Zaoli Zhang

Advanced nanomechanics in the TEM: Effects of thermal annealing on FIB prepared Cu samples

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.

The peculiarity of the metal-ceramic interface

Important properties of materials are strongly influenced or controlled by the presence of solid interfaces, i.e. from the atomic arrangement in a region which is a few atomic spacing wide. Using the quantitative analysis of atom column positions enabled by CS-corrected transmission electron microscopy and theoretical calculations, atom behaviors at and adjacent to the interface was carefully explored. A regular variation of Cu interplanar spacing at a representative metal-ceramic interface was experimentally revealed, i.e. Cu-MgO (001). We also found the periodic fluctuations of the Cu and Mg atomic positions triggered by the interfacial geometrical misfit dislocations, which are partially verified by theoretical calculations using empirical potential approach. Direct measurements of the bond length of Cu-O at the coherent regions of the interface showed close correspondence with theoretical results. By successively imaging of geometrical misfit dislocations at different crystallographic directions, the strain fields around the interfacial geometrical misfit dislocation are quantitatively demonstrated at a nearly three-dimensional view. A quantitative evaluation between the measured and calculated strain fields using simplified model around the geometrical misfit dislocation is shown.

Fracture toughness and structural evolution in the TiAlN system upon annealing

Hard coatings used to protect engineering components from external loads and harsh environments should ideally be strong and tough. Here we study the fracture toughness, KIC, of Ti1−xAlxN upon annealing by employing micro-fracture experiments on freestanding films. We found that KIC increases by about 11% when annealing the samples at 900 °C, because the decomposition of the supersaturated matrix leads to the formation of nanometer-sized domains, precipitation of hexagonal-structured B4 AlN (with their significantly larger specific volume), formation of stacking faults, and nano-twins. In contrast, for TiN, where no decomposition processes and formation of nanometer-sized domains can be initiated by an annealing treatment, the fracture toughness KIC remains roughly constant when annealed above the film deposition temperature. As the increase in KIC found for Ti1−xAlxN upon annealing is within statistical errors, we carried out complementary cube corner nanoindentation experiments, which clearly show reduced (or even impeded) crack formation for annealed Ti1−xAlxN as compared with their as-deposited counterpart. The ability of Ti1−xAlxN to maintain and even increase the fracture toughness up to high temperatures in combination with the concomitant age hardening effects and excellent oxidation resistance contributes to the success of this type of coatings.

Microstructural evolution and grain refinement in an intermetallic titanium aluminide alloy with a high molybdenum content: Paper presented at “XV International Conference on Electron Microscopy”, 15–18 September 2014, Cracow, Poland

Abstract As a strong β-stabilizing alloying element, Mo has gained importance for intermetallic β/γ-TiAl alloys. In general, TiAl alloys containing a significant volume fraction of the disordered body-centered cubic β-phase exhibit improved processing characteristics during hot-working. To increase the understanding of the alloying effect of Mo, a model alloy with the chemical composition Ti-44Al-7Mo-0.1B (in at.%) was investigated. In this work, the microstructural evolution after individual heat-treatment steps was studied by means of scanning as well as conventional and in-situ transmission electron microscopy. Additionally, macro-hardness and nanoindentation measurements were conducted to study the change in hardness due to grain refinement and solid-solution hardening. The variation of the observed macro- and nano-hardness corresponds well with the microstructural evolution. The obtained grain refinement effect leads to a significant increase in the macro-hardness, whereas the increase in the average nano-hardness of the individual phases is related to solid-solution hardening.

Atomic and electronic structures of a transition layer at the CrN/Cr interface

By spherical aberration (CS)-corrected high-resolution transmission electron microscopy (HRTEM) and electron energy-loss spectroscopy (EELS), the atomic and electronic structures at the CrN/Cr interface are studied. A transition layer is formed at the CrN/Cr interface, which is identified as hexagonal Cr2N. The atomic structures at the interfaces are revealed. The elemental concentration distribution across the interface was quantified by EELS. The fine structures of Cr-L2,3 in Cr, CrN, and Cr2N exhibit a subtle difference. The Cr-L2,3 edge in CrN shows a noticeable chemical shift as compared to Cr and Cr2N, accompanied by a slight variation at the corresponding N-K edge.

