Deformation mechanisms in nanocrystalline palladium at large strains

The mechanical behaviour and microstructure evolution of nanocrystalline palladium was investigated. Material with an initial grain size ～10 nm was prepared by inert gas condensation. Instrumented high-pressure torsion straining was used to characterize the flow stress during plastic deformation to shear strains up to 300. A change in primary deformation mechanism was induced by stress-induced grain growth. For grain sizes <40 nm, grain boundary mediated processes (shear banding, grain boundary sliding and grain rotation) controlled the deformation, with dislocation slip, twinning, and grain boundary diffusion providing the accommodation. For larger grain sizes, the operative deformation mechanism was dislocation slip.     

Using ring samples to evaluate the processing characteristics in high-pressure torsion

An Al–3% Mg–0.2% Sc alloy was processed by high-pressure torsion (HPT) using samples in the form of solid disks and rings. Following HPT, all values of the measured Vickers microhardness fall onto a single curve when plotted against the equivalent strain, such that there are increasing values of hardness at the lower strains and hardness saturation above equivalent strains of ～40. This saturation level is independent of the number of revolutions and the applied pressure. The grain size following HPT is ～220 nm, and tensile tests show that the material is superplastic at a testing temperature of 573 K.     

Microstructural characteristics of tungsten-base nanocomposites produced from micropowders by high-pressure torsion

Micropowder mixtures of W–50% Al, W–50% Ti and W–50% Ni were subjected to severe plastic deformation at 573 K using high-pressure torsion (HPT). The powder mixtures were consolidated and nanocomposites of W/Ti, W/Ti and W/Ni, with average grain sizes as small as ～9, ～15 and ～12 nm, respectively, were formed by imposing large shear strains. The nanocomposites exhibited Vickers microhardness as high as ～900 Hv, a level that has rarely been reported for metal–matrix composites. X-ray diffraction analyses together with high-resolution transmission electron microscopy showed that in addition to grain refinement, an increase in the fraction of grain boundaries up to 20%, the dissolution of elements in each other up to ～15 mol.%, an increase in the lattice strain up to 0.6%, and an increase in density of edge dislocations up to 10¹⁶ m^?2 occurred by HPT. The current study introduces the HPT process as an effective route for the production of ultrahigh-strength W-base nanocomposites, fabrication of which is not generally easy when processing at high temperatures because of interfacial reaction and formation of brittle intermetallics.     

Microstructural evolution and grain boundary sliding in a superplastic magnesium AZ31 alloy

Tensile experiments on a fine-grained single-phase Mg–Zn–Al alloy (AZ31) at 673 K revealed superplastic behavior with an elongation to failure of 475% at 1 × 10^?4 s^?1 and non-superplastic behavior with an elongation to failure of 160% at 1 × 10^?2 s^?1; the corresponding strain rate sensitivities under these conditions were ～0.5 and ～0.2, respectively. Measurements indicated that the grain boundary sliding (GBS) contribution to strain ξ was ～30% under non-superplastic conditions; there was also a significant sharpening in texture during such deformation. Under superplastic conditions, ξ was ～50% at both low and high elongations of ～20% and 120%; the initial texture became more random under such conditions. In non-superplastic conditions, deformation occurred under steady-state conditions without grain growth before significant flow localization whereas, under superplastic conditions, there was grain growth during the early stages of deformation, leading to strain hardening. The grains retained equiaxed shapes under all experimental conditions. Superplastic deformation is attributed to GBS, while non-superplastic deformation is attributed to intragranular dislocation creep with some contribution from GBS. The retention of equiaxed grain shapes during dislocation creep is consistent with a model based on local recovery related to the disturbance of triple junctions.     

Synthesis and characterization of mechanically alloyed and shock-consolidated nanocrystalline NiAl intermetallic

