Direct Observation of Quadrupolar Strain Fields forming a Shear Band in Metallic Glasses.

For decades, scanning/transmission electron microscopy (S/TEM) techniques have been employed to analyze shear bands in metallic glasses and understand their formation in order to improve the mechanical properties of metallic glasses. However, due to a lack of direct information in reciprocal space, conventional S/TEM cannot characterize the local strain and atomic structure of amorphous materials, which are key to describe the deformation of glasses. For this work, 4-dimensional-STEM (4D-STEM) is applied to map and directly correlate the local strain and the atomic structure at the nanometer scale in deformed metallic glasses. Residual strain fields are observed with quadrupolar symmetry concentrated at dilated Eshelby inclusions. The strain fields percolate in a vortex-like manner building up the shear band. This provides a new understanding of the formation of shear bands in metallic glass.

Room Temperature Viscous Flow of Amorphous Silica Induced by Electron Beam Irradiation.

The increasing use of oxide glasses in high-tech applications illustrates the demand of novel engineering techniques on nano- and microscale. Due to the high viscosity of oxide glasses at room temperature, shaping operations are usually performed at temperatures close or beyond the point of glass transition Tg . Those treatments, however, are global and affect the whole component. It is known from the literature that electron irradiation facilitates the viscous flow of amorphous silica near room temperature for nanoscale components. At the micrometer scale, however, a comprehensive study on this topic is still pending. In the present study, electron irradiation inducing viscous flow at room temperature is observed using a micropillar compression approach and amorphous silica as a model system. A comparison to high temperature yielding up to a temperature of 1100 °C demonstrates that even moderate electron irradiation resembles the mechanical response of 600 °C and beyond. As an extreme case, a yield strength as low as 300 MPa is observed with a viscosity indicating that Tg has been passed. Those results show that electron irradiation-facilitated viscous flow is not limited to the nanoscale which offers great potential for local microengineering.

Effect of High-Pressure Torsion on the Microstructure and Magnetic Properties of Nanocrystalline CoCrFeNiGax (x = 0.5, 1.0) High Entropy Alloys.

In our search for an optimum soft magnet with excellent mechanical properties which can be used in applications centered around "electro mobility", nanocrystalline CoCrFeNiGax (x = 0.5, 1.0) bulk high entropy alloys (HEA) were successfully produced by spark plasma sintering (SPS) at 1073 K of HEA powders produced by high energy ball milling (HEBM). SPS of non-equiatomic CoCrFeNiGa0.5 particles results in the formation of a single-phase fcc bulk HEA, while for the equiatomic CoCrFeNiGa composition a mixture of bcc and fcc phases was found. For both compositions SEM/EDX analysis showed a predominant uniform distribution of the elements with only a small number of Cr-rich precipitates. High pressure torsion (HPT) of the bulk samples led to an increased homogeneity and a grain refinement: i.e., the crystallite size of the single fcc phase of CoCrFeNiGa0.5 decreased by a factor of 3; the crystallite size of the bcc and fcc phases of CoCrFeNiGa-by a factor of 4 and 10, respectively. The lattice strains substantially increased by nearly the same extent. After HPT the saturation magnetization (Ms) of the fcc phase of CoCrFeNiGa0.5 and its Curie temperature increased by 17% (up to 35 Am2/kg) and 31.5% (from 95 K to 125 K), respectively, whereas the coercivity decreased by a factor of 6. The overall Ms of the equiatomic CoCrFeNiGa decreased by 34% and 55% at 10 K and 300 K, respectively. At the same time the coercivity of CoCrFeNiGa increased by 50%. The HPT treatment of SPS-consolidated HEAs increased the Vickers hardness (Hv) by a factor of two (up to 5.632 ± 0.188) only for the non-equiatomic CoCrFeNiGa0.5, while for the equiatomic composition, the Hv remained unchanged (6.343-6.425 GPa).

Dislocation-toughened ceramics.

