Uniaxial compression of fcc Au nanopillars on an MgO substrate: The effects of prestraining and annealing

The size-dependent strength of face-centered cubic (fcc) metals, as revealed by uniaxial compression of nanopillars, suggests that plasticity is dislocation source-controlled, with fewer sources in smaller pillars producing a “smaller is stronger” effect. To further investigate this phenomenon we have studied the effects of prestraining and annealing on the deformation properties of [0 0 1] Au nanopillars. By making pillars from an epitaxial film of [0 0 1] Au on [0 0 1] MgO, using focused ion beam machining, we are able to create both puck-shaped pillars that can be stably prestrained and pillars with a high aspect ratio, which can be tested in uniaxial compression. We find that prestraining dramatically reduces the flow strength of nanopillars while annealing restores the strength to the pristine levels. These unusual effects are not seen in bulk fcc metals, which behave in the opposite way. We discuss their possible causes in terms of dislocation densities using transmission electron microscopy.     

Deformation behaviour of an advanced nickel-based superalloy studied by neutron diffraction and electron microscopy

Deformation mechanisms under tensile loading at room temperature have been studied in a polycrystalline nickel-based superalloy containing close to 50 vol.% γ′. In order to identify the effect of γ′ particle size on deformation mechanisms, model microstructures with unimodal γ′ size distributions were developed. The investigations were carried out by combining in situ loading experiments using neutron diffraction and two-site elasto-plastic self-consistent plasticity modelling with detailed post-mortem electron microscopy. The microscopy work also includes results for samples strained at 500 °C. During early plastic deformation, the diffraction data demonstrate that γ and γ′ display the same elastic strain response, indicating that at this stage γ′ is cut by dislocations regardless of the γ′ particle size. Scanning electron microscopy studies showed an abundance of shearing processes in all three microstructures, hence supporting the conclusions drawn from the diffraction experiment. As the material is further deformed, elastic load transfer from γ to γ′ was observed in the medium (130 nm) and coarse (230 nm) γ′ microstructures but not in the fine (90 nm) γ′ microstructure. The load transfer can be explained by assuming that Orowan looping becomes an additional operative deformation mode. Transmission electron microscopy confirmed that in the fine γ′ microstructure deformation takes place by strongly coupled dislocations cutting the γ′, while the medium and coarse γ′ microstructures showed additional signs of Orowan looping.     

Hydrogen embrittlement of ferritic steels: Observations on deformation microstructure,nanoscale dimples and failure by nanovoiding

While hydrogen embrittlement of ferritic steels has been a subject of significant research, one of the major challenges in tackling hydrogen embrittlement is that the mechanism of embrittlement is not fully resolved. This paper reports new observations and interpretation of fracture surface features and deformation microstructures underneath the fracture surface, providing a mechanistic view of failure catalyzed by hydrogen. Linepipe grade ferritic steels were tested in air with electrochemically pre-charged hydrogen and in high-pressure H₂ gas. The fracture surface features were studied and compared using high-resolution surface-sensitive scanning electron microscopy, and the deformation microstructures just beneath the fracture surfaces were studied using transmission electron microscopy. Significant dislocation plasticity was observed just beneath both ductile and quasi-brittle fracture surfaces. Further, the dislocation activity just beneath the fracture surfaces was largely comparable with those observed in samples tested without hydrogen. Evidence for hydrogen-enhanced plastic flow localization and shear softening on the sub-micron scale was observed very near the final fracture surface (<2 μm) in the tensile samples. The quasi-brittle fracture surfaces were found to be covered with nanoscale dimples 5–20 nm wide and 1–5 nm deep. Based on analyses of conjugate fracture surfaces, most of the nanodimples appear to be “valley-on-valley” type, rather than “mound-on-valley” type, indicating nanovoid nucleation and growth in the plastically flowing medium prior to ultimate failure. Based on these observations, an alternative scenario of plasticity-generated, hydrogen-stabilized vacancy damage accumulation and nanovoid coalescence as the failure pathway for hydrogen embrittlement is proposed.     

The effect of pre-existing defects on the strength and deformation behavior of α-Fe nanopillars

The effects of two types of pre-existing defects, dislocations and clusters, on the strength and deformation behavior of body-centered cubic Fe nanopillars with a diameter of ～150 nm were investigated using in situ nanocompression in a transmission electron microscope. The plastic deformation of nanopillars containing high initial dislocation densities was observed to be relatively continuous, proceeding via a series of small- and intermediate-scale strain bursts that were associated with the movement/escape of dislocations and the formation of slip bands. Mechanical annealing was observed in nanopillars with high dislocation densities. When the dislocation density was reduced by in situ heating, the nanopillars were much stronger and the plastic deformation behavior transformed to a more abrupt and explosive mode. The introduction of a dispersion of solute atom clusters into nanopillars caused further strengthening as a higher stress level is required for dislocations to pass the clusters. The strengthening effect of cluster dispersion in nanopillars is comparable to that observed in the bulk steel. These phenomena are universal for Fe nanopillars with different crystallographic orientations.     

