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Tungsten-copper composites are used in harsh environments because of their superior material properties. This work addresses a tungsten-copper composite made of 20 wt.% copper, which was subjected to grain refinement by high-pressure torsion, whereby the deformation temperature was varied between room temperature and 400 °C to tailor the grain size. Deformation was performed up to microstructural saturation and verified by hardness measurement and scanning electron microscopy. From the refined nanostructured material, micro-cantilever bending beams with cross-sections spanning from 5 × 5 to 35 × 35 µm2 were cut to examine possible size effects and the grain size influence on the fracture behavior. Fracture experiments were performed in situ inside a scanning electron microscope by applying a quasi-static loading protocol with partial unloading steps. Inspection of the fracture surfaces showed that all cantilevers failed in an inter-crystalline fashion. Nevertheless, remaining coarser tungsten grains impacted the resultant fracture toughness and morphology. Cantilevers fabricated from the 400 °C specimen exhibited a fracture toughness of 220 ± 50 J m 2 . For the room temperature cantilevers, a fracture toughness of 410 ± 50 J m 2 was observed, which declined to 340 ± 30 J m 2 for cantilevers < 10 × 10 µm2, confirming a size effect. The increased fracture toughness is attributed to the delamination-like structures formed in the room temperature sample. [ABSTRACT FROM AUTHOR]

An in situ hydrogen (H) plasma charging and in situ observation method was developed to continuously charge materials, while tensile testing them inside a scanning electron microscope (SEM). The present work will introduce and validate the setup and showcase an application allowing high-resolution observation of H-material interactions in a Ni-based alloy, Alloy 718. The effect of charging time and pre-straining was investigated. Fracture surface observation showed the expected ductile microvoid coalescence behavior in the uncharged samples, while the charged ones displayed brittle intergranular and quasi-cleavage failure. With the in situ images, it was possible to monitor the sample deformation and correlate the different crack propagation rates with the load-elongation curves. H-charging reduced the material ductility, while increasing pre-strain decreased hydrogen embrittlement susceptibility due to the possible suppression of mechanical twinning during the tensile test and, therefore, a reduction in H concentration at grain and twin boundaries. All the presented results demonstrated the validity of the method and the possibility of in situ continuously charging of materials with H without presenting any technical risk for the SEM. [ABSTRACT FROM AUTHOR]

The ability to increase the thermal stability of protective coatings under work load gives rise to scientific and industrial interest in age hardening of complex nitride coating systems such as ceramic-like Ti1-xAlxN. However, the decomposition pathway of these systems from single-phase cubic to the thermodynamically stable binary nitrides (cubic TiN and wurtzite AlN), which are essential for age hardening, are not yet fully understood. In particular, the role of decomposition kinetics still requires more detailed investigation. In the present work, the combined effect of annealing time and temperature upon the nano-structural development of Ti0.46Al0.54N thin films is studied, with a thermal exposure of either 1 min or 120 min in 100 °C steps from 500 °C to 1400 °C. The impact of chemical changes at the atomic scale on the development of micro-strain and mechanical properties is studied by post-annealing investigations using X-ray diffraction, nanoindentation, 3D-atom probe tomography and high-resolution transmission electron microscopy. The results clearly demonstrate that the spinodal decomposition process, triggering the increase of micro-strain and hardness, although taking place throughout the entire volume, is enhanced at high diffusivity paths such as grain or column boundaries and followed within the grains. Ab initio calculations further show that the early stages of wurtzite AlN precipitation are connected with increased strain formation, which is in excellent agreement with experimental observations. [ABSTRACT FROM AUTHOR]

The maximum actuation frequency of magnetic shape-memory alloys (MSMAs) significantly increases with decreasing size of the transducer making MSMAs interesting candidates for small scale actuator applications. To study the mechanical properties of Ni–Mn–Ga single crystals on small length scales, two single-domain micropillars with dimensions of 10×15×30 μm3 were fabricated from a Ni–Mn–Ga monocrystal using dual beam focused ion beam machining. The pillars were oriented such that the crystallographic c direction was perpendicular to the loading direction. The pillars were compressed to maximum stresses of 350 and 50 MPa, respectively. Atomic force microscopy and magnetic force microscopy were performed prior to fabrication of the pillars and following the deformation experiments. Both micropillars were deformed by twinning as evidenced by the stress-strain curve. For one pillar, a permanent deformation of 3.6% was observed and ac twins (10M martensite) were identified after unloading. For the other pillar, only 0.7% remained upon unloading. No twins were found in this pillar after unloading. The recovery of deformation is discussed in the light of pseudoelastic twinning and twin-substrate interaction. The twinning stress was higher than in similar macroscopic material. However, further studies are needed to substantiate a size effect. [ABSTRACT FROM AUTHOR]

