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Activity Convergence between Continuous- and Pulsed-Deposition NiFe Hydroxide Anodes in Liquid Alkaline Electrolyzers
Improving the activity of anodes for the alkaline oxygen evolution reaction (OER) is of interest because of the importance of the reaction in electrochemical technology. There is an abundance of studies which confirm that NiFe hydroxide, often prepared by electrodeposition, is the most active catalyst for the alkaline OER. This relatively high level of confidence in the optimal OER catalyst chemistry suggests that exploration of methods which improve on features besides the chemistry of the films, such as their microstructure, could access new heights of activity. In this study, the possible benefits of pulsed current deposition relative to the conventional continuous current approach to the deposition of NiFe hydroxides were investigated. Pulsed deposition densified the film surfaces by preventing metal ion depletion at the electrode surface during film formation. The Fe content, redox reversibility, and OER activity were higher for the pulsed deposition films relative to their continuous deposition counterparts. Though pulsed deposition imparted a higher OER performance of the films compared to continuous deposition at the three-electrode level, this improved performance was not retained during electrolyzer operation. Rather, a convergence of the cell performance is seen irrespective of the deposition approach. This phenomenon was attributed to the way electrolyzer conditionsrelatively high temperature, base concentration, and current densitycan drive alternate mechanisms for observed performance.
In-situ synchrotron x-ray studies of the microstructure and stability of In 2 O 3 epitaxial films
We report on the synthesis, stability, and local structure of In2O3 thin films grown via rf-magnetron sputtering and characterized by in-situ x-ray scattering and focused x-ray nanodiffraction. We find that In2O3 deposited onto (0 0 1)-oriented single crystal yttria-stabilized zirconia substrates adopts a Stranski-Krastanov growth mode at a temperature of 850 degrees C, resulting in epitaxial, truncated square pyramids with (1 1 1) side walls. We find that at this temperature, the pyramids evaporate unless they are stabilized by a low flux of In2O3 from the magnetron source. We also find that the internal lattice structure of one such pyramid is made up of differently strained volumes, revealing local structural heterogeneity that may impact the properties of In2O3 nanostructures and films.
High performance microstructured Lu[subscript 2]O[subscript 3]:Eu thin film scintillator for X-ray computed tomography
Abstract not provided
Microstructures and properties of superconducting Y-ErBaCuO thin films obtained from disordered Y-ErBaF2Cu films
The preparation procedure used to obtain superconducting thin films by radio frequency magnetron sputtering of a single mosaic target is described in detail. The single mosaic target is composed of (Y-Er), BaF2, and Cu.
(abstract) Optical Scattering and Surface Microroughness of Ion Beam Deposited Au and Pt Thin Films
Thin films of gold and platinum have been deposited onto superpolished fused silica substrates using thermal evaporation, ion assisted deposition (IAD), and ion assisted sputtering. The influence of ion beam flux, thin film material, and deposition rate on the films microroughness have been investigated. Short range surface microroughness of the films has been examined using scanning tunneling microscopy (STM) and atomic force microscopy (AFM). Long range surface microroughness has been characterized using an angle resolved optical scatterometer. Results indicate that ion beam deposited coatings have improved microstructure over thermally evaporated films.
Corrosion Behavior of Aqua-Blasted and Laser-Engraved Type 316L Stainless Steel
The effect of aqua blasting and laser engraving on surface microstructure development, residual stress and corrosion resistance of type 316L stainless steel has been investigated. Aqua blasting resulted in a deformed near-surface microstructure containing compressive residual stresses. Subsequent laser engraving produced a surface layer with tensile residual stresses reaching to a depth of 200 microns. Changes of surface roughness topography were accompanied by the development of a thick oxide/hydroxide film after laser engraving. The atmospheric corrosion behavior of all surfaces with MgCl{sub 2}-laden droplets was compared to their electrochemical response in 1M NaCl and 0.7 M HCl aqueous solutions. The measured total volume loss after atmospheric corrosion testing was similar for all investigated surface conditions. Laser-engraved surface exhibited the smallest number of corrosion sites, but the largest mean corrosion depth.