High temperature deformation behavior of the TC6 titanium alloy under the uniform DC electric field

High temperature deformation behavior of the TC6 titanium alloy under the uniform direct current (DC) electric field was investigated in this study. Based on the physical properties and the equilibrium phase diagrams calculated by the JMatPro metallic material analysis software, the effects of electric field on the mechanical properties of the TC6 and the underlying mechanism were analyzed. The results show that the ductility and failure strain of TC6 at 600 °C (around the recrystallization temperature) are improved about 100% due to the promotion effect of “electron wind” on the dislocation, showing a rather good potential for future practical applications. However, the ductility of TC6 is decreased when the electric field is applied at 900 °C because of its special effect on the phase transformation. Under the action of the DC electric field, the strength of TC6 increases about 15% at the temperature of 700–900 °C, indicating that the electric filed also affects the phase transformation within such temperature range. In addition, the elastic modulus of TC6 is decreased about 50% when the external electric field is applied at 600 °C. It is found for the first time that the electric field can change the elastic deformation behavior of metallic materials apparently under some special conditions.     

Synthesis,structural analysis and in situ transmission electron microscopy mechanical tests on individual aluminum matrix/boron nitride nanotube nanohybrids

Boron nitride nanotube (BNNT)/aluminum matrix composite nanohybrids were fabricated through magnetron sputtering of Al onto dispersed multiwalled BNNTs with average external diameters of 40–50 nm. Aluminum phase coating tightly wrapped the BNNTs after the deposition. The coating thickness in the range of 5–200 nm was controlled by changing sputtering time. Using imaging techniques and electron diffraction analysis in a transmission electron microscope, the Al phase was found to create nanocrystalline shields around individual BNNTs. The chemical states of the hybrid nanomaterials during the initial stages of sputtering were analyzed by X-ray photoelectron spectroscopy. Direct in situ bending and tensile tests on individual BNNT–Al nanocomposites were carried out by using a dedicated transmission electron microscope-atomic force microscope holder. In parallel, high-resolution TEM images and video recordings were taken for the analysis of deformation kinetics and fracture mechanisms. The nanohybrids with a suitably thick aluminum coating (～40 nm) withstood at least nine times higher stresses compared to a pure non-armed Al metal. This pioneering work opens up a prospective pathway for making ultralight and superstrong “dream” structural materials for future automotive and aerospace applications.     

Sample size matters for Al88Fe7Gd5 metallic glass: Smaller is stronger

For metallic single crystals with dimensions in the micrometer and sub-micrometer regime, systematic studies have established that sample size has an obvious influence on the apparent strength, following a “smaller is stronger” trend. For amorphous metals, several metallic glasses (MG) appear to exhibit a similar trend, while a few others do not. Here, another MG is examined, Al₈₈Fe₇Gd₅, using quantitative in situ tensile and compression tests inside electron microscopes, with sample effective diameter covering a wide range (100 nm to 3 μm). A clearly elevated strength is observed, as high as about twice the value of bulk samples, for samples with diameters approaching 100 nm. A size regime is proposed, where the strength is controlled by the nucleation of the shear band, starting from its embryonic stage: the smaller the sample size, the more difficult this nucleation becomes. The size dependence is also discussed from an energy balance perspective: the resulting simple power law fits the data as well as other published strength data for a number of MG systems.     

Microstructure and texture evolution during annealing a cryogenic-SPD processed Al-alloy with a nanoscale lamellar HAGB grain structure

The grain structure and texture evolution during annealing a Al–0.13% Mg submicron-grained alloy, deformed by plane-strain compression (PSC) at cryogenic temperatures, has been investigated by transmission electron microscopy and electron backscatter diffraction. After deformation the alloy contained a lamellar grain structure with a high-angle grain boundary (HAGB) spacing of 190 nm and an area fraction of ～80%. On annealing the grain structure coarsened and transformed from lamellar to equiaxed. Remarkably, the fraction of low-angle grain boundaries (LAGBs) progressively increased during annealing, to ～50% above 300 °C, leading to instability and discontinuous recrystallization at higher temperatures. This resulted in a “bimodal grain structure” comprised of bands of coarser grains and fine subgrains, arising as a result of the increase in proportion of lower-mobility LAGBs. The surprisingly large increase in LAGB fraction on annealing is shown to be related to orientation impingement, originating from the strong texture present after PSC in liquid nitrogen.     