The synthesis, microstructural characterization and microhardness of nanocrystalline B2-phase NiAl intermetallic are discussed in this paper. Nanophase NiAl powders were prepared by mechanical alloying of elemental Ni and Al powders under an argon atmosphere for different times (0–48 h). The alloyed nanocrystalline powders were then consolidated by shock compaction at a peak pressure of 4–6 GPa, to 83% dense compacts. Characterization by transmission electron microscopy (TEM) revealed that the microstructure of the shock-consolidated sample was retained at the nanoscale. The average crystallite size measurements revealed that mechanically alloyed NiAl grain size decreased from 48±27 to 9±3 nm with increasing mechanical alloying time from 8 to 48 h. The long-range-order parameters of powders mechanically alloyed for different times were determined, and were observed to vary between 0.82 for 5 h and 0.63 for 48 h of milling time. Following shock compaction, the long-range-order parameter was determined to be 0.76, 0.69 and 0.66, respectively, for the 16, 24 and 48 h alloyed specimens. Both the mechanically alloyed nanocrystalline NiAl powder and the shock-consolidated bulk specimen showed evidence of grain boundary dislocations, subgrains, and distorted regions. A large number of grain boundaries and defects were observed via high resolution TEM (HRTEM). Shear bands were also observed in the mechanically alloyed NiAl intermetallic powders and in the shock-consolidated compacts. Microhardness measurements of shock-consolidated material showed increasing microhardness with increasing crystallite size refinement, following Hall–Petch behavior.     

Influence of grain size in the near-micrometre regime on the deformation microstructure in aluminium

The effect of grain size on deformation microstructure formation in the near-micrometre grain size regime has been studied using samples of aluminium prepared using a spark plasma sintering technique. Samples in a fully recrystallized grain condition with average grain sizes ranging from 5.2 to 0.8 μm have been prepared using this technique. Examination in the transmission electron microscope of these samples after compression at room temperature to approximately 20% reduction reveals that grains larger than 7 μm are subdivided by cell block boundaries similar to those observed in coarse-grained samples, with a similar dependency on the crystallographic orientation of the grains. With decreasing grain size down to approx. 1 μm there is a gradual transition from cell block structures to cell structures. At even smaller grain sizes of down to approx. 0.5 μm the dominant features are dislocation bundles and random dislocations, although at a larger compressive strain of 30% dislocation rotation boundaries may also be found in the interior of grains of this size. A standard 〈1 1 0〉 fibre texture is found for all grain sizes, with a decreasing sharpness with decreasing grain size. The structural transitions with decreasing grain size are discussed based on the general principles of grain subdivision by deformation-induced dislocation boundaries and of low-energy dislocation structures as applied to the not hitherto explored near-micrometre grain size regime.     

Microstructure and mechanical properties of ultrafine-grained fcc/hcp cobalt processed by a bottom-up approach

Bulk Co samples having a mean grain size of ～300 nm were processed by hot isostatic pressing of a high purity Co nanopowder synthesized by chimie douce. The grain interior exhibited a highly faulted nanoscale lamellar microstructure comprising an intricate mixture of face-centered cubic, hexagonal close-packed phases and nanotwins. Room temperature compression tests carried out at a strain rate of ～2 × 10^?4 s^?1 revealed a yield stress of ～1 GPa, a strain to rupture of ～5%. During straining it was found that the hexagonal close-packed phase content increased from 55% to 65% suggesting a deformation mechanism based on stress-assisted face-centered cubic to hexagonal close-packed phase transformation. In addition, an apparent activation volume of ～3b³ was computed which indicates that the deformation mechanism was controlled by dislocation nucleation from the numerous boundaries. Nonetheless, in such an intricate microstructure, the overall mechanical properties are discussed in term of a complex interplay between lattice dislocation plasticity, transformation-induced plasticity and possibly twin-induced plasticity.     

Microstructural evolution in copper subjected to severe plastic deformation: Experiments and analysis

The evolution of microstructure and the mechanical response of copper subjected to severe plastic deformation using equal channel angular pressing (ECAP) was investigated. Samples were subjected to ECAP under three different processing routes: B_C, A and C. The microstructural refinement was dependent on processing with route B_C being the most effective. The mechanical response is modeled by an equation containing two dislocation evolution terms: one for the cells/subgrain interiors and one for the cells/subgrain walls. The deformation structure evolves from elongated dislocation cells to subgrains to equiaxed grains with diameters of ∼200–500 nm. The misorientation between adjacent regions, measured by electron backscatter diffraction, gradually increases. The mechanical response is well represented by a Voce equation with a saturation stress of 450 MPa. Interestingly, the microstructures produced through adiabatic shear localization during high strain rate deformation and ECAP are very similar, leading to the same grain size. It is shown that both processes have very close Zener–Hollomon parameters (ln Z ∼ 25). Calculations show that grain boundaries with size of 200 nm can rotate by ∼30° during ECAP, thereby generating and retaining a steady-state equiaxed structure. This is confirmed by a grain-boundary mobility calculation which shows that their velocity is 40 nm/s for a 200 nm grain size at 350 K, which is typical of an ECAP process. This can lead to the grain-boundary movement necessary to retain an equiaxed structure.     