Disentangling Electronic Transport and Hysteresis at Individual Grain Boundaries in Hybrid Perovskites via Automated Scanning Probe Microscopy
Underlying the rapidly increasing photovoltaic efficiency and stability of metal halide perovskites (MHPs) is the advancement in the understanding of the microstructure of polycrystalline MHP thin film. Over the past decade, intense efforts have been aimed at understanding the effect of microstructures on MHP properties, including chemical heterogeneity, strain disorder, phase impurity, etc. It has been found that grain and grain boundary (GB) are tightly related to lots of microscale and nanoscale behavior in MHP thin films. Atomic force microscopy (AFM) is widely used to observe grain and boundary structures in topography and subsequently to study the correlative surface potential and conductivity of these structures. For now, most AFM measurements have been performed in imaging mode to study the static behavior; in contrast, AFM spectroscopy mode allows us to investigate the dynamic behavior of materials, e.g., conductivity under sweeping voltage. However, a major limitation of AFM spectroscopy measurements is that they require manual operation by human operators, and as such only limited data can be obtained, hindering systematic investigations of these microstructures. Here, we designed a workflow combining the conductive AFM measurement with a machine learning (ML) algorithm to systematically investigate grain boundaries in MHPs. The trained ML model can extract GBs locations from the topography image, and the workflow drives the AFM probe to each GB location to perform a current–voltage (IV) curve automatically. Then, we are able to have IV curves at all GB locations, allowing us to systematically understand the property of GBs. Using this method, we discovered that the GB junction points are less conductive, potentially more photoactive, and can play critical roles in MHP stability, while most previous works only focused on the difference between GB and grains.
Modeling physical vapor deposition of energetic materials
Morphology and microstructure of organic explosive films formed using physical vapor deposition (PVD) processes strongly depends on local surface temperature during deposition. Currently, there is no accurate means of quantifying the local surface temperature during PVD processes in the deposition chambers. This study focuses on using a multiphysics computational fluid dynamics tool, STARCCM+, to simulate pentaerythritol tetranitrate (PETN) deposition. The PETN vapor and solid phase were simulated using the volume of fluid method and its deposition in the vacuum chamber on spinning silicon wafers was modeled. The model also included the spinning copper cooling block where the wafers are placed along with the chiller operating with forced convection refrigerant. Implicit time-dependent simulations in two- and three-dimensional were performed to derive insights in the governing physics for PETN thin film formation. PETN is deposited at the rate of 14 nm/s at 142.9 °C on a wafer with an initial temperature of 22 °C. The deposition of PETN on the wafers was calculated at an assumed heat transfer coefficient (HTC) of 400 W/m 2 K. This HTC proved to be the most sensitive parameter in determining the local surface temperature during deposition. Previous experimental work found noticeable microstructural changes with 0.5 mm fused silica wafers in place of silicon during the PETN deposition. This work showed that fused silica slows initial wafer cool down and results in ~10 °C difference for the surface temperature at 500 μm PETN film thickness. It was also found that the deposition surface temperature is insensitive to the cooling power of the copper block due to the copper block's very large heat capacity and thermal conductivity relative to the heat input from the PVD process. Future work should incorporate the addition of local stress during PETN deposition. Lastly, based on simulation results, it is also recommended to investigate the impact of wafer surface energy on the PETN microstructure and morphology formation.
Effects of lithium doping on microstructure, electrical properties, and chemical bonds of sol-gel derived NKN thin films
Highly (100/110) oriented lead-free Li{sub x}(Na{sub 0.5}K{sub 0.5}){sub 1−x}NbO{sub 3} (LNKN, x = 0, 0.02, 0.04, and 0.06) thin films are fabricated on Pt/Ti/SiO{sub 2}/Si substrates via a sol-gel processing method. The lithium (Li) dopants modify the microstructure and chemical bonds of the LNKN films, and therefore improve their electrical properties. The optimal values of the remnant polarization (P{sub r} = 14.3 μC/cm{sup 2}), piezoelectric coefficient (d{sub 33} = 48.1 pm/V), and leakage current (<10{sup −5} A/cm{sup 2}) are obtained for a lithium addition of x = 0.04 (i.e., 4 at. %). The observation results suggest that the superior electrical properties are the result of an improved crystallization, a larger grain size, and a smoother surface morphology. It is shown that the ion transport mechanism is dominated by an Ohmic behavior under low electric fields and the Poole-Frenkel emission effect under high electric fields.
