Flash-sintered (FS) ceramics have shown promising mechanical deformability at room temperature compared to conventional sintered ceramics. One major contributing factor to plasticity is high-density defects, such as dislocations, stacking faults and point defects, resulted presumably from the high electrical field during flash sintering. However, such direct experiemtnal evidence for defect formation and evolution under the electric field remains lacking. Here we performed in situ biasing experiments in FS and conventionally sintered (CS) polycrystalline TiO2 in a transmission electron microscope (TEM) to compare the defect evolution dynamics. In situ TEM studies revealed the coalescence of point defects under the electrical field in both FS and CS TiO2 and the subsequent formation of stacking faults, which are often referred to as Wadsley defects. Surprisingly, under the electrical field, the average fault growth rate in the FS samples is 10 times as much as that in the CS TiO2. Furthermore, the Magnéli phase, a 3D oxygen-deficient phase formed by the aggregation of Wadsley defects, is observed in the FS samples, but not in the CS samples. The present study provides new insights into defect dynamics in FS ceramics.

We have studied the high-pressure compression behavior of molybdenum up to 60 GPa by synchrotron radial x-ray diffraction（RXRD） in a diamond anvil cell（DAC）. It is found that all diffraction peaks of molybdenum undergo a split at around 27 GPa, and we believe that a phase transition from a body-centered cubic structure to a rhombohedral structure at room pressure has occurred. The slope of pressure–volume curve shows continuity before and after this phase transition,when fitting the pressure–volume curves of the body-centered cubic structure at low pressure and the rhombohedral structure at high pressure. A bulk modulus of 261.3（2.7） GPa and a first-order derivative of the bulk modulus of 4.15（0.14） are obtained by using the nonhydrostatic compression data at the angle ψ = 54.7°between the diffracting plane normal and stress axis.

Twin boundaries have enabled unique mechanical and physical properties in metallic materials. However, growth twins are rarely observed in Al due to its high stacking fault energy. In this study, we report on the synthesis of high-density growth twins in sputtered Al/Mg multilayer films. The formation mechanisms of incoherent and coherent twin boundaries are discussed. Besides, the incoherent twin boundary related structure, 9R phase, was also identified. This study highlights an effective method to elevate the twin /9R phase density in metals with high stacking fault energy.

Although intermetallics are attractive for their high strength, many of them are often brittle at room temperature, thereby severely limiting their potential as structural materials. Here, we report on a previously unidentified deformable nanocrystalline CoAl intermetallics with Co-rich thick grain boundaries (GBs). In situ micropillar compression studies show that nanocrystalline CoAl with thick GBs exhibits ultrahigh yield strength, exceeding 4.5 gigapascals. Unexpectedly, nanocrystalline CoAl intermetallics also show prominent work hardening to a flow stress of 5.7 gigapascals up to 20% compressive strain. Transmission electron microscopy studies show that deformation induces abundant dislocations inside CoAl grains with thick GBs, which accommodate plastic deformation. Molecular dynamics simulations reveal that the Co-rich thick GBs play a vital role in promoting nucleation of dislocations at the Co/CoAl interfaces, thereby enhancing the plasticity of the intermetallics. This study provides a perspective to promoting the plasticity of intermetallics via the introduction of thick GBs.

Recent works of epitaxial nanotwinned metals and alloys with different stacking fault energies are reviewed to elaborate the relationship among synthesis conditions, intrinsic factors, twin structure and various properties.

Recent experimental studies show that co-sputtering solutes with Al, together, can refine columnar grain size around few tens of nanometers and promote the formation and enhance the stability of planar defects such as stacking faults (SFs) and grain boundaries (GBs) in Al alloys. These crystal defects and fine columnar grains result in high strength, enhanced strain hardening and thermal stability of Al alloys. Using first-principles density-functional theory (DFT) calculations, we studied the role of eleven solutes in tailoring kinetics and energetics of adatoms and clusters on Al {111} surface, stable and unstable stacking fault energies, and kinetic energy barriers for the migration of defects. The calculations show that most solutes can effectively refine columnar grain size by decreasing the diffusivity of adatoms and surface clusters. These solutes do not necessarily decrease the stacking fault energy of Al alloys, but reduce the formation energy of faulted surface clusters and increase the energy barriers for the recovery of faulted surface clusters. Correspondingly, the formation of SFs is kinetically promoted during sputtering. Furthermore, solutes are segregated into the core of Shockley partial dislocations and play a pinning effect on SFs, SF arrays and twin boundaries, enhancing the thermal stability of these crystal defects. These findings provide insights into the design of high-strength Al alloys for high-temperature applications.

Nanotwinned Al/Ti multilayers have exhibited size-dependent microstructure evolution and high strength. However, their deformation mechanisms are less well understood. In this work, we investigated the deformation mechanisms of nanotwinned Al/Ti multilayers with FCC/HCP layer interfaces by using in situ micropillar compression tests. Nanotwinned Al/Ti multilayers exhibit compressive strength up to 2.4 GPa and good work hardening capability. Post-compression TEM analyses reveal high-density stacking faults and the HCP-to-FCC phase transformations in Ti. Molecular dynamics simulations elucidate the mechanisms of deformation induced phase transformation in Ti and the influence of collective movement of partial dislocations on the deformability of Al/Ti multilayers.

