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Achieving an optimal balance between strength and ductility in advanced engineering materials has long been a challenge for researchers. In the field of material strengthening, most approaches that prevent or impede the motion of dislocations involve ductility reduction. In the present study, we propose a strengthening approach based on spinodal decomposition in which Cu and Al are introduced into a ferrous medium-entropy alloy. The matrix undergoes nanoscale periodic spinodal decomposition via a simple one-step aging procedure. Chemical fluctuations within periodic spinodal decomposed structures induce spinodal hardening, leading to a doubled strengthening effect that surpasses the conventional precipitation strengthening mechanism. Notably, the periodic spinodal decomposed structures effectively overcome strain localization issues, preserving elongation and doubling their mechanical strength. Spinodal decomposition offers high versatility because it can be implemented with minimal elemental addition, making it a promising candidate for enhancing the mechanical properties of various alloy systems.
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Chemical short-range order in disordered solid solutions often emerges with specific heat treatments. Unlike thermally activated ordering, mechanically derived short-range order (MSRO) in a multi-principal-element Fe40Mn40Cr10Co10 (at%) alloy originates from tensile deformation at 77 K, and its degree/extent can be tailored by adjusting the loading rates under quasistatic conditions. The mechanical response and multi-length-scale characterisation pointed to the minor contribution of MSRO formation to yield strength, mechanical twinning, and deformation-induced displacive transformation. Scanning and high-resolution transmission electron microscopy and the anlaysis of electron diffraction patterns revealed the microstructural features responsible for MSRO and the dependence of the ordering degree/extent on the applied strain rates. Here, we show that underpinned by molecular dynamics, MSRO in the alloys with low stacking-fault energies forms when loaded at 77 K, and these systems that offer different perspectives on the process of strain-induced ordering transition are driven by crystalline lattice defects (dislocations and stacking faults).
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The effect of carbon doping contents on the microstructure, hardness, and corrosion properties of heat-treated AISI steel grades of plain carbon steel was investigated in this study. Various microstructures including coarse ferrite-pearlite, fine ferrite-pearlite, martensite, and bainite were developed by different heat treatments i.e. annealing, normalizing, quenching, and austempering, respectively. The developed microstructures, micro-hardness, and corrosion properties were investigated by a light optical microscope, scanning electron microscope, electromechanical (Vickers Hardness tester), and electrochemical (Gamry Potentiostat) equipment, respectively. The highest corrosion rates were observed in bainitic microstructures (2.68-12.12 mpy), whereas the lowest were found in the fine ferritic-pearlitic microstructures (1.57-6.36 mpy). A direct correlation has been observed between carbon concentration and corrosion rate, i.e. carbon content resulted in an increase in corrosion rate (2.37 mpy for AISI 1020 to 9.67 mpy for AISI 1050 in annealed condition).
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The use of Pipelines for long-distance transportation of crude oil, natural gas and similar applications is increasing and has pivotal importance in recent times. High specific strength plays a crucial role in improving transport efficiency through increased pressure and improved laying efficiency through reduced diameter and weight of line pipes. TRIP-based high-strength and high-ductility alloys comprise a mixture of ferrite, bainite, and retained austenite that provide excellent mechanical properties such as dimensional stability, fatigue strength, and impact toughness. This study performs microstructure analysis using both Nital etching and LePera etching methods. At the time of Nital etching, it is difficult to distinctly observe second phase. However, using LePera etching conditions it is possible to distinctly measure the M/A phase and ferrite matrix. The fraction measurement was done using OM and SEM images which give similar results for the average volume fraction of the phases. Although it is possible to distinguish the M/A phase from the SEM image of the sample subjected to LePera etching. However, using Nital etching is nearly impossible. Nital etching is good at specific phase analysis than LePera etching when using SEM images.
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Conductive and stretchable electrodes that can be printed directly on a stretchable substrate have drawn extensive attention for wearable electronics and electronic skins. Printable inks that contain liquid metal are strong candidates for these applications, but the insulating oxide skin that forms around the liquid metal particles limits their conductivity. This study reveals that hydrogen doping introduced by ultrasonication in the presence of aliphatic polymers makes the oxide skin highly conductive and deformable. X-ray photoelectron spectroscopy and atom probe tomography confirmed the hydrogen doping, and first-principles calculations were used to rationalize the obtained conductivity. The printed circuit lines show a metallic conductivity (25,000 S cm-1), excellent electromechanical decoupling at a 500% uniaxial stretching, mechanical resistance to scratches and long-term stability in wide ranges of temperature and humidity. The self-passivation of the printed lines allows the direct printing of three-dimensional circuit lines and double-layer planar coils that are used as stretchable inductive strain sensors.
