Microstructural, texture, plastic anisotropy and superplasticity development of ZK60 alloy during equal channel angular extrusion processing

In this study, equal channel angular pressing (ECAP) was exploited to refine the grain size of a ZK60 magnesium alloy in multi-processing steps, namely at temperatures of 250˚C, 200˚C and 150˚C, producing an ultrafine-grained (UFG) structure. The microstructural development and texture evolution during ECAP were systemically investigated by electron backscattered diffraction (EBSD) analysis. The microstructure of the ECAP processed alloy was remarkably refined to an average grain size of 600 nm. During ECAP process the original fiber texture of the as-extruded alloy was gradually weakened and eventually replaced by a stronger texture component coinciding with ECAP shear plane. The ECAP processed material showed a proper balance of tensile as well as compression strength and tensile ductility at room temperature. Yield strength of 273 and 253 MPa in tension and compression, respectively, ultimate tensile strength of 298 MPa and fracture elongation of about 30% were obtained in the UFG alloy. A transition from ductile–brittle to ductile fracture consisting of very fine and equiaxed dimples was also found in the ECAP processed material. Compared to the as-received alloy, a combination of grain refinement and texture development in the UFG alloy gave rise to a notable reduction in mechanical asymmetric behavior at room temperature. The superplastic behavior of the as-extruded and ECAP processed alloy was also investigated at 200˚C with strain rate of 1.0×10-3 s-1. The concurrent effect of grain boundary sliding and favorable basal texture in the UFG alloy led to an achievement of elongation value of about 300% while, under similar testing conditions, the elongation of about 140% was obtained in the as-extruded alloy

Origin of improved tunability and loss in N2 annealed barium strontium titanate films

Barium strontium titanate (BSTO) thin films were deposited on Pt(111) by high throughput evaporative physical vapor deposition and then annealed at 650 °C for 30 min under N2 atmosphere. Using advanced transmission electron microscopy, energy-dispersive x-ray spectroscopy and electron energy-loss spectroscopy, we directly show that not only does N substitute for O in the BSTO lattice but that it also compensates for Ti3+ ions, suppressing conductivity, thereby reducing dielectric loss and enhancing dielectric tunability. However, this effect is negated near the film edge where we speculate that exposed Pt acts as a reservoir of adsorbed/absorbed O and alters the local N2 concentration during annealing

Tailoring the mechanical and degradation performance of Mg-2.0Zn-0.5Ca-0.4Mn alloy through microstructure design

A novel Mg-2.0Zn-0.5Ca-0.4Mn alloy has been formulated and processed through melt spinning and hot extrusion to enhance its mechanical and degradation properties. Microstructural characterization of rapidly solidified alloy ribbons consolidated by extrusion revealed a fine and fully recrystallized microstructure with average size of 4 µm. The conventionally extruded alloy consisted of several course second-phase strips as coarse as 100 µm, while the extrusion-consolidated ribbons were devoid of any second phases larger than 100 nm. Rapid solidification followed by extrusion processing resulted in significantly randomized texture where the majority of the basal planes were tilted toward transverse and extrusion directions. Such a weak texture resulted in higher activity of basal planes and thereby considerably improved the fracture elongation from 4% to 19%, while retaining relatively high tensile strength of 294 MPa. In addition to high strength and ductility due to the reduced activity of deformation twining during compression, the extrusion-consolidated alloy ribbons showed lower yielding asymmetric ratio than that measured for the conventionally extruded alloy (1.25 versus 1.61). Electrochemical measurements and immersion tests indicated that application of rapid solidification followed by extrusion remarkably reduced the corrosion rate from 2.49 mm/year to 0.37 mm/year due to recrystallization completion and suppression of coarse second-phase formation

Wear induced ripplocation during dry sliding wear of TiC-based composite

Monolithic TiC and TiC particulate ceramic composite containing 30 and 50 mol.%SiC were consolidated and synthesized using spark plasma sintering (SPS) without sintering aids. The as-sintered bulk samples microstructural evolution and dry sliding room-temperature tribological properties against Al2O3 ball were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Raman analysis. The role of coefficient of thermal expansion (CTE) mismatch between TiC and SiC as well as cubic to hexagonal SiC phase transformation on the evolution of residual stresses in the composite was also investigated. The friction and wear properties of the monolithic TiC were superior to that of the composite with frictional heating-induced tribo-oxidation playing a dominant role in the wear mechanism. The increase in friction and wear of the composite is attributed to wear-induced stress-relaxation of the previously trapped residual stresses in the composite leading to extensive ripplocation of the TiC grains and consequent SiC grain pull-outs. Herein, we report for the first time on the wear-induced mechanical exfoliation of carbon, its subsequent decomposition into graphite and eventual deformation by micromechanism involving nucleation and propagation of ripples