The mechanical strength of commercial Al alloys rarely exceeds 700 MP. Recent studies show that nanotwinned Al alloys and other nanocolumnar metals exhibit superb mechanical behaviors but a discrepancy between tensile and hardness measurements often emerges and their orientation dependent deformation mechanisms remain unclear. Here, we inspect the mechanical response of columnar nanotwinned Al-Fe alloys with emphasis on response of grain boundaries to in-situ tension and compression tests along both in-plane and out-of-plane directions inside a scanning electron microscope. Our studies reveal ultra-high out-of-plane tensile and compressive stress, exceeding 1.8 GPa, and an in-plane tensile and compressive stress of 1.1 and 1.6 GPa, respectively. Post-mortem TEM analyses were performed to elucidate the orientation-dependent plastic anisotropy and tension-compression asymmetry in columnar nanotwinned Al-Fe alloys. This study provides an important forward step towards the understanding of deformation mechanisms in high-strength nanotwinned Al alloys and metals with nanocolumnar or non-equiaxed grains.

Three tungsten powder samples—one coarse grained (c-W; grain size: 1 µm–3 µm) and two nanocrystalline (n-W; average grain sizes: 10 nm and 50 nm)—are investigated under nonhydrostatic compression in a diamond anvil cell in separate experiments, and their in situ X-ray diffraction patterns are recorded. The maximum microscopic deviatoric stress in each tungsten sample, a measure of the yield strength, is determined by analyzing the diffraction line width. Over the entire pressure range, the strength of tungsten increases noticeably as the grain size is decreased from 1 µm–3 µm to 10 nm. The results show that the yield strength of tungsten with an average crystal size of 10 nm is around 3.5 times that of the sample with a grain size of 1 µm–3 µm.

To raise mechanical strength of metallic materials, methods such as grain refinement and amorphization are usually utilized but sacrifice plasticity. Strength and plasticity are largely dictated by dislocation-defect interactions in crystalline materials and by shear banding in metallic glasses, depending significantly on the length scales of microstructural features. Here we report on the evolution of microstructures and multistage phase transformations from micro/nanocrystalline to an entirely amorphous structure, realized by tailoring the composition of Cr in co-sputtered Al100 xCrx (x = 0-25 at%) alloys. The associated Cr segregation caused the formations of different dual-phase nanocomposites. In-situ micromechanical experiments revealed that the flow stress of Al-Cr alloys can reach 2.4 GPa and the deformation behaviors varied drastically with Cr composition. This study established the mechanistic connection between the Cr composition-dependent evolution of microstructure and ultrahigh strength as well as plasticity, and revealed the benefits of building nanocomposites through a multistage phase transformation to improve the plasticity of nanocrystalline and amorphous materials.

Layer thickness dependent mechanical behaviors of metallic nanolaminates have been extensively investigated. In a recent study [1], we show that a particular defect network, consisting of layer interface, stacking faults and twin boundaries, plays an important role in achieving high strength in Cu/Co multilayers. Here, we report a follow-up study on the effect of layer thickness on this unique interplay of defect networks. To this end, we investigate the mechanical behavior of highly textured Cu (111)/Co (0002) multilayers with individual layer thickness of 5, 25 and 100 nm. In situ micropillar compression tests show that the Cu/Co 25 nm multilayers have a much higher strength than 100 nm and 5 nm multilayers. Post-deformation TEM analyses and MD simulations reveal the layer thickness dependent variations of defect density dominating the strengthening effect in multilayers. This study provides new perspectives on optimal defect networks for the design of high strength, deformable metallic materials.

The equation of state (EOS) of Cr3C2 at high pressure is studied by the synchrotron radiation x-ray diffraction (XRD) in a diamond anvil cell (DAC) at ambient temperature, and density functional theory (DFT). The XRD analysis shows that the orthorhombic structure is maintained to a maximum pressure of 44.5 GPa. The XRD data show that the bulk modulus is K-0= 292 (18) GPa with K-0 '=3.25(0.85). In addition, the high-pressure compression behavior of Cr3C2 is studied by first principles calculations. The obtained bulk modulus of Cr(3)C(2)is 323 (1) GPa.

ZnS has been widely used as an infrared optical material due to its superb optical properties, but its mechanical properties are less well understood. In this study, we investigated the size-dependent mechanical behavior of vacuum hot-pressed ZnS micropillars with a diameter of 3, 1.5, and 0.5 μm by in-situ microcompression tests in a scanning electron microscope. A clear size effect was observed. The 3 μm micropillars showed the highest variability of stress-strain behavior. Whereas the 0.5 μm pillars exhibited higher flow stress and improved strain-hardening capability to a compressive strain of ~10%. Post-mortem microscopy analyses coupled with ASTAR crystal orientation mapping suggest that plastic deformation is accommodated by stress-induced wurtzite-to-sphalerite phase transformation and the formation of abundant stacking faults and deformation twins. Meanwhile, the substantial strain hardening derives from preexisting stacking faults, twin boundaries, and grain boundaries that hinder the propagation of partial dislocations. This study provides a fresh perspective on the design of ceramic materials with high strength and plastic flow ability.

