Surface Oxide Layer Research Articles

X-ray photoelectron spectroscopy surface oxidation study of remote plasma-enhanced chemical vapor deposition-grown Ge1−xSnx/Si alloys

Recent progress in the remote plasma-enhanced chemical vapor deposition of Ge1−xSnx grown directly on Si substrates has improved crystal structure quality. To understand the impact of postgrowth storage, we study oxidation states of Ge1−xSnx alloys, for x values of 7.5%, 8.8%, 12.5%, and 19.3%. A surface oxidation layer formed naturally at room temperature over five months is quantified using angle-resolved x-ray photoelectron spectroscopy. The GeSn alloys exhibit a high surface oxide concentration with a minimum of 77% in Sn 3d peak analysis. Ge is less susceptible to oxidation than Sn, with oxidation percentages ranging from 25% to 86%. The Sn dopant enhances the oxidation features associated with the Ge 3p peak, aiding surface oxidation and penetrating further into the film. It is feasible that the 4+ state Sn from the precursor readily oxidizes postgrowth resulting in an oxide-rich surface layer.

Ni–Cr dental alloys - porcelain firing impact on corrosion properties and surface characteristics

Biocompatibility is a critical aspect of the use of materials in the human body. The use of base metal alloys in dentistry is primarily regulated by health and safety standards set by regulatory authorities in various countries. The porcelain-fused-to-metal (PFM) process applied to Ni-Cr dental alloys can alter their properties, particularly in terms of corrosion and surface characteristics. This study aimed to assess the effect of the heat processing used for dental porcelain firing on these properties. The two casted alloys: Ceramic N and Ivoclar Vivadent 4all, used in the study were characterized by analyzing the microstructure by scanning electron microscopy (SEM), composition with energy dispersive x-ray spectroscopy (EDS), hardness, surface profile and electrochemical corrosion resistance (Ecorr, jcorr, polarization curve, Ebr and electrochemical impedance spectroscopy (EIS) results), as well as ions release before and after the simulated porcelain firing. Based on the conducted research the following conclusions can be drawn: Analyzes of the material characteristics before and after the simulation showed that the discussed process, although it does not cause the formation of chemical impurities on the surface of the alloys, results in changes in the chemical composition and structure of surface oxides, increases roughness and reduces hardness. The results of the corrosion examinations showed a deterioration in anti-corrosion properties after the simulation. The statistically significant decrease in corrosion resistance may result from the increased heterogeneity of the surface oxide layers and partial changes in their composition.

Temperature-copper content induced wear mechanism transition in Cu/Ni60A composites

Coppery blast furnace tuyere is easily damaged in high temperature wear environment. Preparing a Ni60A coating by plasma cladding is an effective method to improve its wear resistance and service life. Controlling the appropriate dilution rate is the key to obtain high-quality coatings. The existing research has no clear conclusion on the range of dilution rate of coating for coppery tuyere. In this paper, a series of Cu/Ni60A composites with different copper content (10 wt%, 20 wt%, 40 wt% and 60 wt%) were prepared to mimic Ni60A coatings exhibiting distinct dilution rate. Under the coupling change of temperature and copper content, the wear mechanism of Cu/Ni60A composites showed a complex transition law. Copper content, surface oxide layer (NiO or CuO) and high-temperature softening temperature were the decisive factors of wear transition. The applicable temperatures of Cu/Ni60A composites with low copper content (10 %, 20 %), middle copper content (40 %) and high copper content (60 %) were about 600 °C, 400 °C and 300 °C, respectively. Combined with the heat transfer analysis results, the suitable dilution rates for the coating applied to the inner wall (＜10 %) and front end (10 %-20 %) of tuyere was revealed.