Filling modes of polymer during submicron and nano-fabrication near glass transition temperature

In this study, we used a glass mold coated with TiN layer to fabricate submicron and nano-gratings on a PMMA (polymethylmethacrylate) film. The cavities on the mold, with sizes varying from 71 nm to 980 nm, was etched by ion beam. The deformation and filling modes of polymer during fabrication process were studied. Dual-peak deformations, which were considered as the characteristic filling modes of “viscous-dominant” polymer, were observed. Because our fabrication experiments were conducted near the glass transition temperature (T_g) of PMMA at which the polymer was “elastic–plastic-dominant”, the appearance of the dual-peak filling mode meant solid-state polymer might exhibit some characters of fluidic polymer at submicron and nano-scale. In addition, we presented a simple and effective mold release process at the end of this paper, which could reduce defects during molding release process.     

3-D Raman spectroscopy measurements of the symmetry of residual stress fields in plastically deformed sapphire crystals

The development of methods to characterize materials in three dimensions, such as tomography by X-rays, focused ion beam and electrons, has led to progress in the understanding of materials properties. Recently, even stress and deformation tensors could be measured in three dimensions. Specifically the stress fields around indents in metals were studied by three-dimensional (3-D) X-ray stress microscopy. In this paper, we investigate the 3-D residual stress field around a microindent using confocal Raman microscopy with a lateral resolution of 300 nm and a depth resolution of 600 nm. The model system investigated was single crystalline sapphire, which was indented normal to its basal c(0 0 0 1) plane. A cross-section of the indent was studied by transmission electron microscopy to visualize the deformed microstructure. The major result is that the geometry of the indenter has no direct influence on the symmetry of the resulting residual stress field. Residual stresses directly depend on the crystal symmetry and the defect structures formed during indentation. Confocal Raman microscopy is a powerful method for analyzing 3-D stress fields and the corresponding defect structures (by peak width analysis) with a resolution in the submicron range.     

Study of strain softening behavior of Al–Al3Sc multilayers using microcompression testing

Multilayer thin films with bilayer thicknesses in the nanometer range have been reported to have very high strengths. A previous study has shown that Al–Al₃Sc multilayers, with bilayer thicknesses as small as 6 nm, have hardnesses as high as ～3 GPa as measured by sharp tip nanoindentation. In the present study, we have avoided some of the complications associated with sharp tip nanoindentation by directly measuring the yield strengths and strain hardening/softening properties of Al–Al₃Sc multilayers using microcompression testing methods with a nanoindenter. The results show the expected trend of increasing yield strength with decreasing bilayer thickness, and compare favorably with estimates of the yield strengths based on sharp tip nanoindentation. During deformation, the Al–Al₃Sc multilayer pillars with smaller bilayer spacings experience considerable strain softening, resulting in a “flat-top mushroom” shape after deformation. We have developed a numerical model to account for this inhomogeneous deformation behavior and to calculate stress–strain relationships during strain softening. A new transmission electron microscopy study of a deformed pillar shows that the softening is a result of destruction of the layered structure due to shearing and rotation.     

Elastic instability condition of the raft structure during creep deformation in nickel-base superalloys

A condition for destabilizing the raft structure has been deduced from elastic energy calculations with the concept of “effective eigenstrain”, where the effect of creep deformation is included in addition to the lattice mismatch. The calculations indicate that the 0 0 1 raft structure is stabilized by a small amount of creep deformation but becomes unstable when the creep strain in the γ phase exceeds the magnitude required to fully relax the lattice mismatch. The excess creep strain is required to produce an internal elastic field that suppresses further creep deformation, and has to be introduced in the primary creep stage. Via the instability of the 0 0 1 raft structure, the raft structure gradually turns into a wavy one in the second creep stage before its collapse.     

