carried out. The results exhibit a decrease in the pop-in load and an increase in hardness on the exposed tungsten sample after deuterium exposure. No significant influence of grain orientation on the pop-in load was observed. After a desorption time of td ≥ 168 h, both the pop-in load and hardness exhibit a recovering trend toward the reference state without deuterium exposure. The decrease of pop-in load is explained using the defactant theory, which suggests that the presence of deuterium facilitates the dislocation nucleation. The increase of hardness is discussed based on two possible mechanisms of the defactant theory and hydrogen pinning of dislocations.

Besides the high spatial resolution achieved in aberration-corrected scanning transmission microscopy, beam-induced dynamic effects have to be considered for quantitative chemical characterization on the level of single atomic columns. The present study investigates the influence of imaging conditions in an aberration-corrected scanning transmission electron microscope on the beam-induced atomic migration at a complex Ag-segregated, nanofaceted Cu grain boundary. Three distinct imaging conditions including static single image and serial image acquisition have been utilized. Chemical information on the Ag column occupation of single atomic columns at the grain boundary was extracted by the evolution of peak intensity ratios and compared to idealized scanning transmission electron microscopy image simulations. The atomic column occupation is underestimated when using conventional single frame acquisition due to an averaging of Ag atomic migration events during acquisition. Possible migration paths for the beam-induced atomic motion at a complex Cu grain boundary are presented.

In this study, the interfacial adhesion of Cu and TiN on an annealed borophosphosilicate glass (BPSG) in a multilayer material stack was investigated. The two material systems, Cu/BPSG and TiN/BPSG, are representatives for weak and strong interfaces, respectively. A weak and a strong interface was chosen to identify possible differences in the fracture path selection for the multilayer material systems. To investigate this, in situ 4-point-bending experiments were performed under an optical microscope and in a scanning electron microscope. Complementary ex situ 4-point-bending experiments were carried out on the identical material systems. These tests revealed that for the two analyzed systems there is a large discrepancy in the success rate of failure along the interface of interest, which is a prerequisite for determining the corresponding interface energy release rate. This phenomenon can be understood by using theoretical findings of earlier studies reported in the literature, which are in agreement with the experimental outcome of the in situ 4-point-bending measurements presented here.

Fracture toughness testing of materials at the micrometer scale has become essential due to the continuing miniaturization of devices accompanied by findings of size effects in fracture behavior. Many techniques have emerged in the recent past to carry out fracture toughness measurements at the relevant micro and nanolength scales, but they lack ASTM standards that are prescribed for bulk scale tests. Also, differences in reported values arise at the microscale due to the sample preparation technique, test method, geometry, and investigator. To correct for such discrepancies, we chose four different fracture toughness test geometries in practice, all of them micromachined in the focused ion beam (FIB), to investigate the fracture toughness of Si(100) at the micrometer scale. The average KIC that emerges from all four cases is a constant (0.8 MPa m1/2). The advantages and limitations of each of these geometries in terms of test parameters and the range of materials that can be tested are discussed.

In this paper, the physical metallurgy and properties of a novel family of high-strength γ-TiAl-based alloys is reviewed succinctly. These so-called TNM™ alloys contain Nb and Mo additions in the range of 3 - 7 atomic percent as well as small additions of B and C. For the definition of the alloy composition thermodynamic calculations using the CALPHAD method were conducted. The predicted phase transformation and ordering temperatures were verified by differential scanning calorimetry and in situ high-energy X-ray diffraction. TNM alloys solidify via the β-phase and exhibit an adjustable β-phase volume fraction at temperatures, where hot-working processes are performed. Due to the high volume fraction of β-phase these alloys can be processed isothermally as well as under near conventional conditions. In order to study the occurring deformation and recrystallization processes during hot-working, in situ diffraction experiments were conducted during compression tests at elevated temperatures. With subsequent heat-treatments a significant reduction of the β-phase is achieved. These outstanding features of TNM alloys distinguish them from other TiAl alloys which must exclusively be processed under isothermal conditions and/or which always exhibit a high fraction of β-phase at service temperature. After hot-working and multi-step heat-treatments, these alloys show yield strength levels > 800 MPa at room temperature and also good creep resistance at elevated temperatures.

The spatial resolution of the transmission electron microscope makes it an ideal environment in which to continuously track the real-time response of a system to an external stimulus and to discover and quantify the rate-limiting fundamental microscopic processes and mechanisms governing the macroscopic properties. Advances in instrumentation, stage design, recording media, computational power, and image manipulation software are providing new opportunities for not only observing the microscopic mechanisms but also measuring concurrently the macroscopic response. In this article, the capability of this technique as applied to mechanical properties of materials is highlighted.

In this study a two-step heat treatment was applied to high Nb containing γ-TiAl based alloys in order to investigate the initial stage of the lamellae formation in ordered α2-grains as well as in massively transformed γm-grains. The first heat treatment step, conducted in the single α-phase field followed by oil quenching, leads to a microstructure consisting of supersaturated α2-grains and a small volume fraction of γm-grains. The second step of the heat treatment was performed below the eutectoid temperature, i.e. within the (α2+γ)-phase field region and was again followed by oil quenching. There, the formation of ultra-fine γ-lamellae takes place in the α2-grains and (some) fine α2-lamellae are formed in the γm-grains. In both cases the lamellae show a Blackburn orientation relationship with the matrix grain. It was found that the precipitation of γ-laths in the supersaturated α2-grains is faster than the formation of α2-laths in γm-grains. The characteristics of the initial stage of formation were investigated by transmission electron microscopy.