Reaction characteristics of Al–Mg alloy fuels with heterogeneous oxidation shell structures

Al–Mg alloy fuels are the most widely used Al-based alloy fuel in energetic material systems owing to their low ignition temperature and fast reaction. However, their surface oxide layer structure and oxidation, ignition, and combustion mechanisms differ from those of single-metal fuels. Furthermore, insufficient information has been reported on Al–Mg alloy fuels. In this study, Al–Mg alloy fuels were formed by introducing Mg into Al via centrifugal atomization. The microstructure and thermal reaction characteristics of the Al–Mg alloy fuel were evaluated. The ignition and combustion characteristics of the Al–Mg alloy fuels were monitored via single-particle ignition. When the Mg content was increased from 5 % to 40 %, a typical core–shell structure formed, the oxide shell thickness increased from 4.50 to 6.41 nm, and the content of the internal alloy compounds gradually increased. The surfaces of the Al–Mg alloy fuel particles with different Mg contents exhibited heterogeneous oxidation shells. Compared to Al powder, the Al–Mg alloy fuel exhibited better melting and oxidation peak temperatures and higher oxidation weight gain. As the Mg content was increased, the combustion of the Al–Mg alloy fuel intensified with more severe microexplosions and a shorter combustion time. The microexplosion of the Al–Mg alloy fuel was elucidated by theoretical calculations, and its combustion mechanism was proposed. The detailed description of the oxide layer structure, oxidation, and combustion of the Al–Mg alloy fuel provides a reliable explanation of its energy release mechanism in energetic material systems.

In situ steam oxidation of nickel phosphide/carbon composite nanofibers as anode materials for lithium-ion batteries

The synthesis of self-standing nickel phosphide/carbon (NixP/C) composite nanofibers is accomplished through a one-pot electrospinning and in situ steam oxidation after the carbothermal reduction process. Control over the levels of in situ steam oxidizers in the forms of crystal water and nitrates in the precursor fibers is achieved by systematically adjusting the drying temperature before the high-temperature heat treatment. This led to structural modifications in the final products analyzed through comprehensive characterizations. Mechanistic insights into the in situ steam oxidation process are provided, emphasizing its potential in optimizing electrode materials. Electrochemical assessments reveal significantly improved performance in the sample prepared from the media with optimal content of oxidizers, attributed to a tailored surface oxide layer, electronic configuration, and microstructure, enabling enhanced reaction kinetics and minimizing volume expansion. This results in exceptional cycling stability and notable capacity retention during prolonged charge-discharge cycles. Thus, NixP/C achieves the highest initial charge capacity of 719.5 mAh g−1 with an initial Coulombic efficiency of 61% and maintains a high capacity of 590.7 mAh g−1 after 100 cycles at a current density of 0.1 A g−1.

Correlating gas permeability and morphology of bio-based polyether-block-amide copolymer membranes by IR nanospectroscopy

The gas permeability of polymer membranes is determined by their nanoscale morphology, which strongly depends on the membrane fabrication. Here, we demonstrate how the correlation between gas permeability and fabrication-dependent nanoscale morphology of polymer membranes can be elucidated by infrared (IR) nanospectroscopy based on elastic IR scattering at an atomic force microscope tip. Specifically, we fabricated membranes of PEBAX® RNEW – a bio-based polyether-block-amide copolymer – by solvent casting and extrusion, achieving unprecedented CO2 permeability and CO2/N2 selectivity for the solvent-cast membranes. For the extruded membranes, however, we found an about 50 % reduced CO2 permeability, which could not be explained by differential scanning calorimetry and conventional IR spectroscopy. In contrast, IR nanospectroscopy revealed a highly crystalline polyether oxide (PEO) surface layer on the extruded membranes, not observed for the solvent-cast membranes. Annealing of the extruded membranes at 110 °C transformed the crystalline into amorphous PEO layers, as confirmed by IR nanospectroscopy, yielding a gas permeability close to that of the solvent-cast membranes. We thus attribute the dramatic gas reduction of the extruded membranes to their highly crystalline surface layers. Generally, studying polymer morphology by IR nanospectroscopy provides valuable information for better understanding the local gas permeability properties of polymer membranes.