Towards revealing key factors in mechanical instability of bioabsorbable Zn-based alloys for intended vascular stenting

Zn-based alloys are recognized as promising bioabsorbable materials for cardiovascular stents, due to their biocompatibility and favorable degradability as compared to Mg. However, both low strength and intrinsic mechanical instability arising from a strong strain rate sensitivity and strain softening behavior make development of Zn alloys challenging for stent applications. In this study, we developed binary Zn-4.0Ag and ternary Zn-4.0Ag-xMn (where x = 0.2–0.6wt%) alloys. An experimental methodology was designed by cold working followed by a thermal treatment on extruded alloys, through which the effects of the grain size and precipitates could be thoroughly investigated. Microstructural observations revealed a significant grain refinement during wire drawing, leading to an ultrafine-grained (UFG) structure with a size of 700 nm and 200 nm for the Zn-4.0Ag and Zn-4.0Ag-0.6Mn, respectively. Mn showed a powerful grain refining effect, as it promoted the dynamic recrystallization. Furthermore, cold working resulted in dynamic precipitation of AgZn3 particles, distributing throughout the Zn matrix. Such precipitates triggered mechanical degradation through an activation of Zn/AgZn3 boundary sliding, reducing the tensile strength by 74% and 57% for Zn-4.0Ag and Zn-4.0Ag-0.6Mn, respectively. The observed precipitation softening caused a strong strain rate sensitivity in cold drawn alloys. Short-time annealing significantly mitigated the mechanical instability by reducing the AgZn3 fraction. The ternary alloy wire showed superior microstructural stability relative to its Mn-free counterpart due to the pinning effect of Mn-rich particles on the grain boundaries. Eventually, a shift of the corrosion regime from localized to more uniform was observed after the heat treatment, mainly due to the dissolution of AgZn3 precipitates. Statement of Significance Owing to its promising biodegradability, zinc has been recognized as a potential biodegradable material for stenting applications. However, Zn's poor strength alongside intrinsic mechanical instability have propelled researchers to search for Zn alloys with improved mechanical properties. Although extensive researches have been conducted to satisfy the mentioned concerns, no Zn-based alloys with stabilized mechanical properties have yet been reported. In this work, the mechanical properties and stability of the Zn-Ag-based alloys were systematically evaluated as a function of microstructural features. We found that the microstructure design in Zn alloys can be used to find an effective strategy to not only improve the strength and suppress the mechanical instability but also to minimize any damage by augmenting the corrosion uniformity

Characterizing oxygen atoms in perovskite and pyrochlore oxides using ADF-STEM at a resolution of a few tens of picometers

We present an aberration corrected scanning transmission electron microscopy (ac-STEM) analysis of perovskite (LaFeO3) and pyrochlore (Yb2Ti2O7 and Pr2Zr2O7) oxides and demonstrate that both the shape and contrast of visible atomic columns in annular dark-field (ADF) images are sensitive to the presence of nearby atoms of low atomic number (e.g. oxygen). We show that point defects (e.g. oxygen vacancies), which are invisible – or difficult to observe due to limited sensitivity – in x-ray and neutron diffraction measurements, are the origin of the complex magnetic ground state of pyrochlore oxides. In addition, we present a method by which light atoms can be resolved in the quantitative ADF-STEM images. Using this method, we resolved oxygen atoms in perovskite and pyrochlore oxides and propose this method to be suitable for other materials containing both light and heavy elements

High quality factor cold sintered Li2MoO4BaFe12O19 composites for microwave applications

Ceramics-ceramic composites in series (1-x)Li2MoO4-xBaFe12O19 (LMO-BF12, 0.00 ≤ x ≤ 0.15) have been cold sintered at 120 °C and their structure and properties characterized. X-ray diffraction, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) confirmed that compositions were dual phase and had a dense microstructure. Composites in the xBF12-(1-x)LMO (0.0 ≤ x ≤ 0.15) series resonated at MW frequencies (∼6 GHz) with 5.6≤εr ≤ 5.8 and Qf = 16,000–22,000 GHz, despite the black colour of compositions with x > 0. The permeability of the composites was measured in the X band (∼8 GHz) and showed an increase from 0.94 (x = 0.05) to 1.02 (x = 0.15). Finite element modelling revealed that the volume fraction of BF12 dictates the conductivity of the material, with a percolation threshold at 10 vol% BF12 but changes in εr as a function of x were readily explained using a series mixing model. In summary, these composites are considered suitable for the fabrication of dual mode or enhanced bandwidth microstrip patch antennas

