Search

Nanocrystalline and nanotwinned materials achieve exceptional strengths through small grain sizes. Due to large areas of crystal interfaces, they are highly susceptible to grain growth and creep deformation, even at ambient temperatures. Here, ultrahigh strength nanotwinned copper microstructures have been stabilized against high temperature exposure while largely retaining electrical conductivity. By incorporating less than 1 vol% insoluble tungsten nanoparticles by a novel hybrid deposition method, both the ease of formation and the high temperature stability of nanotwins are dramatically enhanced up to at least 400 °C. By avoiding grain coarsening, improved high temperature creep properties arise as the coherent twin boundaries are poor diffusion paths, while some size‐based nanotwin strengthening is retained. Such microstructures hold promise for more robust microchip interconnects and stronger electric motor components. [ABSTRACT FROM AUTHOR]

• High cycle fatigue strains mapped by nanoscale resolution digital image correlation. • Fine bands of deformation in lamellar γ-TiAl alloy formed ∼50 nm from interfaces. • Unlike monotonic loading, high cycle fatigue strains remain highly localised. • Strain gradients develop along slip bands, increasing in magnitude with cycling. Microcompression testpieces of a lamellar γ-TiAl alloy were high cycle fatigued up to 105 cycles at stress ratios of 0.5–0.7, to maximum stresses above and below the yield stress. The localised deformation was studied by nano-scale digital image correlation strain mapping of a Pt patterned side-face of the pillars. With crystal orientation mapping, the fatigue deformation lines were found to locate at the γ/γ and γ/α 2 lamellar interfaces. The deformation lines were closely spaced slip lines in transmission electron imaging. Gradients of shear strain developed along the deformation lines, increasing in magnitude as cycling progressed. Extensive transverse twinning also occurred. [ABSTRACT FROM AUTHOR]

Lamellar γ-TiAl has a microstructure that spans multiple length scales: lamellar thickness (10 nm–1 μm), γ domain length (100 nm–10 μm) and colony size (100 μm–1 mm). Only by characterizing the deformation across the different scales can one understand how the microstructure influences plasticity and damage formation in this material. Here, we use digital image correlation and electron backscatter diffraction to map strain and lattice rotation with both sub-colony and sub-lamella spatial resolution in a polycrystalline lamellar γ-TiAl alloy with TiB 2 inclusions. Two lamellar thicknesses and temperatures are tested. It is shown that the hard mode-oriented colonies undergo minimal plastic strain. However, as the temperature is increased, macroscopic deformation bands develop across colonies of different orientations, independent of their local lamellar orientations. Increasing magnification, it is apparent that some segments of these bands occur by slip or twinning parallel to the lamellae, and others by transverse lattice rotation. In the thin lamellar condition, such macroscopic deformation bands also occur along colony boundaries; this causes a significant inhomogeneity in the strain distribution. Such strain inhomogeneities are also further characterised here at the microstructural scale of single lamellae, and locally at boride particles. • Nanoscale resolution digital image correlation (HR-DIC) strain mapping up to 700 °C. • Characterisation of plastic deformation and mechanical damage across multiple length scales in lamellar γ-TiAl. • Macroscopic bands of heightened deformation developed, focused at grain boundaries. • Methods to repress deformation bands by microstructural modifications are discussed. [ABSTRACT FROM AUTHOR]