Data Sets Formation on the Physical Properties of Oxide Scale Components for Theoretical Assessment of Efficiency Parameters of Laser Cleaning of Carbon Steels and Related Processes

There is a need in machine-building industries nowadays to automate technologies, in particular, laser ones, to remove surface oxide layers – mill scale, rust – from steel products/pieces in order to improve the energy effectiveness of processing. Herewith, a theoretical assessment method for the intensity of heating of the oxide layer and the phase transition in it can be used to optimize laser cleaning (LC) of the steel surface. To realize this, it is possible to use some calculation and modeling procedures that require, as a first step, the data collection and verification on the temperature-dependent properties of iron-containing condensed phases, as possible components contained, in particular, in scale, which is typically widespread into various metal products. In this regard, the formation of database for characteristics of oxide scale components by the way of selection of information on thermophysical (including optical) properties of the components mentioned and of steel base, which are required for a reliable calculation of the thermal efficiency parameters of the technology for laser cleaning of carbon steels, as well as such actively developed related technologies as laser cutting, drilling, coating remelting, etc., was chosen as the task of our research. An analytical overview of published experimental data made it possible to systematize information on a number of transport and other physical properties of iron-containing components at ambient pressure, including thermal conductivity (k) and diffusivity (a), density ρ, irradiation absorptance and integral emissivity in the temperature range from T ≈ 298 K to the melting temperatures of oxide and metal phases and above them. At the same time, a preliminary thermochemical estimation shows (on the calculated data) the existence of such thermodynamically stable forms of the condensed phase in the heating spot of scale layers during its LC at the melting point and above it, as Fe3O4, FeO, and Fe, which is consistent with known experimental data. Comparison of the values of a calculated by us (using the published values of k, ρ and molar heat capacity and using extrapolation in the high-temperature region) for the types of scale components under consideration with a set of experimental values of this parameter in current literature revealed the presence of differences for both oxide and metal phases. These new values make it possible to fill in a gap in the temperature range T = 1600–1800 K that existed in the data on the thermal diffusivity. The value of a = (0.83–0.92)·10–6 m2/s was also calculated for liquid iron oxide for the T ≈ 1800 K, which was not measured experimentally, that, obviously, prevented modeling of not only laser surface processing, melting and cleaning of steels, but also calculations in the field of metallurgical and other technologies, which are characterized by the presence of iron oxide melts during heating.

High temperature oxidation behavior of liquid phases sintered SiC ceramics with ZrB2 addition

The oxidation property of liquid-phase sintered silicon carbide (LPS-SiC) ceramics with ZrB2 addition was studied after oxidation test in air at 1400 °C. The results indicate that the addition of ZrB2 decreased the degree of polymerization (DOP) of the silicate networks in the oxide layer, suppressing the additional oxidation caused by residual bubbles in the oxide layer of LPS-SiC, which bypassed the layer and directly corroded the material internally. After 100 h of oxidation, the additional oxidation depth was found to be 125 μm in the sample without ZrB2 and 0 μm in those containing 10 wt% ZrB2. Simultaneously, the decrease in DOP facilitates the migration of crystalline phases. The generated ZrSiO4 can migrate and aggregate at the interface between the surface oxide layer and the SiC/ZrB2 matrix, forming a continuous ZrSiO4 barrier. This impedes the diffusion of the oxidant and enhances the oxidation resistance. However, an insufficient ZrB2 content leads to a discontinuous ZrSiO4 layer, thereby weakening its protective effect. Simultaneously, a decrease in DOP increases the rate of oxygen diffusion, resulting in an increase in the oxidation layer thickness. This study contributes to a better understanding of the failure mechanisms of LPS-SiC in oxidizing environments and provide a reference for the design of oxidation-resistant LPS-SiC materials.

Imidazoline As a Volatile Corrosion Inhibitor for Mitigation of Top- and Bottom-of-the-Line CO2 Corrosion in Carbon Steel Pipelines.