Characterization of nickel-based microlattice materials with structural hierarchy from the nanometer to the millimeter scale

Novel nickel-based microlattice materials with structural hierarchy spanning three different length scales (nm, μm, mm) are characterized microstructurally and mechanically. These materials are produced by plating a sacrificial template obtained by self-propagating photopolymer waveguide prototyping. Ni–P films with a thickness of 120 nm to 3 μm are deposited by electroless plating, whereas thicker films (5–26 μm) are obtained by subsequent electrodeposition of a pure Ni layer. This results in cellular materials spanning three orders of magnitude in relative density, from 0.01% to 8.5%. The thin electroless Ni–P films have ultra-fine grain size (7 nm) and a yield strength of ～2.5 GPa, whereas the thicker electrodeposited Ni films exhibit a much broader distribution with average grain size of 116 nm and strong (1 0 0) texture in the plating direction, resulting in a yield strength of ～1 GPa. Uniaxial compression experiments reveal two distinct mechanical responses. At ultra-low densities (<0.1%), these lattices exhibit nearly full recovery after strains up to more than 50%, and damping coefficients an order of magnitude larger than for conventional Ni foams. At higher densities (0.1–10%), the compression behavior is fully plastic, similar to traditional cellular metals. A simple mechanical analysis reveals that the transition occurs when the thickness-to-diameter ratio of the truss elements is of the order of the yield strain of the material, in agreement with experimental observations. Optical and electron imaging of deformed lattices show that the deformation largely localizes around the nodes. In the ultra-light regime, the microlattice materials are stiffer and stronger than any existing alternative.     

High-temperature strength of compacted sub-micrometer aluminium powder

Aluminium powders with a mean particle size of around 1 μm were compacted by cold isostatic pressing (CIP) and additional forging. The specimens are characterized by hot compression tests, dilatometry and metallography. A 3D interconnected structure of alumina films <5 nm in thickness is observed by transmission electron microscopy and field emission gun scanning electron microscopy; it is associated with the natural oxide skin which covers every aluminium powder and occupies around 3 vol.%. The compression tests are carried out in the range of 350–520 °C at strain rates of 0.003–3 s^?1. The compressive strength was 100–150 and 130–180 MPa for the CIPed and forged samples, respectively. The low strain rate sensitivity m (<0.08) suggests that the alumina network forms a barrier, which suppresses any restoration mechanism across the grain boundaries as well as grain boundary sliding during hot deformation. The high strength of such compacted sub-micron Al powder is attributed to the conservation of a 3D alumina closed cell network filled with elastoplastic aluminium.     

Attraction of semiconductor nanowires: An in situ observation

In situ deformation transmission electron microscopy was used to study the attraction behavior of GaAs semiconductor nanowires (NWs). The NWs demonstrated an interesting phenomenon of either head-to-head or body-to-body attraction at distances that depend on the NW diameters. The NWs with a diameter of ～25 nm attracted at a distance of ～25 nm, while large-diameter NWs of ～55 nm showed no obvious attraction. The underlying mechanism governing the attraction of the NWs is proposed and discussed with a mechanistic model. The diameter dependence on the NW attraction behavior is discussed. The finding provides an understanding of the Ampère force in nanostructured materials caused by an electron-beam-induced current while technologically it provides useful hints for designing NW-based devices according to the diameter-dependent attraction behavior of NWs.     

Strengthening mechanisms in a high-strength bulk nanostructured Cu–Zn–Al alloy processed via cryomilling and spark plasma sintering

A bulk nanostructured alloy with the nominal composition Cu–30Zn–0.8Al wt.% (commercial designation brass 260) was fabricated by cryomilling of brass powders and subsequent spark plasma sintering (SPS) of the cryomilled powders, yielding a compressive yield strength of 950 MPa, which is significantly higher than the yield strength of commercial brass 260 alloys (～200–400 MPa). Transmission electron microscopy investigations revealed that cryomilling results in an average grain diameter of 26 nm and a high density of deformation twins. Nearly fully dense bulk samples were obtained after SPS of cryomilled powders, with average grain diameter 110 nm. After SPS, 10 vol.% of twins is retained with average twin thickness 30 nm. Three-dimensional atom-probe tomography studies demonstrate that the distribution of Al is highly inhomogeneous in the sintered bulk samples, and Al-containing precipitates including Al(Cu,Zn)–O–N, Al–O–N and Al–N are distributed in the matrix. The precipitates have an average diameter of 1.7 nm and a volume fraction of 0.39%. Quantitative calculations were performed for different strengthening contributions in the sintered bulk samples, including grain boundary, twin boundary, precipitate, dislocation and solid-solution strengthening. Results from the analyses demonstrate that precipitate and grain boundary strengthening are the dominant strengthening mechanisms, and the calculated overall yield strength is in reasonable agreement with the experimentally determined compressive yield strength.     