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Synthesizing semiconductor nanoparticles through core/shell structuring is an effective strategy to promote the functional, physical, and kinetic performance of optoelectronic materials. However, elucidating the internal structure and related atomic distribution of core/shell structured quantum dots (QDs) in three dimensions, particularly at heterostructure interfaces, has been an overarching challenge. Herein, by applying complementary analytical techniques of electron microscopy and atom probe tomography, the dimensional, structural, topological, and compositional information on commercially available 11.8 nm-sized CdSSe/ZnS QDs were obtained. Systematic experiments at high resolution reveal the presence of a 1.8 nm-thick Cd xZn1 - xS inner shell with a composition gradient between the CdSe core and the ZnS outermost shell. More strikingly, the inner shell shows compositional variation because of competitive atomic configuration between Cd and ZnS, but it structurally retains a zinc-blende crystal structure with the core. The inner shell may grow through the decreased reactivity of S with Cd, followed by atomic diffusion-related processes. The composition-competitive gradient inner shell alleviates lattice misfit strain at heterostructure interfaces, thereby enhancing the quantum yield and photostabilty to a greater extent than those of other single-shell structures. Thus, this precise measurement approach could offer a potential pathway to develop a wide variety of three-dimensional core/shell-structured materials.
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The strengthening mechanism of the metallic material is related to the hindrance of the dislocation motion, and it is possible to achieve superior strength by maximizing these obstacles. In this study, the multiple strengthening mechanism-based nanostructured steel with high density of defects was fabricated using high-pressure torsion at room and elevated temperatures. By combining multiple strengthening mechanisms, we enhanced the strength of Fe-15 Mn-0.6C-1.5 Al steel to 2.6 GPa. We have found that solute segregation at grain boundaries achieves nanograined and nanotwinned structures with higher strength than the segregation-free counterparts. The importance of the use of multiple deformation mechanism suggests the development of a wide range of strong nanotwinned and nanostructured materials via severe plastic deformation process.
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We present a new method of preparing needle-shaped specimens for atom probe tomography from freestanding Pd and C-supported Pt nanoparticles. The method consists of two steps, namely electrophoresis of nanoparticles on a flat Cu substrate followed by electrodeposition of a Ni film acting as an embedding matrix for the nanoparticles. Atom probe specimen preparation can be subsequently carried out by means of focused-ion-beam milling. Using this approach, we have been able to perform correlative atom probe tomography and transmission electron microscopy analyses on both nanoparticle systems. Reliable mass spectra and three-dimensional atom maps could be obtained for Pd nanoparticle specimens. In contrast, atom probe samples prepared from C-supported Pt nanoparticles showed uneven field evaporation and hence artifacts in the reconstructed atom maps. Our developed method is a viable means of mapping the three-dimensional atomic distribution within nanoparticles and is expected to contribute to an improved understanding of the structure-composition-property relationships of various nanoparticle systems.
RESUMO
Creation of nanometer-scale conductive filaments in resistive switching devices makes them appealing for advanced electrical applications. While in situ electrical probing transmission electron microscopy promotes fundamental investigations of how the conductive filament comes into existence, it does not provide proof-of-principle observations for the filament growth. Here, using advanced microscopy techniques, electrical, 3D compositional, and structural information of the switching-induced conductive filament are described. It is found that during in situ probing microscopy of a Ag/TiO2 /Pt device showing both memory- and threshold-switching characteristics, a crystalline Ag-doped TiO2 forms at vacant sites on the device surface and acts as the conductive filament. More importantly, change in filament morphology varying with applied compliance currents determines the underlying switching mechanisms that govern either memory or threshold response. When focusing more on threshold switching features, it is demonstrated that the structural disappearance of the filament arises at the end of the constricted region and leads to the spontaneous phase transformation from crystalline conductive state into an initial amorphous insulator. Use of the proposed method enables a new pathway for observing nanosized features in a variety of devices at the atomic scale in three dimensions.