Synthesis and microstructural evolution in ternary metalloceramic Ti3SiC2 consolidated via the Maxthal 312 powder route

A bulk specimen containing Ti3SiC2, TiSi2 and TiC was prepared through an in situ spark plasma sintering/solid-liquid reaction powder metallurgy method using the Maxthal 312 (nominally-Ti3SiC2) powder as a starting material. The reaction mechanism, phase constituents and evolution of the microstructure were systematically investigated by X-ray diffraction (XRD), optical microscopy, scanning electron microscopy (SEM) equipped with energy dispersive spectroscopy (EDS) system, transmission electron microscopy (TEM), Raman spectroscopy, differential scanning calorimetry (DSC) and Vickers microhardness testing. Phase analysis and microstructural characterization revealed that the bulk sample contained binary ancillary phases, possibly due to Si evaporation and/or carburization. The deformed microstructure around the indents revealed evidence of plasticity, intrinsic lubricity and toughening. The Microstructural and orientation relationships between the phases contained in the bulk sample are reported

Atomic structure study of the pyrochlore Yb₂Ti₂O₇ and its relationship with low-temperature magnetic order

There has been great interest in the magnetic behavior of pyrochlore oxides with the general formula A2B2O7, in which rare-earth (A) and transition metal (B) cations are ordered on separate interpenetrating lattices of corner-sharing tetrahedra. Such materials exhibit behaviors including quantum spin-ice, (quantum) spin-liquid, and ordered magnetic ground states. Yb2Ti2O7 lies on the boundary between a number of competing magnetic ground states. Features in the low-temperature specific heat capacity that vary in sharpness and temperature from sample to sample suggest that, in some cases, the magnetic moments order, while in others, the moments remain dynamic down to temperatures as low as ∼16 mK. In this paper, three different Yb2Ti2O7 samples, all grown by the optical floating zone technique but exhibiting quite different heat capacity behavior, are studied by aberration-corrected scanning transmission microscopy (STEM). Atomic-scale energy-dispersive x-ray analysis shows that a crystal with no specific heat anomaly has substitution of Yb atoms on Ti sites (stuffing). We show that the detailed intensity distribution around the visible atomic columns in annular dark field STEM images is sensitive to the presence of nearby atoms of low atomic number (in this case oxygen) and find significant differences between the samples that correlate both with their magnetic behavior and measurements of Ti oxidation state using electron energy loss spectroscopy. These measurements support the view that the magnetic ground state of Yb2Ti2O7 is extremely sensitive to disorder

High electromechanical response in the non morphotropic phase boundary piezoelectric system PbTiO3-Bi(Zr1/2Ni1/2)O-3

There is a general perception that a large piezoelectric response in ferroelectric solid solutions requires a morphotropic/polymorphic phase boundary (MPB/PPB), i.e., a composition driven interferroelectric instability. This correlation has received theoretical support from models which emphasize field driven polarization rotation and/or interferroelectric transformations. Here, we show that the ferroelectric system ( 1 − x ) PbTi O 3 − ( x ) Bi ( Zr 1 / 2 Ni 1 / 2 ) O 3 (PT-BNZ), which shows d 33 ( ∼ 400 p C / N ) comparable to the conventional MPB/PPB systems, does not belong to this category. In the unpoled state the compositions of PT-BNZ showing large d 33 exhibit a coexistence of tetragonal and cubiclike (CL) phases on the global length scale. A careful examination of the domain strucures and global structures (both in the unpoled and poled states) revealed that the CL phase has no symptom of average rhombohedral distortion even on the local scale. The CL phase is rather a manifestation of tetragonal regions of short coherence length. Poling increases the coherence length irreversibly which manifests as poling induced CL → P 4 m m transformation on the global scale. PT-BNZ is therefore qualitatively different from the conventional MPB piezoelectrics. In the absence of the composition and temperature driven interferroelectric instability in this system, polarization rotation and interferroelectric transformation are no longer plausible mechanisms to explain the large electromechanical response. The large piezoelectricity is rather associated with the increased structural-polar heterogeneity due to domain miniaturization without the system undergoing a symmetry change. Our study proves that attainment of large piezoelectricity does not necessarily require interferroelectric instability (and hence morphotropic/polymorphic phase boundary) as a criterion