Modern nanoindentation devices are capable of dynamic experimentations, which allow us to exploit instrumented hardness tests extensively. Beside the assets of recording mechanical properties continuously over displacement, there are ongoing debates whether the superimposed force alters the material’s hardness. We will show for a broad range of materials that significant hardness differences are noted between dynamic and static tests, even for large displacements. Those mainly result from a changing indentation strain-rate during the hold segment at peak load. This fact must be implicitly considered in studies using static indentation tests to guarantee comparability of obtained nanoindentation hardness values and derived quantities. IMPACT STATEMENT A mismatch between static and dynamic nanoindentation hardness has been identified to result from strain-rate deviations during hold segments in static nanoindentation tests, in particular affecting rate-sensitive materials. [ABSTRACT FROM PUBLISHER]

Driven by the ongoing miniaturization and increasing integration in microelectronics devices, very thin metallic films became ever more important in recent years. Accordingly also the capability of determining specific physical and mechanical properties of such arrangements gained increasing importance. Miniaturized testing methods to evaluate, for example, the mechanical properties of thin metallic multilayers are therefore indispensable. A novel in-situ micromechanical approach is examined in the current study and compared to existing methods regarding their capability to determine the interface toughness of specific interfaces in multilayer configurations. Namely, sputter deposited copper and tungsten thin films with a thickness of approx. 500nmon a stress-free silicon (100) substrate are investigated. The multilayer stacks consist of different materials that vary in microstructure, elastic properties and residual stress state. We examine the interface toughness via double cantilever beam tests, nanoindentation and novel miniaturized shear tests. The choice of a proper test method is indispensable when addressing strong interfaces, such as the W-Cu interface, in the presence of weaker ones. Finally, it is demonstrated that miniaturized shear testing is a very promising approach to test such strong interfaces as the interface of interest to fail is predefined by the sample geometry. [ABSTRACT FROM AUTHOR]

Metallic thin films are widely used and relied upon for various technologies. Direct measurements of fracture toughness are rare for metallic thin films and existing methods for obtaining these measurements often do not provide characterization of the cracking process for determination of crack growth mechanisms. To rectify this, we explore a new technique which utilizes doubly clamped, in-situ three-point bend testing of micro-scale and nano-scale specimens. This is done by in-situ scanning electron microscopy (SEM) and transmission electron microscopy (TEM) mechanical testing for specimens with thicknesses of 2500 nm (SEM), 500 nm (SEM) and 100 nm (TEM). For in-situ TEM, a novel notching method is employed using the converged electron beam which achieves a notch radius of approximately 5 nm. Additionally, we present supporting characterization using Electron Backscatter Diffraction (EBSD) for 2500 nm thick specimens as a demonstration of the potential of this technique for understanding local deformation. Analysis of the acquired data presents several issues that require addressing, and recommendations for future improvements are given. [ABSTRACT FROM AUTHOR]

Small specimen testing techniques have a long history in nuclear material research due to the limitations posed by nuclear facilities. The limited space in reactors and the fact that the samples are oftentimes radioactive in addition to the increasing need to obtain mechanical properties from ion beam irradiated samples require small specimen mechanical testing. With the application of modern focused ion beam sample preparation techniques and the enhancement of nanoindentation instruments, the size scale has been moved to even smaller scales and new geometries. Micrometer and even nanometer size samples are feasible, but raise the question of comparability to large scale properties for engineering applications. In this review, we summarize available small scale materials testing techniques and potential shortcomings based on examples from the literature, as well as introduce novel experimental approaches conducted using microcompression testing, microbend bar testing, and nanoindentation at ambient and nonambient conditions. [ABSTRACT FROM PUBLISHER]

Theories of small-scale plasticity often invoke effects of strain gradient, and this is best tested by comparison of experimental stress–strain data obtained with and without well defined strain gradients. We provide new results to add to the body of data for 25–150-µm Cu wires in tension, 10–125-µm Cu and Ni foils in flexure and 10–125-µm Ni foils in tension, and test whether the data can adequately discriminate between the theories. What the collected data shows is that there are size effects in yield strain, as well as in the strain-hardening behaviour in the low-strain and high-strain regimes. Within the experimental scatter, the data is largely consistent with theories that invoke, and those that do not invoke, effects of strain gradients. The tension data in particular are too scattered, and the differences in the theoretical predictions are not sufficiently stark, to discriminate between the theories. However, we find that the flexure data for Cu and Ni agree within experimental error, indicating that material-specific properties such as elastic moduli and stacking fault energies are not involved in the size effect. [ABSTRACT FROM AUTHOR]

The effect of focused ion beam (FIB) fabrication on the mechanical properties of miniaturized mechanical tests has recently been realized, but is not well documented. In this study, the effect of post thermal annealing on the plastic properties of FIB fabricated micro- and nanometer-sized Cu samples was studied by means of advanced analytic and in situ transmission electron microscopy. In situ heating experiments on thin films and pillars revealed a reduction of the initially high dislocation density, but never a recovery of the bulk dislocation density. Aberration-corrected atomic imaging documented the recovery of a pristine crystalline surface structure upon annealing, while electron energy-loss spectroscopy showed that the remaining contamination layer consisted of amorphous carbon. These structural observations were combined with the mechanical data from in situ tests of annealed micro- and nanometer-sized tensile and compression samples. The thermal annealing in the micron regime mainly influences the initial yield point, as it reduces the number of suited dislocation sources, while the flow behavior is mostly unaffected. For the submicron samples, the annealed material sustains significantly higher stresses throughout the deformation. This is explained by the high stresses required for surface-mediated dislocation nucleation of the annealed material at the nanoscale. In the present case, the FIB affected the surface near defects and facilitated dislocation nucleation, thereby lowering the material strength. [ABSTRACT FROM AUTHOR]