Prevalence of shear banding in compression of Zr41Ti14Cu12.5Ni10Be22.5 pillars as small as 150 nm in diameter

Recently, the size dependence of mechanical behaviors, particularly the yield strength and plastic deformation mode, of bulk metallic glasses (BMG) has created a great deal of interest. Contradicting conclusions have been drawn by different research groups, based on various experiments on different BMG systems. Based on in situ compression transmission electron microscopy (TEM) experiments on Zr₄₁Ti₁₄Cu_12.5Ni₁₀Be_22.5 (Vit 1) nanopillars, this paper provides strong evidence that shear banding still prevails at specimen length scales as small as 150 nm in diameter. This is supported by in situ and ex situ images of shear bands, and by the carefully recorded displacement bursts under load control as well as load drops under displacement control. Finite element modeling of the stress state within the pillar shows that the unavoidable geometry constraints accompanying such experiments impart a strong effect on the experimental results, including non-uniform stress distributions and high level hydrostatic pressures. The seemingly improved compressive ductility is believed to be due to such geometry constraints. Observations underscore the notion that the mechanical behavior of metallic glasses, including strength and plastic deformation mode, is size independent at least in Vit 1.     

Nanoindentation of porous bulk and thin films of La0.6Sr0.4Co0.2Fe0.8O3−δ

In this paper we show how reliable measurements on porous ceramic films can be made by appropriate nanoindentation experiments and analysis. Room-temperature mechanical properties of the mixed-conducting perovskite material La_0.6Sr_0.4Co_0.2Fe_0.8O_3?δ (LSCF6428) were investigated by nanoindentation of porous bulk samples and porous films sintered at temperatures from 900 to 1200 °C. A spherical indenter was used so that the contact area was much greater than the scale of the porous microstructure. The elastic modulus of the bulk samples was found to increase from 33.8 to 174.3 GPa and hardness from 0.64 to 5.32 GPa as the porosity decreased from 45% to 5% after sintering at 900–1200 °C. Densification under the indenter was found to have little influence on the measured elastic modulus. The residual porosity in the “dense” sample was found to account for the discrepancy between the elastic moduli measured by indentation and by impulse excitation. Crack-free LSCF6428 films of acceptable surface roughness for indentation were also prepared by sintering at 900–1200 °C. Reliable measurements of the true properties of the films were obtained by data extrapolation provided that the ratio of indentation depth to film thickness was in the range 0.1–0.2. The elastic moduli of the films and bulk materials were approximately equal for a given porosity. The 3-D microstructures of films before and after indentation were characterized using focused ion beam/scanning electron microscopy tomography. Finite-element modelling of the elastic deformation of the actual microstructures showed excellent agreement with the nanoindentation results.     

Effect of strain rate on microstructure of polycrystalline oxygen-free high conductivity copper severely deformed at liquid nitrogen temperature

The microstructure of polycrystalline oxygen-free high conductivity copper subjected to severe uniaxial single compression at liquid nitrogen temperature and strain rates ranging from 10^?2 to 10⁵ s^?1 is characterized using transmission electron microscopy, X-ray diffraction and differential scanning calorimetry. A difference in strain rate leads to a change in the density, character and arrangement of dislocations, as well as the size and configuration of dislocations cells/(sub)grains in the deformed sample. A threshold strain rate of 10³ s^?1 is identified for the formation of localized deformation bands, which characterizes heterogeneity of deformation at high strain rates. These bands are composed of grains that are significantly smaller than those outside them, as well as those obtained at strain rates lower than 10³ s^?1. Under particular conditions, grains as small as several nanometers can be generated in the vicinity of these bands, through the activation of rotational dynamic recrystallization. Amorphization is identified as a deformation mechanism in structures consisting of grains smaller than ～13 nm, and this offers an explanation for the “inverse Hall–Petch effect”. A model that illustrates the initiation and propagation of an amorphous phase during deformation is proposed. Deformed samples exhibit the tendency of an increase in strength with the value of the Zener–Hollomon parameter, which captures strain rate and temperature rise during deformation. This study suggests that a strain rate in the order of 10² s^?1 should be adopted in severe plastic deformation techniques to produce nanometer-sized grains.     

In situ TEM straining of single crystal Au films on polyimide: Change of deformation mechanisms at the nanoscale

In situ transmission electron microscopy straining experiments were performed on 40, 60, 80 and 160 nm thick single crystalline Au films on polyimide substrates. A transition in deformation mechanisms was observed with decreasing film thickness: the 160 nm thick film deforms predominantly by perfect dislocations while thinner films deform mainly by partial dislocations separated by stacking faults. In contrast to the 160 nm thick film, interfacial dislocation segments are rarely laid down by threading dislocations for the thinner films. At the late stages of deformation in the thicker Au films prior to fracture, dislocations start to glide on the (0 0 1) planes (cube-glide) near the interface with the polymer substrate. The impact of size-dependent dislocation mechanisms on thin film plasticity is addressed.