Laser compression of nanocrystalline tantalum

Nanocrystalline tantalum (grain size ～70 nm) prepared by severe plastic deformation (high-pressure torsion) from monocrystalline [1 0 0] stock was subjected to shock compression generated by high-energy laser (～350–850 J), creating pressure pulses with initial duration of ～3 ns and amplitudes of up to ～145 GPa. The laser beam, with a spot radius of ～1 mm, created a crater of significant depth (～135 μm). Transmission electron microscopy revealed few dislocations within the grains and an absence of twins at the highest shock pressure, in contrast with monocrystalline tantalum. Hardness measurements were conducted and show a rise as the energy deposition surface is approached, evidence of shock-induced defects. The grain size was found to increase at a distance of 100 μm from the energy deposition surface as a result of thermally induced grain growth. The experimentally measured dislocation densities are compared with predictions using analyses based on physically based constitutive models, and the similarities and differences are discussed in terms of the mechanisms of defect generation. A constitutive model for the onset of twinning, based on a critical shear stress level, is applied to the shock compression configuration. The predicted threshold pressure at which the deviatoric component of stress for slip exceeds the one for twinning is calculated and it is shown that it is increased from ～24 GPa for the monocrystalline to ～150 GPa for the nanocrystalline tantalum (above the range of the present experiments). Calculations using the Hu–Rath analysis show that grain growth induced by the post shock-induced temperature rise is consistent with the experimental results: grains grow from 70 to 800 nm within the post-shock cooling regime when subjected to a laser pulse with energy of 684 J.     

Atom probe tomographic study of a friction-stir-processed Al–Mg–Sc alloy

The microstructure of a twin-roll-cast Al–4.5Mg–0.28Sc at.% alloy after friction-stir processing, performed at two tool rotational rates, was investigated by atom probe tomography. Outside the stir zone, the peak-aged alloy contains a high number density (～8.0 × 10²³ m^?3) of ～1.5 nm radius Al₃Sc (L1₂) precipitates with a minor Mg content, providing an increase of ～600 MPa in the Vickers microhardness. In the stir zone of the sample processed at 400 rpm rotational rate, the microhardness increase is mainly due to grain refinement, rather than precipitate strengthening, because the Al₃Sc precipitates, with spherical lobed cuboids and platelet-like morphology, grow and coarsen to a 10–20 nm radius. The Sc supersaturation across the stir-processed zone has a concentration gradient, which is higher on the retreating side and lower on the advancing side of the friction-stir tool. Hence, after aging at 290 °C for 22 h, the microhardness increase within the stir zone also displays a gradient due to precipitate strengthening with varying precipitate volume fractions. In the stir zone for the sample processed at 325 rpm rotational rate, the microhardness increase is also predominantly due to grain refinement, as coarse Al₃Sc precipitates form heterogeneously at grain boundaries with a platelet-like morphology. The hardness remains unchanged after a 290 °C aging treatment. This is because the Al₃Sc precipitates are highly heterogeneously distributed due to a combination of a small Sc supersaturation (0.05 at.%) in the matrix, the existence of dislocations, and a large area per unit volume of grain boundaries (～4–6 × 10⁶ m^?1).     

Transition from homogeneous-like to shear-band deformation in nanolayered crystalline Cu/amorphous Cu–Zr micropillars: Intrinsic vs. extrinsic size effect

The microcompression method was used to investigate the compressive plastic flow behavior of nanolayered crystalline/amorphous (C/A) Cu/Cu–Zr micropillars within wide ranges of intrinsic layer thicknesses (h ～ 5–150 nm) and extrinsic sample sizes (350–1425 nm) with the goal of revealing the intrinsic size effect, extrinsic size effect and their interplay on the plastic deformation behavior. The nanolayered C/A micropillars exhibited deformation behaviors of strain-hardening followed by strain-softening that were dependent on the thickness of the layers. At h ? 10 nm, the strain-softening is related to shear deformation that is caused by fractures in the amorphous layers. At h > 10 nm, however, the strain-softening is related to the reduction in dislocation density caused by dislocation absorption. Correspondingly, the deformation mode of the C/A micropillars transitioned from homogeneous-like to shear band type as h decreased to the critical value of ～10 nm, which is indicative of a significant intrinsic size effect. The extrinsic size effect on the plastic deformation also became remarkable when h was less than ～10 nm, and the interplay between the intrinsic and extrinsic size effects leads to an ultrahigh strength of ～4.8 GPa in the C/A micropillars, which is close to the ideal strength of Cu and considerably greater than the ideal strength of the amorphous phase. The underlying strengthening mechanism was discussed, and the transition in deformation mode was quantitatively described by considering the strength discrepancy between the two constituent crystalline and amorphous layers at different length scales.     