Abstract The distribution of strain in hard mode oriented lamellar stacks of the two-phase γ-TiAl/α 2 -Ti 3 Al alloy Ti-45Al-2Nb-2Mn (at.%)-0.8 vol% TiB 2 was measured at several temperatures up to 633 °C by in situ micropillar compression, complemented by electron backscatter diffraction orientation mapping and digital image correlation strain mapping of a thermally stable surface Pt speckle pattern. Post-mortem transmission electron microscopy further identified the finest scale deformation structures. It was found that slip and twinning transverse to the lamellae operates within discreet bands that zigzag across the lamellar structure. The shear strain within each band is approximately constant across the pillar width. This is inconsistent with current energetic models for transverse twin formation in γ-TiAl, which assume independent, non-interacting twins. This is explained using a mathematical formulation for the stress required to operate this transverse mechanical twinning as a function of strain. This study has elucidated how the multi-scale combination of several transverse twinning systems on different {111} planes in γ-TiAl lamellae can relieve the elastic stresses generated at a lamellar interface by the primary (highest Schmid factor) twinning system. It is thought that the facilitation of this mechanism will promote the ductilisation of lamellar γ-TiAl alloys. This is crucial for an increased damage tolerance and ease of component manufacture, leading to a more widespread use of γ-TiAl alloys. Graphical abstract Image 1 [ABSTRACT FROM AUTHOR]

Abstract The occurrence of plasticity below the macroscopic yield stress during tensile monotonic loading of nearly lamellar Ti-45Al-2Nb-2Mn(at%)-0.8 vol% TiB 2 at both 25 °C and 700 °C, and in two conditions of lamellar thickness, was measured by digital image correlation strain mapping of a remodelled Au surface speckle pattern. Such initial plasticity, not necessarily related to the presence of common stress concentrators such as hard particles or cracks, could occur at applied stresses as low as 64% of the general yield stress. For a same applied strain it was more prominent at room temperature, and located as slip and twinning parallel to, and near to or at (respect.) lamellar interfaces of all types in soft mode-oriented colonies. These stretched the full colony width and the shear strain was most intense in the centre of the colonies. Further, the most highly operative microbands of plasticity at specimen fracture were not those most active prior to yielding. The strain mapping results from polycrystalline tensile loading were further compared to those from microcompression testing of soft-mode stacks of lamellae milled from single colonies performed at the same temperatures. Combined with post-mortem transmission electron microscopy of the pillars, the initial plasticity by longitudinal dislocation glide was found to locate within 30–50 nm of the lamellar interfaces, and not at the interfaces themselves. The highly localised plasticity that precedes high cycle fatigue failure is therefore inherently related to the lamellar structure, which predetermines the locations of plastic strain accumulation, even in a single loading cycle. Graphical abstract Image 1 [ABSTRACT FROM AUTHOR]

The stress required to activate twinning of the longitudinal < 11 2 ¯ ] { 111 } system in the lamellar γ-TiAl phase of the alloy Ti-45Al-2Nb-2Mn (at.%)-0.8 vol.% TiB 2 was measured at several temperatures up to 700 °C by in situ micropillar compression of soft mode oriented γ-TiAl/α 2 -Ti 3 Al lamellar stacks. The lamellae undergoing deformation twinning were identified by electron backscatter diffraction orientation mapping. In some cases, such lamellae were not constrained by domain or colony boundaries and longitudinal twinning was the only deformation mechanism observed based on digital image correlation strain maps. The resolved shear stress for such unconstrained twinning was found to increase monotonically with temperature from 25 °C to 700 °C. This is consistent with the stacking fault energy increasing with temperature as found in many metallic alloys, suggesting that the increased ease of deformation twinning at high temperature in bulk TiAl alloys is due to the increased ease with which the twinning shear can be accommodated by the neighbouring domains and lamellae with increasing temperature, rather than a thermal softening of the intrinsic twinning mechanism. [ABSTRACT FROM AUTHOR]

In this paper the occurrence of twinning parallel to the lamellae during compression at 700 °C of a polycrystalline nearly lamellar commercial γ-TiAl alloy, Ti-45Al-2Nb-2Mn(at%)-0.8 vol% TiB 2 , has been studied and shown to lead to the formation of cracks at colony boundaries. However, the occurrence of this longitudinal twinning mode was less common by at least a factor of ten in tests at room temperature. Furthermore, the debonding of colony boundaries caused by the shear strain of longitudinal twinning is exacerbated when the same γ-TiAl variant favourably oriented for twinning occurs repeatedly in the lamellar structure. This effect was caused by the preferential nucleation of certain γ-TiAl variants in the presence of TiB 2 boride reinforcement. It is shown that the boride additions increase the probability of double, triple or even higher order multiply stacked γ-variants. This increases the resulting shear strain that must be accommodated and hence the probability of crack nucleation. [ABSTRACT FROM AUTHOR]