Functional and structural ceramics have become irreplaceable in countless high-tech applications. However, their inherent brittleness tremendously limits the application range and, despite extensive research efforts, particularly short cracks are hard to combat. While local plasticity carried by mobile dislocations allows desirable toughness in metals, high bond strength is widely believed to hinder dislocation-based toughening of ceramics. Here, we demonstrate the possibility to induce and engineer a dislocation microstructure in ceramics that improves the crack tip toughness even though such toughening does not occur naturally after conventional processing. With modern microscopy and simulation techniques, we reveal key ingredients for successful engineering of dislocation-based toughness at ambient temperature. For many ceramics a dislocation-based plastic zone is not impossible due to some intrinsic property (e.g. bond strength) but limited by an engineerable quantity, i.e. the dislocation density. The impact of dislocation density is demonstrated in a surface near region and suggested to be transferrable to bulk ceramics. Unexpected potential in improving mechanical performance of ceramics could be realized with novel synthesis strategies.

Control of polarization in bulk ferroelectrics by mechanical dislocation imprint.

Defects are essential to engineering the properties of functional materials ranging from semiconductors and superconductors to ferroics. Whereas point defects have been widely exploited, dislocations are commonly viewed as problematic for functional materials and not as a microstructural tool. We developed a method for mechanically imprinting dislocation networks that favorably skew the domain structure in bulk ferroelectrics and thereby tame the large switching polarization and make it available for functional harvesting. The resulting microstructure yields a strong mechanical restoring force to revert electric field-induced domain wall displacement on the macroscopic level and high pinning force on the local level. This induces a giant increase of the dielectric and electromechanical response at intermediate electric fields in barium titanate [electric field-dependent permittivity (ε33) ≈ 5800 and large-signal piezoelectric coefficient (d 33*) ≈ 1890 picometers/volt]. Dislocation-based anisotropy delivers a different suite of tools with which to tailor functional materials.

A Multiple Length-Scales Nanoimprinting Approach on Nanocrystalline and Strongly Deformed CuZn30 Alloys.

Metallic Nanoimprinting is a new approach to form robust surface structures on metals at various length scales. The shape and size of the formed structures not only depends on the dimensions of the Nanoimprinting die but also the mechanical behaviour of the imprinted material and its microstructure. To characterise the Nanoimprinting process, a multi length-scale-approach was used by varying the cavities (widths between 20 nm and 2.76 µm) as well as the microstructure of the alloy. CuZn30 was used in different cold-worked and heat-treated conditions, with grain sizes from 100 nm up to 277 µm, thus, covering a wide range of hardening behaviours and grain size to cavity width ratios. Experimental results show that the work hardening behaviour as well as the subgrain or grain size have a major influence on the forming characteristics during Nanoimprinting and a nearly ideal plastic behaviour (no work hardening) leads to the largest extrusion heights. For materials with a pronounced work hardening, low extrusion heights were measured for all cavity widths. This work demonstrates the potential of a simple imprinting process to generate surface features on metallic materials with a width <300 nm and an aspect ratio >1.

Local Deformation of Glasses is Mediated by Rigidity Fluctuation on Nanometer Scale.

Microscopic deformation processes determine defect formation on glass surfaces and, thus, the material's resistance to mechanical failure. While the macroscopic strength of most glasses is not directly dependent on material composition, local deformation and flaw initiation are strongly affected by chemistry and atomic arrangement. Aside from empirical insight, however, the structural origin of the fundamental deformation modes remains largely unknown. Experimental methods that probe parameters on short or intermediate length-scale such as atom-atom or superstructural correlations are typically applied in the absence of alternatives. Drawing on recent experimental advances, spatially resolved Raman spectroscopy is now used in the THz-gap for mapping local changes in the low-frequency vibrational density of states. From direct observation of deformation-induced variations on the characteristic length-scale of molecular heterogeneity, it is revealed that rigidity fluctuation mediates the deformation process of inorganic glasses. Molecular field approximations, which are based solely on the observation of short-range (interatomic) interactions, fail in the prediction of mechanical behavior. Instead, glasses appear to respond to local mechanical contact in a way that is similar to that of granular media with high intergranular cohesion.