Microstructure and texture development in hydrostatically extruded Mg–Al–Zn alloys during tensile testing at intermediate temperatures

Tensile testing of hydrostatically extruded round bars of AZ31 and AZ61 has been performed to analyse the flow behaviour as well as the microstructure and texture development as a function of temperature (175–225 °C) and strain rate (0.0001–0.01 s^?1). The post-testing microstructure is a result of dynamic recrystallization with varying significance of different texture components. In some cases the resulting textures are found to be similar to those textures that typically develop during extrusion of rare-earth-containing magnesium alloys. Dynamic recrystallization (DRX) and grain boundary sliding (GBS) are considered as the mechanisms that generate the changes in texture. Precipitates can exert a grain boundary pinning effect limiting grain growth. These different mechanisms contribute differently to the texture development if the testing parameters are changed.     

Nanocrystalline FeAl intermetallic produced by mechanical alloying followed by hot-pressing consolidation

In the present study mechanical alloying followed by hot-pressing consolidation has been used to obtain bulk nanocrystalline FeAl intermetallic compound. Nanocrystalline powder of Fe(Al) solid solution was the product of ball milling. This powder was sintered at 1000 °C for 180 s under a pressure of 7.7 GPa. Structural investigations of the consolidated material revealed that ordering of the Fe(Al) and its transformation into FeAl intermetallic occur during sintering and that the mean crystallite size of FeAl is 23 nm. The microhardness of the produced material is 1235 HV0.2, its density is 99.8% of theoretical value and its open porosity is 0%. The results obtained show that the quality of compaction with preserving nanometric grain size of the FeAl intermetallic is satisfactory and its microhardness is relatively high.     

Microstructure and tensile behavior of a friction stir processed magnesium alloy

In this work the effect of multi-pass friction stir processing (FSP) followed by warm pressing on an as-extruded ZK60 Mg plate was investigated. The microstructure, texture and resulting mechanical properties are reported here. Multi-pass FSP to partial depths on the top and bottom plate surfaces produced a novel, layered structure with three distinct microstructural zones associated with stirred, transition and core regions. In the stirred zone, FSP, followed by pressing at 200 °C, created a 0.8 μm ultrafine grain size which accounts for ～55 vol.% of the material. The transition region (～10 vol.%), showed extensively sheared coarse grains distributed in a matrix of finer grains. However, the core region (～35 vol.%) showed extensive twinning inside coarse grains in an overall bimodal microstructure reminiscent of extrusion. The processed Mg with a strong basal texture exhibited high yield strength (>300 MPa) and retention of adequate tensile ductility (>10%). The enhancement in mechanical properties of processed Mg is found to be highly influenced by the layered microstructure: UFG grained stirred zone, finer precipitates and strong basal texture.     

Microstructure changes during non-conventional heat treatment of thin Ni–Ti wires by pulsed electric current studied by transmission electron microscopy

Transmission electron microscopy, electrical resistivity measurements and mechanical testing were employed to investigate the evolution of microstructure and functional superelastic properties of 0.1 mm diameter as-drawn Ni–Ti wires subjected to a non-conventional heat treatment by controlled electric pulse currents. This method enables a better control of the recovery and recrystallization processes taking place during the heat treatment and accordingly a better control on the final microstructure. Using a stepwise approach of millisecond pulse annealing, it is shown how the microstructure evolves from a severely deformed state with no functional properties to an optimal nanograined microstructure (20–50 nm) that is partially recovered through polygonization and partially recrystallized and that has the best functional properties. Such a microstructure is highly resistant against dislocation slip upon cycling, while microstructures annealed for longer times and showing mostly recrystallized grains were prone to dislocation slip, particularly as the grain size exceeds 200 nm.     

Hardening of pure metals by high-pressure torsion: A physically based model employing volume-averaged defect evolutions

A physically based model to predict the increment of hardness and grain refinement of pure metals due to severe plastic deformation by high-pressure torsion (HPT) is proposed. The model incorporates volume-averaged thermally activated dislocation annihilation and grain boundary formation. Strengthening is caused by dislocations in the grain and by grain boundaries. The model is tested against a database containing all available reliable data on HPT-processed pure metals. It is shown that the model accurately predicts hardening and grain size of the pure metals, irrespective of crystal structure (face-centred cubic, body-centred cubic and hexagonal close packed). Measured dislocation densities also show good correlation with predictions. The influence of stacking fault energy on hardening is very weak (of the order of ?0.03 GPa per 100 J mol^?1).     