Physical vapour deposition combined with atomic layer deposition was exploited to design a model system of UFG aluminium with a narrow grain size and shape distribution, including two types of interfaces (Al-Al & Al-Al 2 O 3), with Al-Al grain boundary orientations exclusively parallel to the loading axis. This enabled isolated study of the strengthening mechanisms that ultrathin oxide layers would provide in a metal multilayer structure. The Al/Al 2 O 3 crystalline/amorphous multilayers with 240 nm metal layers and oxide thicknesses in the range <1 nm–12 nm (i.e. to below the natural oxidation thickness), were microcompressed, yielding a pseudo-macroscopic yield strength of 532 MPa – over 100 MPa higher than the literature-conforming oxide-free reference. The homogenous co-deformation of the structure, with barrelling of the individual metal layers at the micropillar edges, results from the high bonding strength of the metal with its native oxide, meaning no failure or sliding at the interface, unlike previous Al/ceramic multilayer studies. Only the thicker (≥5 nm) oxide layers fractured in-plane: at locations coincident with vertical Al-Al grain boundaries. An analysis of contributions to the strength of these crystalline/amorphous metal/ceramic hybrid multilayers is carried out, identifying the Al-Al 2 O 3 interface to be the crucial factor, rather than the in-plane tensile stiffness and considerable plasticity of ALD Al 2 O 3 itself. The strengthening effect of the oxide layer was effective down to a layer thickness of just 0.5 nm. [Display omitted] [ABSTRACT FROM AUTHOR]

The occurrence of longitudinal twinning in the engineering alloy Ti-45Al-2Nb-2Mn (at.%)-0.8 vol.% TiB 2 has been studied by measuring the changes in crystallographic orientation within individual lamellae during microcompression. Twinning in this alloy appeared to be a nucleation-limited process with the twins growing from lamellar boundaries at resolved shear stresses as low as 100 MPa, consistent with observations elsewhere. However, instead of forming twins ~ 10–200 nm in thickness, as in polysynthetically twinned crystals, the longitudinal twins in this alloy were initiated at a lamellar boundary and then spread through the whole lamella. [ABSTRACT FROM AUTHOR]

• Nanoscale digital image correlation (HR-DIC) strain mapping of HCF up to 670 °C. • Microplasticity mainly in softmode colonies: parallel to lamellae, near interfaces. • Poor strain transfer across colony boundaries at both temperatures. • At 25 °C, maximum stress influenced the slip band count more than did the cycle count. Microplasticity in a lamellar TiAl alloy upon high cycle tensile fatigue was measured by high resolution digital image correlation strain mapping at several stress and cycle increments, at 25 °C and 670 °C, for two lamellar thicknesses. Plastic deformation occurred primarily in soft-mode colonies at both temperatures, operating by slip parallel to the lamellae, and near lamellar interfaces. Plastic strains generally decreased to zero by the colony boundary; strain transfer across such boundaries was rare at both temperatures. At 25 °C, the maximum applied stress influenced the number of slip bands more so than did the number of loading cycles. [ABSTRACT FROM AUTHOR]