Advanced Nanoindentation Testing for Studying Strain-Rate Sensitivity and Activation Volume.

Nanoindentation became a versatile tool for testing local mechanical properties beyond hardness and modulus. By adapting standard nanoindentation test methods, simple protocols capable of probing thermally activated deformation processes can be accomplished. Abrupt strain-rate changes within one indentation allow determining the strain-rate dependency of hardness at various indentation depths. For probing lower strain-rates and excluding thermal drift influences, long-term creep experiments can be performed by using the dynamic contact stiffness for determining the true contact area. From both procedures hardness and strain-rate, and consequently strain-rate sensitivity and activation volume can be reliably deducted within one indentation, permitting information on the locally acting thermally activated deformation mechanism. This review will first discuss various testing protocols including possible challenges and improvements. Second, it will focus on different examples showing the direct influence of crystal structure and/or microstructure on the underlying deformation behavior in pure and highly alloyed material systems.

Experimental and theoretical confirmation of the scaling exponent 2 in pyramidal load displacement data for depth sensing indentation.

A series of articles by Kaupp et al. have recently been published in "Scanning," containing erroneous claims about the curvature of pyramidal nanoindentation loading curves. The present paper recalls the theoretical reasons why, for self-similar indenter shapes like pyramidal or conical indentations, the load scales with the indentation depth squared. Furthermore, experimental evidence for that behavior is provided for a wide variety of materials, ranging from ceramics to metals and polymers.

Micromechanics and ultrastructure of pyrolysed softwood cell walls.

Pyrolytic conversion causes severe changes in the microstructure of the wood cell wall. Pine wood pyrolysed up to 325 °C was investigated by transmission electron microscopy, atomic force microscopy and nanoindentation measurements to monitor changes in structure and mechanical properties. Latewood cell walls were tested in the axial, radial and tangential directions at different temperatures of pyrolysis. A strong anisotropy of elastic properties in the native cell wall was found. Loss of the hierarchical structure of the cell wall due to pyrolysis resulted in elastic isotropy at 300 °C. The development of the mechanical properties with increasing temperature can be explained by alterations in the structure and it was found that the elastic properties were clearly related to length and orientation of the microfibrils.

Cell-based resurfacing of large cartilage defects: long-term evaluation of grafts from autologous transgene-activated periosteal cells in a porcine model of osteoarthritis.

OBJECTIVE: To investigate the potential of transgene-activated periosteal cells for permanently resurfacing large partial-thickness cartilage defects. METHODS: In miniature pigs, autologous periosteal cells stimulated ex vivo by bone morphogenetic protein 2 gene transfer, using liposomes or a combination of adeno-associated virus (AAV) and adenovirus (Ad) vectors, were applied on a bioresorbable scaffold to chondral lesions comprising the entire medial half of the patella. The resulting repair tissue was assessed, 6 and 26 weeks after transplantation, by histochemical and immunohistochemical methods. The biomechanical properties of the repair tissue were characterized by nanoindentation measurements. Implants of unstimulated cells and untreated lesions served as controls. RESULTS: All grafts showed satisfactory integration into the preexisting cartilage. Six weeks after transplantation, AAV/Ad-stimulated periosteal cells had adopted a chondrocyte-like phenotype in all layers; the newly formed matrix was rich in proteoglycans and type II collagen, and its contact stiffness was close to that of healthy hyaline cartilage. Unstimulated periosteal cells and cells activated by liposomal gene transfer formed only fibrocartilaginous repair tissue with minor contact stiffness. However, within 6 months following transplantation, the AAV/Ad-stimulated cells in the superficial zone tended to dedifferentiate, as indicated by a switch from type II to type I collagen synthesis and reduced contact stiffness. In deeper zones, these cells retained their chondrocytic phenotype, coinciding with positive staining for type II collagen in the matrix. CONCLUSION: Large partial-thickness cartilage defects can be resurfaced efficiently with hyaline-like cartilage formed by transgene-activated periosteal cells. The long-term stability of the cartilage seems to depend on physicobiochemical factors that are active only in deeper zones of the cartilaginous tissue.