Formation of nanostructures in commercial-purity titanium via cryorolling

Microstructure evolution in commercial-purity titanium during plane-strain multipass rolling to a true thickness strain of 2.66 at 77 and 293 K was quantified. Deformation at both temperatures was accompanied by twinning. At 77 K, twinning was more extensive in terms of the fraction of twinned grains and the duration of the twinning stage. Rolling to a true thickness strain of 2.66 resulted in the formation of a microstructure with a grain/subgrain size of ～80 nm at 77 K or ～200 nm at 293 K. The contribution of various mechanisms to the strength of titanium following rolling at 77 and 293 K was analyzed quantitatively.     

Ductilisation of tungsten (W): On the shift of the brittle-to-ductile transition (BDT) to lower temperatures through cold rolling

Here we show that cold rolling decreased the brittle-to-ductile transitions (BDT) temperature of tungsten (W). Furthermore, we show that the BDT temperature correlates with the grain size (the smaller the grain size, the lower the BDT temperature) following a Hall–Petch-like equation. This relation between the grain size and the BDT temperature is well known from ferrous materials and is generally accepted in the steel community.Our ductilisation approach is the modification of the microstructure through cold rolling. In this work, we assess three different microstructures obtained from (i) hot-rolled, (ii) cold-rolled, and (iii) hot-rolled and annealed (1 h/2000 °C, annealed in H₂) tungsten plates. From these plates, Charpy impact test samples with dimensions of 1 × 3 × 27 mm³, without notch, were cut and tested in the L-S and T-S directions. The results show the following BDT temperatures: 675 °C/948 K (L-S, “annealed”), 375 °C/648 K (L-S, “hot-rolled”) and 125 °C/398 K (L-S, “cold-rolled”). The microstructure of the plates is analysed by means of SEM (EBSD: grain size, subgrains, texture, KAM), FIB (channelling contrast) and TEM analyses (bright field imaging).The question of how cold rolling decreases the BDT temperature is discussed against the background of (i) microcracking, crack branching, and crack bridging effects; (ii) texture effects; (iii) the role of dislocations; and (iv) the impact of impurities, micropores, and sinter pores. Our results suggest that the availability of dislocation sources (dislocation boundaries, grain boundaries; in particular, IDBs and HAGBs) is the most important parameter responsible for the increase of the cleavage resistance stress, σ_F, or the decrease of the BDT temperature, respectively.     

Texture evolution and mechanical properties of ion-irradiated Au thin films

Microstructure control of thin films is of particular importance for improving the reliability of microdevices in terms of electromigration, fatigue damage and hillocking. High-energy ion bombardment has turned out to be an appropriate modification instrument as it leads to selective grain growth, resulting in single-crystal-like structures. The current work addresses the effect of 7 MeV Au⁺ and 1.5 MeV N⁺ irradiation at high fluences (up to 45 × 10¹⁶ ions cm^?2) on the microstructure and the mechanical properties of 500 nm Au thin films of small initial grain size (70–90 nm). The following microstructure changes were observed: selective grain growth, texture changes, sputtering, interfacial degradation, formation of geometrically necessary dislocations, and defect clusters. Hardening behavior was found to be a consequence of grain growth (Hall–Petch effect) and the formation of ion-induced defects.     

Observations on the effect of a magnetic field on the annealing texture and microstructure evolution in zirconium

The effect of a magnetic field on the development of texture and microstructure in cold-rolled (80%) commercially pure zirconium (Zr701) was investigated. The specifically oriented sheet specimens were annealed at 550 °C for 15, 30 and 45 min and at 700 °C for 60, 90 and 180 min in a magnetic field of 19 T and 17 T, respectively. X-ray diffraction and electron backscatter diffraction measurements were used to characterize the crystallographic texture and the grain microstructure. The results revealed that the magnetic annealing promotes grain growth in the investigated material. This becomes apparent from the faster development of specific “grain growth” texture components and the bigger mean grain size after magnetic annealing. Magnetic annealing at 700 °C resulted in asymmetry of the two major texture components that constantly increased with annealing time. This effect is attributed to a magnetic driving force for grain growth arising from the anisotropic magnetic susceptibility of zirconium.