The microstructure and He + ion irradiation behavior of novel low-activation W-Ta-Cr-V refractory high entropy alloy for nuclear applications
Microstructure and nanohardness of a nearly equimolar W-Ta-Cr-V high entropy alloy (HEA), as well as its irradiation response under He + irradiation, were investigated. The single-phase body-centered cubic nanostructured alloy with a 1 µm thick layer was fabricated on a silicon substrate using a magnetron sputtering method. The HEA film has a complex microstructure consisting of micrometric domains that exhibit internal nanostructure controlled by their crystal orientation. The measured nanohardness of the W-Ta-Cr-V alloy is 13 ± 2 GPa, which significantly exceeds the hardness of nanocrystalline tungsten as a result of the high solid-solution strengthening effect. In order to evaluate the irradiation resistance of the HEA film, the material was irradiated with 200 keV He + ions at room temperature, with two different ion fluences: 1 × 10 16 and 5 × 10 16 ions/cm 2 . Using transmission electron microscopy, a high density of extremely fine He bubbles is observed that were uniformly distributed in the matrix. The increase of He + ion fluence increased the density of bubbles, whereas their size remained at a similar level, which indicates that the damage proceeds by the nucleation of additional He bubbles, not by their growth.
High-Throughput Open-Air Plasma Activation of Metal-Oxide Thin Films with Low Thermal Budget
Sputter-processed oxide films are usually annealed at high temperature (activation process) to achieve stable electrical characteristics through the formation of strong metal-oxide chemical bonds. For instance, indium– gallium–zinc oxide (IGZO) films typically need a thermal treatment at 300 °C for ≥1 h as an activation process. We introduce an open-air plasma treatment (OPT) to rapidly and effectively activate sputter-processed IGZO films. The OPT effectively induces metal-oxide chemical bonds in IGZO films at temperatures as low as 240 °C, with a dwell time on the order of a second. Furthermore, by controlling the plasma-processing conditions (scan speed, distance α between plasma nozzle and samples, and gas flow rate), the electrical characteristics and the microstructure of the IGZO films can be easily tuned. Finally, OPT can be utilized to implement a selective activation process. Plasma-treated IGZO thin-film transistors (TFTs) display comparable electrical characteristics to those of conventionally thermal treated IGZO TFTs. Through in-depth optical, chemical, and physical characterizations, we validate that OPT simultaneously dissociates weak chemical bonds by UV radiation and ion bombardment and reestablishes the metal-oxide network by radical reaction and OPT-induced heat.
Structural and optical properties of electron beam evaporated yttria stabilized zirconia thin films
Yttria stabilized zirconia (10 mole % Y{sub 2}O{sub 3}) thin films were deposited on quartz substrates using electron beam physical vapor deposition at the substrate temperatures in the range 300 – 973 K. XRD analysis showed cubic crystalline phase of YSZ films with preferred orientation along (111). The surface roughness was found to increase with the increase of deposition temperatures. The optical band gap of ∼5.7 eV was calculated from transmittance curves. The variation in the optical properties is correlated with the changes in the microstructural features of the films prepared as a function of substrate temperature.
Crystallized Silicon Nanostructures - Experimental Characterization and Atomistic Simulations
We have synthesized silicon nanocrystalline structures from thermal annealing of thin film amorphous silicon-based multilayers. The annealing procedure that was carried out in vacuum at temperatures up to 1100 °C is integrated in a X-ray diffraction (XRD) setup for real-time monitoring of the formation phases of the nanostructures. The microstructure of the crystallized films is investigated through experimental measurements combined with atomistic simulations of realistic nanocrystalline silicon (nc-Si) models. The multilayers consisting of uniformly alternating thicknesses of hydrogenated amorphous silicon and silicon oxide (SiO2) were deposited by plasma enhanced chemical vapor deposition on crystalline silicon and Corning glass substrates. The crystallized structure consisting of nc-Si structures embedded in an amorphous matrix were further characterized through XRD, Raman spectroscopy, and Fourier transform infrared measurements. We are able to show the different stages of nanostructure formation and how the sizes and the crystallized mass fraction can be controlled in our experimental synthesis. The crystallized silicon structures with large crystalline filling fractions exceeding 50% have been simulated with a robust classical molecular dynamics technique. The crystalline filling fractions and structural order of nc-Si obtained from this simulation are compared with our Raman and XRD measurements.