Increasing demand for energy and reduction of carbon dioxide emissions has revived interest in nuclear energy. Designing materials for radiation environments necessitates a fundamental understanding of how radiation-induced defects alter mechanical properties. Ion beams create radiation damage efficiently without material activation, but their limited penetration depth requires small-scale testing. However, strength measurements of nanoscale irradiated specimens have not been previously performed. Here we show that yield strengths approaching macroscopic values are measured from irradiated ~400?nm-diameter copper specimens. Quantitative in situ nanocompression testing in a transmission electron microscope reveals that the strength of larger samples is controlled by dislocation-irradiation defect interactions, yielding size-independent strengths. Below ~400?nm, size-dependent strength results from dislocation source limitation. This transition length-scale should be universal, but depends on material and irradiation conditions. We conclude that for irradiated copper, and presumably related materials, nanoscale in situ testing can determine bulk-like yield strengths and simultaneously identify deformation mechanisms. [ABSTRACT FROM AUTHOR]

The morphology and microstructure of Al2O3 thin films deposited by pulsed direct current magnetron sputtering were studied in the as-grown state and after vacuum annealing at 1000 °C for 12 h using transmission electron microscopy. For the coating deposited under low ion bombardment conditions, the film consists of small γ- and/or δ-Al2O3 grains embedded in an amorphous matrix. The grain size at the region close to the interface to the substrate was much larger than that of the remaining layer. Growth of the γ-Al2O3 phase is promoted during annealing but no transformation to α-Al2O3 was detected. For high-energetic growth conditions, clear evidence for γ-Al2O3 formation was found in the upper part of the coating with grain size much larger than for low-energetic growth, but the film was predominately amorphous at the interface region. Annealing resulted in the transformation of γ-Al2O3 to α-Al2O3, while the mainly amorphous part crystallized to γ-Al2O3. [ABSTRACT FROM AUTHOR]

Synchrotron X-ray microdiffraction was used to characterize the deformation structure of single crystalline Cu micro-tensile specimens which were oriented for single slip. The 3-µm thick samples were strained in situ in a scanning electron microscope (SEM). Electron microscopy observations revealed glide steps at the surface indicating single slip. While the slip steps at the surface must have formed by the predominant activation of the primary glide system, analysis of Laue peak streaking directions revealed that, even at low strains, dislocations had been activated and stored on an unpredicted slip system. Furthermore, the µLaue scans showed that multiple slip takes over at a later state of deformation. [ABSTRACT FROM AUTHOR]

For a better mechanistic understanding of the deformation phenomena that occur during nanoindentation testing, complimentary experimental techniques are critical. This overview presents several methods capable of analyzing the local microstructure of materials undergoing nanoindentation across different length scales, including etch pit analysis, electron backscatter diffraction, and in situ nanoindentation in a transmission electron microscope. Case studies of deformation mechanisms are provided, and the benefits and limitations of these complimentary experimental techniques are discussed. [ABSTRACT FROM AUTHOR]

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This article discusses crystal rotations in micro-compressed single copper columns that are dislocation-induced. Although flow stress of such single crystal compression samples has been found to be size dependent through the use of a focused ion beam, no model has been proposed to explain this unusual behavior. Experiments with dislocation starvation, surface image stresses, and consideration of stochastic single-ended dislocation sources have also failed to develop a model. This study applies an in situ set-up for the loading experiments and, subsequently, local crystal orientation of the deformed samples is analyzed by electron backscatter diffraction to examine the microstructural development.

In situ microdiffraction experiments were conducted on focused ion beam machined single crystal Cu pillars oriented for double slip. During deformation, the crystal undergoes lattice rotation on both the primary and critical slip system. In spite of the initial homogeneous microstructure of the Cu pillar, rotation sets in already at yield and is more important at the top of the pillar than at the bottom, demonstrating the inhomogeneous stress state during a microcompression experiment. The rotation results are confirmed by electron backscatter diffraction measurements. [ABSTRACT FROM AUTHOR]

Extended abstract of a paper presented at Microscopy and Microanalysis 2012 in Phoenix, Arizona, USA, July 29 – August 2, 2012. [ABSTRACT FROM PUBLISHER]

Extended abstract of a paper presented at Microscopy and Microanalysis 2012 in Phoenix, Arizona, USA, July 29 – August 2, 2012. [ABSTRACT FROM AUTHOR]

Extended abstract of a paper presented at Microscopy and Microanalysis 2010 in Portland, Oregon, USA, August 1 – August 5, 2010. [ABSTRACT FROM PUBLISHER]