Transmission electron microscopical study of teenage crown dentin on the nanometer scale

This is the first transmission electron microscopic study of teenage crown dentin on the nanometer scale. Samples for TEM were prepared by mechanical thinning and chemical polishing that allowed obtaining the electron transparent foils. It was firstly shown that human dentin possesses the layered morphology: the layers are oriented normally to the main axis of a tooth and have the thickness of ~50nm. HA inorganic phase of teenage crown dentin is in the amorphous state. The cellular structure, which was formed from collagen fibers (diameter is ~5nm), are observed near DEJ region in teenage dentin, whereas bioorganic phase of teenage crown dentin near the pulp camera does not contain the collagen fibers. Cracks in dentin thin foils have sharp tips, but big angles of opening (~30°) with plastic zone ahead crack tip. It means that young crown human dentin exhibits ductile or viscous-elastic fracture behavior on the nanometer scale.

Origin of large plasticity and multiscale effects in iron-based metallic glasses

The large plasticity observed in newly developed monolithic bulk metallic glasses under quasi-static compression raises a question about the contribution of atomic scale effects. Here, nanocrystals on the order of 1–1.5 nm in size are observed within an Fe-based bulk metallic glass using aberration-corrected high-resolution transmission electron microscopy (HRTEM). The accumulation of nanocrystals is linked to the presence of hard and soft zones, which is connected to the micro-scale hardness and elastic modulus confirmed by nanoindentation. Furthermore, we performed systematic simulations of HRTEM images at varying sample thicknesses, and established a theoretical model for the estimation of the shear transformation zone size. The findings suggest that the main mechanism behind the formation of softer regions are the homogenously dispersed nanocrystals, which are responsible for the start and stop mechanism of shear transformation zones and hence, play a key role in the enhancement of mechanical properties.Iron-based bulk metallic glasses are remarkably plastic, but the origin of their plasticity remains challenging to isolate. Here, the authors use high resolution microscopy to show that nanocrystals are dispersed within the glass and form hard and soft zones that are responsible for enhancing ductility.

Microstructural and texture evolution of copper-(chromium, molybdenum, tungsten) composites deformed by high-pressure-torsion

Abstract Cu-refractory metal composites containing Cr, Mo or W were subjected to severe plastic deformation using room temperature high-pressure torsion (HPT). A lamellar microstructure developed in each of the composites at equivalent strains of ∼75. The refractory metals developed {hkl}⟨111⟩ fibre textures with a slight tilt to the tangential direction. This texture was stronger and more clearly defined in Mo and W than in Cr. By applying additional HPT deformation to these samples, perpendicular to the original shear strain, it was found that the lamellar structure of Cu30Mo70 and Cu20W80 (wt%) composites could be retained at high equivalent strains and the refractory layer thickness could be reduced to 20–50 nm in Cu20W80 and 10–20 nm in Cu30Mo70. Although neighbouring regions of the microstructure were aligned and there was evidence of local texture in both composites, the bulk texture of Cu30Mo70 became weaker during this second step of HPT deformation. This was attributed to the refractory metal lamellae being discontinuous and imperfectly aligned. This work shows that it is possible to form ultrafine composites of Cu-group VI refractory metals via high-pressure torsion, with namolamellar structures being possible where there is a sufficient volume fraction of Mo or W.

Study on the Atomic and Electronic Structure in CrN (VN, TiN) Films using Cs-Corrected TEM

Transition metal nitrides have found wide-spread applications in the cuttingand machiningtool industry due to their extreme hardness, thermal stability and resistance to corrosion. The increasing demand of these nitrides requires an in-depth understanding of their structures at the atomic level. This has led to some experimental and theoretical researches [1-6]. The films used in this study were deposited by reactive direct current magnetron sputtering of a Cr/V/Ti metal target in an Ar+N2 atmosphere at a constant total pressure of 1 Pa, a target power of 6 kW, and a temperature of 350°C. A TEM/STEM JEOL 2100F operated at 200 kV and equipped with an image-side CS-corrector and a Gatan imaging filter (Tridiem) was utilized for characterizing the film structure.