Microstructure evolution of wrought nickel based superalloy GH4037 in the semi-solid state
Highlights: • Semi-solid isothermal treatment of wrought superalloy (SSITWS). • Near-globular microstructure. • Carbide precipitates. - Abstract: Study on semi-solid processing of superalloy is little reported due to the difficulties in fabricating semi-solid billets. In this manuscript, a novel method called semi-solid isothermal treatment of wrought superalloy (SSITWS) was firstly proposed in order to fabricate semi-solid billets of superalloy. The effects of isothermal temperature and soaking time on microstructure of Ni-based superalloy GH4037 in the semi-solid state were investigated. The results show that the near-globular microstructure of wrought GH4037 superalloy can be obtained by the semi-solid isothermal treatment. The average grain size increased and the roundness decreased with the prolonged soaking time at 1350 °C and 1360 °C. When the isothermal temperature was elevated to 1370 °C or 1380 °C, the microstructure evolution was complex due to the combination of breaking up mechanism and coarsening mechanism. At 1390 °C, the dendritic grains were obviously observed in the microstructure. With the increasing of isothermal temperature and soaking time, the liquid boundary film coarsening behavior occurred in the microstructure. With the increasing of soaking time, the size of intragranular liquid droplets increased, but the amount of them decreased. When the isothermal temperature was high, the intragranular liquid droplets disappeared. The coarsening rate constant at 1360 °C was lower compared to that at 1350 °C. However, when the isothermal temperature was higher than 1370 °C, the coarsening kinetics was not suitable for describing the microstructure evolution. The discrete carbide precipitates appeared in the grain boundaries. The distribution of Ti and Mo were higher in the grain boundaries than that in solid grains, and the distribution of other elements was homogenous in the grain boundaries and inside the grains.
Influence of Protection Layers on Thermal Stability of Nitride Thin Films
Nitrides are commonly studied for their properties relevant to numerous coating applications, and have been recently used to synthesize newly predicted materials in thin film form. However, thermodynamic stability of such nitride materials is difficult to experimentally evaluate, due to limited thermal budget of thin films. Here we show that thermal stability of nitride films can be extended using protection layers. Specifically, we find that zirconium nitride (ZrN) thin films are stable up to at least 1200°C annealing temperature in N2 atmosphere, if aluminum nitride (AlN) diffusion barriers and capping layers are used. X-ray diffraction (XRD) measurements show the expected thermodynamically stable rocksalt structure of ZrN, and scanning electron microscopy (SEM) confirms compact microstructure of these ZrN films. Without such protection layers, transient bixbyite Zr2ON2 phase and high-temperature ZrSi2 phase are observed after annealing by XRD, SEM, and auger electron spectroscopy (AES), due to side reaction with native surface oxide (ZrOx) and substrate (Si) respectively. These results demonstrate that protection layers are beneficial to increase the thermal budget of nitride thin films, for evaluating thermodynamic stability of new nitride materials, for capturing transient metastable phases during crystallization, and for using functional nitride coatings in extreme environments.
Induced lattice strain in epitaxial Fe-based superconducting films on CaF{sub 2} substrates: A comparative study of the microstructures of SmFeAs(O,F), Ba(Fe,Co){sub 2}As{sub 2}, and FeTe{sub 0.5}Se{sub 0.5}
The microstructures of SmFeAs(O,F), Ba(Fe,Co){sub 2}As{sub 2}, and FeTe{sub 0.5}Se{sub 0.5} prepared on CaF{sub 2} substrates were investigated using transmission electron microscopy. The SmFeAs(O,F)/CaF{sub 2} interface is steep, without a disordered layer. By contrast, a chemical reaction occurs at the interface in the cases of Ba(Fe,Co){sub 2}As{sub 2} and FeTe{sub 0.5}Se{sub 0.5}. The reaction layers are located on opposite sides of the interface for Ba(Fe,Co){sub 2}As{sub 2} and FeTe{sub 0.5}Se{sub 0.5}. We found that the lattice distortion of the three superconducting films on the CaF{sub 2} substrates enhances the T{sub C} values compared with films prepared on oxide substrates. The origin of this lattice deformation varies depending on the superconducting material.
Anisotropic domains and antiferrodistortive-transition controlled magnetization in epitaxial manganite films on vicinal SrTiO 3 substrates
We studied the microstructural evolution and magnetism of ferroelastic La 0.9 Sr 0.1 MnO 3 (LSMO) epitaxial thin films grown on SrTiO 3 (001) substrates with different miscut angles. The substrate miscut angle plays a critical role in controlling the in-plane magnetic anisotropy. The microscopic origin of such magnetic anisotropy is attributed to the formation of anisotropic stripe domains along the surface step terraces. The magnetization in the LSMO films was found to be selectively modulated by the antiferrodistortive phase transition of the SrTiO 3 substrate. This phenomenon has been qualitatively explained by a strain modified Stoner–Wohlfarth model. We conclude that the magnetization modulation by the SrTiO 3 phase transition depends on h, the ratio of applied magnetic field to the saturation field. Such modulation is only visible with h < 1. The established domain microstructure–anisotropy–magnetism correlation in manganite films can be applied to a variety of complex oxide thin films on vicinal substrates.