Nanoprecipitates or grain refinement can effectively enhance the mechanical strength of Al alloys, but the room-temperature strengths of precipitation hardened and nanocrystalline Al alloys often fall below 1 GPa. Furthermore, they are largely plagued by precipitous mechanical softening at elevated temperature below 300°C, mostly due to degraded microstructural stability. Here, we report a mechanism of coupled solute effect in nanotwinned Al-Fe-Ti alloys that enables stability of nanograins up to 400°C and an unprecedented high-temperature flow stress of ~ 1.7 GPa at 300°C. The supersaturated Fe solutes in Al act as effective grain refiner, forming superstrong solid solution alloys. More importantly, empirical evidence combined with first principle calculations indicate that the Ti solutes delay the agglomeration of Fe solutes, thereby remarkably extending the temperature window for the stability of nanograins in nanotwinned Al alloys. This study highlights the opportunity to design ultrastrong and stable nanostructured alloys for potential high temperature applications via a coupled solute effect.

Aluminum (Al) alloys have a multitude of applications, notably in the automotive, aerospace and coating industries, yet they exhibit significantly lower mechanical strength than conventional steels. Nanotwins drastically improve mechanical strength while retaining ductility. However, the high SFE of Al largely prevents twinning. Here, we synthesize Al-Zr alloy films containing an abundance of incoherent twin boundaries and 9R phases. These alloys exhibit an extended solid solubility of Zr, retaining a columnar nanotwinned structure across all compositions. These films reach a hardness up to 4.2 GPa with 10 at% Zr and demonstrate the capacity for producing strong Al alloys with nanotwins.

To investigate the role of interlayers on the growth, microstructure, and physical properties of 3D nanocomposite frameworks, a set of novel 3D vertically aligned nanocomposite (VAN) frameworks are assembled by a relatively thin interlayer (M) sandwiched by two consecutively grown La 0.7 Sr 0.3 MnO 3 (LSMO)‐ZnO VANs layers. ZnO nanopillars from the two VAN layers and the interlayer (M) create a heterogeneous 3D frame embedded in the LSMO matrix. The interlayer (M) includes yttria‐stabilized zirconia (YSZ), CeO 2 , SrTiO 3 , BaTiO 3 , and MgO with in‐plane matching distances increasing from ≈3.63 to ≈4.21 Å, and expected in‐plane strains ranging from tensile (≈8.81% on YSZ interlayer) to compressive (≈–6.23% on MgO interlayer). The metal‐insulator transition temperature increases from ≈133 K (M = YSZ) to ≈252 K (M = MgO), and the low‐field magnetoresistance peak value is tuned from ≈36.7% to ≈20.8%. The 3D heterogeneous frames empower excellent tunable magnetotransport properties and promising potentials for microstructure‐enabled applications.

Al alloys have widespread industrial applications. However, their mechanical strength is often much lower than steels. Here, we investigate the influence of solutes on achieving ultrahigh strength and thermal stability of nanotwinned Al alloys. In situ micropillar compression tests show the addition of a small amount of Ti can significantly increase the mechanical strength of Al-Ni alloys to 2 GPa. Deformation induced detwinning, Ni segregation and grain coarsening as discovered in binary Al-Ni alloys are mostly absent in the ternary Al-Ni-Ti alloys. Moreover, the ternary Al-Ni-Ti alloys have outstanding thermal stability. Density function theory calculations reveal the synergetic pinning effect of Ni-Ti solute pairs on incoherent twin boundaries. This study demonstrates that the proper selection of synergistic solute pairs is critical to improve the thermal stability and mechanical properties of nanotwinned Al alloys.

Deformation twinning and dislocation glide are two primary deformation mechanisms in hexagonal close packed (HCP) metals. Here we show, via in situ micropillar compression tests, that HCP Co pillars with high-density stacking faults exhibit a high yield strength and significant plasticity. Transmission electron microscopy studies reveal the formation of extensive face-centered cubic (FCC) Co phase after deformation. Molecular dynamics simulations confirm the deformation induced phase transformation, and shed light on the deformation mechanisms in HCP Co with pre-existing stacking faults. This study provides new insights into achieving high strength and plasticity in HCP metals via stacking faults and phase transformation.

High-density growth nanotwins enable high-strength and good ductility in metallic materials. However, twinning propensity is greatly reduced in metals with high stacking fault energy. Here we adopted a hybrid technique coupled with template-directed heteroepitaxial growth method to fabricate single-crystal-like, nanotwinned (nt) Ni. The nt Ni primarily contains hierarchical twin structures that consist of coherent and incoherent twin boundary segments with few conventional grain boundaries. In situ compression studies show the nt Ni has a high flow strength of ∼2 GPa and good deformability. Moreover, the nt Ni has superb corrosion behavior due to the unique twin structure in comparison to coarse grained and nanocrystalline counterparts. The hybrid technique opens the door for the fabrication of a wide variety of single-crystal-like nt metals with unique mechanical and chemical properties.