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The control of solution-processed emitting layers in organic-based optoelectronic devices enables cost-effective processing and highly efficient properties. However, a solution-based protocol for emitter fabrication is highly complex, and the link between the device performance and internal nanoscale features as well as three associated fabricating parameters (e.g., the employed solvents, annealing temperatures, and molecular concentration) needs to be understood. Here, this study investigates the influence of the solution-processing parameters on the nanostructure-property relationship in light emitters that consist of iridium complexes doped in polymer. The boiling points and evaporation rates of the selected solvents govern the nanomorphology of molecular aggregation in the as-processed state, and the aggregation is either needle-like, spherical, or even a mixture of needles and spheres. Furthermore, a direct observation via in situ heating microscopy indicates that annealing of emitters containing a needle-type aggregation promotes the associated molecular transport, leading to a substantial reduction in the surface roughness. Consequently, a nearly threefold increase in the current efficiency of the device is induced. These findings have important implications for the tuning of the aggregation of iridium complexes for emitters used in the new evolution of high-performance organic-based optoelectronic devices.
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Two challenges exist in laser-assisted atom probe tomography (APT). First, a drastic decline in mass-resolving power is caused, not only by laser-induced thermal effects on the APT tips of bulk oxide materials, but also the associated asymmetric evaporation behavior; second, the field evaporation mechanisms of bulk oxide tips under laser illumination are still unclear due to the complex relations between laser pulse and oxide materials. In this study, both phenomena were investigated by depositing Ni- and Co-capping layers onto the bulk LaAlO3 tips, and using stepwise APT analysis with transmission electron microscopy (TEM) observation of the tip shapes. By employing the metallic capping, the heating at the surface of the oxide tips during APT analysis became more symmetrical, thereby enabling a high mass-resolving power in the mass spectrum. In addition, the stepwise microscopy technique visualized tip shape evolution during APT analysis, thereby accounting for evaporation sequences at the tip surface. The combination of "capping" and "stepwise APT with TEM," is applicable to any nonconductors; it provides a direct observation of tip shape evolution, allows determination of the field evaporation strength of oxides, and facilitates understanding of the effects of ultrafast laser illumination on an oxide tip.
RESUMO
Understanding the mechanism responsible for the temperature-dependent performances of emitting layers is essential for developing advanced phosphorescent organic light emitting diodes. We described the morphological evolution occurring in PVK:Ir(ppy)3 binary blend films, with respect to thermal annealing up to 300 °C, by coupling atomic force microscopy and transmission electron microscopy. In particular, in situ temperature-dependent experimental characterization was performed to directly determine the overall sequence of morphological evolution occurring in the films. The device thermally annealed at 200 °C exhibits a noticeable enhancement in the performances, compared to the devices in the as-processed state and to the devices annealed at 300 °C. Our approaches reveal that the Ir(ppy)3 molecules, with a needle-like structure in the as-processed state, were aggregated, and thus diffused into PVK without a morphological change at the temperature regime between 150 °C and 200 °C. Moreover, both network-like and droplet patterns existed in the devices annealed at 300 °C, which was beyond the glass temperature of PVK, leading to a profound increase in the surface roughness. The observed pattern formation is discussed in terms of viscoelastic phase separation. Based on our experimental findings, we propose that the performances of the devices are significantly controlled by the diffusion of dopant molecules and the morphological evolution of the host materials in binary blend systems.
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We introduce a new experimental approach for the identification of the atomistic position of interstitial carbon in a high-Mn binary alloy consisting of austenite and ε-martensite. Using combined nano-beam secondary ion mass spectroscopy, atomic force microscopy and electron backscatter diffraction analyses, we clearly observe carbon partitioning to austenite. Nano-beam secondary ion mass spectroscopy and atom probe tomography studies also reveal carbon trapping at crystal imperfections as identified by transmission electron microscopy. Three main trapping sites can be distinguished: phase boundaries between austenite and ε-martensite, stacking faults in austenite, and prior austenite grain boundaries. Our findings suggest that segregation and/or partitioning of carbon can contribute to the austenite-to-martensite transformation of the investigated alloy.