• Physical vapor deposition and atomic layer deposition systems were integrated. • The sample was transferred within deposition chambers without breaking high vacuum. • An Al-Al 2 O 3 multilayer brick-mortar structure was deposited by the hybrid system. • Each ultrathin Al 2 O 3 sublayer interrupted the grain growth of the Al sublayer. • Surface oxidation of Al sublayers was circumvented by keeping sample in high vacuum. A hybrid thin film deposition system was built by combining physical vapor deposition (PVD) with atomic layer deposition (ALD) without breaking high vacuum, which was achieved by a chamber-in-chamber design. The vacuum is better than 1 × 10−5 Pa during the entire sample transfer process between the ALD and PVD chambers. The Al-Al 2 O 3 multilayers synthesized by the PVD-ALD integrated system consist of ALD Al 2 O 3 sublayers between pure PVD Al sublayers. The Al 2 O 3 sublayers, with incremental thickness of 1 nm from 1 to 10 nm, effectively interrupted the grain growth of the ~250 nm thick Al sublayers. Native surface oxide formation on the PVD deposited pure Al sublayers was circumvented by keeping the substrate in high vacuum between processing steps. The pure Al sublayers are constituted of equiaxed grains with no epitaxial or texture relationship with the neighboring layers. The Al grain boundaries are parallel to the film growth direction and extend the height of each Al sublayer, to form a brick-and-mortar type microstructure. In this system, ALD allows precise control of the thickness of each ultrathin Al 2 O 3 layer, to thicknesses below the native surface oxide thickness of pure Al, and avoids further natural oxidation through the low-oxygen environment of the PVD-ALD system. [ABSTRACT FROM AUTHOR]

Gas-assisted focused electron-beam-induced deposition is a versatile tool for the direct writing of complex-shaped nanostructures with unprecedented shape fidelity and resolution. While the technique is well-established for various materials, the direct electron beam writing of silver is still in its infancy. Here, we examine and compare five different silver carboxylates, three perfluorinated: [Ag2(µ-O2CCF3)2], [Ag2(µ-O2CC2F5)2], and [Ag2(µ-O2CC3F7)2], and two containing branched substituents: [Ag2(µ-O2CCMe2Et)2] and [Ag2(µ-O2CtBu)2], as potential precursors for focused electron-beam-induced deposition. All of the compounds show high sensitivity to electron dissociation and efficient dissociation of Ag-O bonds. The as-deposited materials have silver contents from 42 at.% to above 70 at.% and are composed of silver nano-crystals with impurities of carbon and fluorine between them. Precursors with the shortest carbon-fluorine chain ligands yield the highest silver contents. In addition, the deposited silver content depends on the balance of electron-induced ligand co-deposition and ligand desorption. For all of the tested compounds, low electron flux was related to high silver content. Our findings demonstrate that silver carboxylates constitute a promising group of precursors for gas-assisted focused electron beam writing of high silver content materials. [ABSTRACT FROM AUTHOR]

The strain rate (ε ˙) and temperature (T) dependent mechanical response of single crystal magnesium (Mg) micropillars compressed along the [ 2 ¯ 110 ] direction (a -axis) is investigated from room temperature to 573 K and from 10-3 to 100 s-1. The loading direction was chosen to disfavour basal slip activation by a low Schmid factor, allowing the investigation of the rate-sensitivities of extension twinning and prismatic slip. For T ≤ 423 K, the plasticity was governed by extension twinning for the entire range of the applied strain rates. At T > 423 K and for ε ˙ ≤ 10 s-1, extension twinning did not occur and a continuous plastic flow induced by prismatic dislocation mediated plasticity was observed: the twin to slip transition takes place due to the decrease of the critical resolved shear stress of non-basal slip. For ε ˙ > 10 s-1, however, the accommodation of the plastic deformation by activation of prismatic slip is not enough to match the applied deformation rate, favouring again deformation twinning. The first part of this work provides a complete overview of the mutual effects of T and ε ˙ on the transition points of deformation modes in Mg at the microscale. In a second stage, the influence of thermal and kinetic contributions on the evolution of the flow stress leading to the slip to twin transition at 573 K has been assessed in more detail. Within the slip-dominated plasticity regime, this work provides a quantitative assessment of the increases in the saturation stress (stage III) with ε ˙ at high temperature, showing how the strain rate dependency of the dislocation generation rate in the pillar and escape rate at the free surfaces of the structure controls the stress evolution in Mg microcrystals. [Display omitted] [ABSTRACT FROM AUTHOR]