15 research outputs found

    Laser-assisted nanofabrication of multielement complex oxide core–shell nanoparticles

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    Nanoparticles with core–shell motifs are of particular interest because they enable combining multiple functionalities at nanoscale. However, a key challenge in designing such novel structures is to phase-separate the constituents at the core and shell regions, especially in thermodynamically miscible systems. In this study, we report the successful formation of self-organized Cr2O3-Fe2O3 core–shell nanoparticles by adopting a non-equilibrium route of pulsed laser-induced dewetting of an alloyed thin film. In this process, the evolution of nanoparticles takes place from the rupture of the initially flat liquid-phase alloyed film under laser irradiation. A continued laser pulsing results in the ripening of the morphologies at different stages eventually leading to a final droplet shape nanoparticle. Using highly sensitive 3D chemical mapping of individual nanoparticles and thermal simulations, we reveal that thermodynamically-soluble Cr2O3 and Fe2O3 phase-segregate in the core and shell regions, respectively, within ∼ 100 ns during a fast solidification process, leveraging the difference in the cooling rates, surface energies and enthalpy of mixing at high-temperatures. With these results, we present a non-equilibrium laser-assisted pathway that can be used to create core–shell nanostructures with dissimilar characteristics

    Creep strength boosted by a high-density of stable nanoprecipitates in highchromium steels

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    There is a need worldwide to develop materials for advanced power plants with steam temperatures of 700°C and above that will achieve long-term creep-rupture strength and low CO2 emissions. The creep resistance of actual 9-12Cr steels is not enough to fulfil the engineering requirements above 600°C. In this paper, the authors report their advances in the improvement of creep properties of this type of steels by the microstructural optimization through nano-precipitation using two methodologies. 1) Applying a high temperature austenitization cycle followed by an ausforming step (thermomechanical treatment, TMT) to G91 steel, to increase the martensite dislocation density and, thus, the number density of MX precipitates (M = V ,Nb; X = C ,N) but at the expense of deteriorating the ductility. 2) Compositional adjustments, guided by computational thermodynamics, combined with a conventional heat treatment (no TMT), to design novel steels with a good ductility while still possessing a high number density of MX precipitates, similar to the one obtained after the TMT in G91. The microstructures have been characterized by optical, scanning and transmission electron microscopy, EBSD and atom probe tomography. The creep behaviour at 700°C has been evaluated under a load of 200 N using small punch creep tests.The authors would like to thank James Burns for assistance in performing APT sample preparation and running the APT experiments. The authors are grateful for the dilatometer tests by Phase Transformation laboratory and for the SEM microscopy by the Microscopy Lab at CENIM-CSIC. This work contributes to the Joint Programme on Nuclear Materials (JPNM) of the European Energy Research Alliance (EERA).Peer reviewe

    Understanding Mechanical Properties of Nano-Grained Bainitic Steels from Multiscale Structural Analysis

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    Steel components working in extreme conditions require materials presenting the highest performances. Nowadays, nanoengineering is being applied to the development of ultra-high strength steels as a key-enabling technology in the steel sector. The present article describes the multiscale structure of nano-grained steels designed using atomic transformation theory and processed by a simple heat treatment. Outstanding mechanical properties for these novel steels are reported, and strain-hardening mechanisms are discussed.This research was funded by the European Research Fund for Coal and Steel under the contracts RFSR-CT-2014-00016 and RFSR-CT-2014-00019 and the Spanish Ministry of Economy and Competitiveness under the contracts MAT2016-80875-C3-1-RWe acknowledge support by the CSIC Open Access Publication Initiative through its Unit of Information Resources for Research (URICI

    Probing the Location and Speciation of Elements in Zeolites with Correlated Atom Probe Tomography and Scanning Transmission X-Ray Microscopy

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    Characterizing materials at nanoscale resolution to provide new insights into structure property performance relationships continues to be a challenging research target due to the inherently low signal from small sample volumes, and is even more difficult for nonconductive materials, such as zeolites. Herein, we present the characterization of a single Cu-exchanged zeolite crystal, namely Cu-SSZ-13, used for NOX reduction in automotive emissions, that was subject to a simulated 135,000-mile aging. By correlating Atom Probe Tomography (APT), a single atom microscopy method, and Scanning Transmission X-ray Microscopy (STXM), which produces high spatial resolution X-ray Absorption Near Edge Spectroscopy (XANES) maps, we show that a spatially non-uniform proportion of the Al was removed from the zeolite framework. The techniques reveal that this degradation is heterogeneous at length scales from micrometers to tens of nanometers, providing complementary insight into the long-term deactivation of this catalyst system

    Perovskite Solar Cells with Near 100% Internal Quantum Efficiency Based on Large Single Crystalline Grains and Vertical Bulk Heterojunctions

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    Imperfections in organometal halide perovskite films such as grain boundaries (GBs), defects, and traps detrimentally cause significant nonradiative recombination energy loss and decreased power conversion efficiency (PCE) in solar cells. Here, a simple layer-by-layer fabrication process based on air exposure followed by thermal annealing is reported to grow perovskite films with large, single-crystal grains and vertically oriented GBs. The hole-transport medium Spiro-OMeTAD is then infiltrated into the GBs to form vertically aligned bulk heterojunctions. Due to the space-charge regions in the vicinity of GBs, the nonradiative recombination in GBs is significantly suppressed. The GBs become active carrier collection channels. Thus, the internal quantum efficiencies of the devices approach 100% in the visible spectrum range. The optimized cells yield an average PCE of 16.3 ± 0.9%, comparable to the best solution-processed perovskite devices, establishing them as important alternatives to growing ideal single crystal thin films in the pursuit toward theoretical maximum PCE with industrially realistic processing techniques

    Probing the Location and Speciation of Elements in Zeolites with Correlated Atom Probe Tomography and Scanning Transmission X-Ray Microscopy

    No full text
    Characterizing materials at nanoscale resolution to provide new insights into structure property performance relationships continues to be a challenging research target due to the inherently low signal from small sample volumes, and is even more difficult for nonconductive materials, such as zeolites. Herein, we present the characterization of a single Cu-exchanged zeolite crystal, namely Cu-SSZ-13, used for NOX reduction in automotive emissions, that was subject to a simulated 135,000-mile aging. By correlating Atom Probe Tomography (APT), a single atom microscopy method, and Scanning Transmission X-ray Microscopy (STXM), which produces high spatial resolution X-ray Absorption Near Edge Spectroscopy (XANES) maps, we show that a spatially non-uniform proportion of the Al was removed from the zeolite framework. The techniques reveal that this degradation is heterogeneous at length scales from micrometers to tens of nanometers, providing complementary insight into the long-term deactivation of this catalyst system
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