To investigate the origin of the high strength of thin films, in-situ cross-sectional TEM deformation experiments have been performed on several metallic films attached to rigid substrates. Thermal cycles, comparable to those performed using laser reflectometry, were applied to thin foils inside the TEM and dislocation motion was recorded dynamically on video. These observations can be directly compared to the current models of dislocation hardening in thin films. As expected, the role of interfaces is crucial, but, depending on their nature, they can attract or repel dislocations. When the film/interface holds off dislocations, experimental values of film stress match those predicted by the Nix-Freund model. In contrast, the attracting case leads to higher stresses that are not explained by this model. Two possible hardening scenarios are explored here. The first one assumes that the dislocation/interface attraction reduces dislocation mobility and thus increases the yield stress of the film. The second one focuses on the lack of dislocation nucleation processes in the case of attracting interfaces, even though a few sources have been observed in-situ.

The wafer curvature technique was used to analyze stresses in fine-grained, 50 nm to 2 μm thick Au films on silicon substrates between room temperature and 500°C. The microstructural evolution was analyzed by scanning electron microscopy (SEM), focused ion beam (FIB) microscopy and transmission electron microscopy (TEM). In situ heating experiments inside a scanning electron microscope provided a comparison between the morphological development and the stress-temperature behavior of the film. Hillock formation was observed, but it can only partially account for the stress relaxation measured by the wafer curvature technique.

When confronted by severe geometric constraints, dislocations may respond in unforeseen ways. One example of such unexpected behavior is parallel glide in unpassivated, ultrathin (200 nm and thinner) metal films. This involves the glide of dislocations parallel to and very near the film/substrate interface, following their emission from grain boundaries. In situ transmission electron microscopy reveals that this mechanism dominates the thermomechanical behavior of ultrathin, unpassivated copper films. However, according to Schmid's law, the biaxial film stress that evolves during thermal cycling does not generate a resolved shear stress parallel to the film/substrate interface and therefore should not drive such motion. Instead, it is proposed that the observed dislocations are generated as a result of atomic diffusion into the grain boundaries. This provides experimental support for the constrained diffusional creep model of Gao et al.[1], in which they described the diffusional exchange of atoms between the unpassivated film surface and grain boundaries at high temperatures, a process that can locally relax the film stress near those boundaries. In the grains where it is observed, parallel glide can account for the plastic strain generated within a film during thermal cycling. One feature of this mechanism at the nanoscale is that, as grain size decreases, eventually a single dislocation suffices to mediate plasticity in an entire grain during thermal cycling. Parallel glide is a new example of the interactions between dislocations and the surface/interface, which are likely to increase in importance during the persistent miniaturization of thin film geometries.

In this study of thin film plasticity, the relationship between thermomechanical behavior and dislocation motion has been investigated in copper constrained by a silicon substrate. The stress-temperature behavior as determined from wafer curvature experiments has been directly compared to deformation microstructures observed during in situ thermal cycling of plan-view specimens in the transmission electron microscope. The flow stress of copper films with thicknesses ranging from 100 nm to 400 nm was found to be constant, indicating that strengthening mechanisms may be saturated in this thickness regime. Moreover, unexpected dislocation glide on a plane parallel to the film surface, which should experience no resolved shear stress, provides potential evidence for the occurrence of constrained diffusional creep in a 270 nm film.

In situ transmission electron microscopy has been utilized to study dislocation plasticity in a 200 nm thick copper film. The behavior of dislocations in a [111]-oriented grain was recorded during a thermal cycle. During cooling, it was observed that dislocations were emitted from a grain boundary triple junction in regular intervals of 30°C to 40°C. Subsequent glide occurred on a (111) plane parallel to the film surface, despite the expectation of zero resolved shear stress on such planes. The initial emitted dislocations remained close to the triple junction, avoiding contact with another [111] grain rotated by 17°. Glide into the opposite end of the grain was initiated only after the injection of several additional dislocations, which induced strong curvature in all dislocations near the active triple junction. Post mortem examination of dislocation curvature revealed that an inhomogeneous stress state existed within the grain.

The influence of Si on the microstrucure of Ti-Si-N coatings was studied, since it controls the mechanical properties of the coatings. At low Si-contents columnar {111}-textured TiN grains form. Increasin the Si-content to >4at% causes a transition to equiaxed {200}-textured TiN grains. The equiaxed TiN grains reveal grain diameters of ∼6 nm for coatings containing 11 at% Si.

γ-T1AI (Cr, Mo, Si, B) specimens with two different fine lamellar microstructures were produced by vacuum arc melting followed by a two-stage heat treatment. The average lamellar spacing was determined to be 200 nm and 25–50 nm, respectively. Creep tests at 700°C showed a very strong primary creep for both samples. After annealing for 24 hours at 1000 °C the primary creep for both materials is significantly decreased. The steady-state creep for the specimens with the wider lamellar spacing appears to be similar to the creep behavior prior to annealing while the creep rate of the material with the previously smaller lamellar spacing is significantly higher. Optical microscopy and TEM-studies show that the microstructure of the specimens with the wider lamellar specing is nearly unchanged, whereas the previously finer material was completely recrystallized to a globular microstructure with a low creep resistance. The dissolution of the fine lamellar microstructure was also observed during creep tests at 800 °C as manifested in an acceleration of the creep rate. It is concluded that extremely fine lamellar microstructures come along with a very high dislocation density and internal stresses which causes the observed high primary creep. The microstructure has a composition far away from the thermodynamical equilibrium which leads to a dissolution of the structure even at relatively low temperatures close to the intended operating temperature of γ-T1AI structural parts. As a consequence this limits the benefit of fine lamellar microstructures on the creep behavior.