A fatty acid imidazoline-based inhibitor was synthesized via a facile solvent-free synthesis method between tall oil fatty acid (TOFA) and diethylenetriamine (DETA) under atmospheric conditions with a short reaction time. The as-synthesized imidazoline (S-Imd) acted as an effective inhibitor for reducing or preventing corrosion of carbon steel pipelines at both bottom of the line (BOL) and top of the line (TOL) positions under simulated conditions of a gas pipeline in a CO2-saturated environment. The inhibition efficacy was examined by both weight loss and electrochemical measurements, such as the electrochemical impedance spectrum (EIS), potentiodynamic polarization (PDP), and linear polarization resistance (LPR). The results revealed that the S-Imd, 2-(8-heptadecenyl)-2-imidazoline-1-ethanamin, at 300 ppm exhibited a superior inhibition efficiency of up to 91.6 and 89.9% for BOL and TOL corrosion tests, respectively. The surface morphology of the carbon steel test specimens was also examined using scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDAX), and contact angle analysis. It was found that the as-synthesized S-Imd acted as a mixed-type inhibitor that exhibited a decreased surface roughness and oxide layer on carbon steel surfaces. However, the water contact angle was found to increase, implying enhanced hydrophobicity of the surface. Adsorption of the imidazoline molecules on carbon steel surfaces followed the Langmuir adsorption isotherm. The present work provides very promising results in the synthesis and utilization of the studied imidazoline as a volatile corrosion inhibitor (VCI), especially for carbon steel pipelines in petroleum industries.

Characterizing oxidation, thickness, and composition of metallic glass thin films with combined electron probe microanalysis and X-ray photoelectron spectroscopy

Metallic glass thin films (MGTFs) are a recently developed class of alloy coatings with potential applications ranging from biomedical devices to electrical components. Their tribological performance in service conditions is dictated by MGTF bulk composition but can be limited by the native oxide surface that inevitably forms upon exposure to atmosphere. Surface oxidation, thickness, and composition of ZrCuNiAl MGTFs were characterized using a combination of X-ray photoelectron microscopy (XPS) and electron probe microanalysis (EPMA). MGTF samples with nominal thicknesses of 50, 500, and 1500 nm were sputtered onto Si and SiN wafer substrates within a high vacuum deposition chamber and their amorphicity was confirmed by X-ray diffraction. XPS depth profiling identified the thin film composition and showed that the surface oxide was dominated by a mixed layer of mostly ZrO2, a little oxidized Al, and some metallic Zr. EPMA X-ray intensities were acquired as a function of beam energy to excite characteristic X-rays from different depths of the MGTFs and reconstructed using open-source thin film analysis software BadgerFilm, to determine the composition and thickness of sample layers. EPMA results constrain the composition to be Zr54Cu29Al10Ni7 within 0.7 at. % variation and total thicknesses to be 49, 470, and 1546 nm. Using the oxide composition identified from XPS depth profiling as an input for BadgerFilm analysis, EPMA results indicate the surface oxidation layer on each of the thin film samples was 6.5 ± 1.1 nm thick and uniform across a 0.25 mm region of the film.

Theoretical study on the hydrogen distribution and diffusion at the PuO2/α-Pu2O3 interface.

The interface is a region in the crystal that significantly changes various characteristics. There must be an interface between oxides of different valence states in the surface oxide layer of plutonium. In this work, a first principles approach based on DFT was used to study the hydrogen distribution and diffusion at the PuO2/α-Pu2O3 interface systematically. Our research reveals that at the interface, hydrogen can be captured by the O atoms of PuO2 and by the oxygen vacancies (OVs) of α-Pu2O3, and the capture of OVs is more energetically advantageous. On the PuO2 side, the cost of H atom diffusion towards the interface gradually increases. On the α-Pu2O3 side, the cost of H atoms diffusing inward from the interface gradually increases. OVs that already contain H atoms are more conducive to capturing H atoms. The formation of the interface has little effect on the hydrogen capture ability of O in PuO2, but it will reduce the capture ability of OVs in α-Pu2O3. Overall, the formation of interfaces has no disruptive impact on the behavior of hydrogen in the two plutonium oxides. This is closely related to the fact that α-Pu2O3 originates from PuO2 under anaerobic conditions. The difference in hydrogen behavior comes from the changes in the atomic environment and ion valence state caused by the OVs. This work supports further understanding of the behavior of hydrogen in plutonium oxides and provides a reference for further research on plutonium corrosion prevention.

In Vitro Inflammatory Cell-Induced Corrosion Using a Lymphocyte and Macrophage Coculture

BackgroundCobalt-chromium-molybdenum (CoCrMo) and titanium alloys have been used for orthopaedic implants for decades. However, recent evidence has shown that inflammatory cell-induced corrosion (ICIC) can damage these metal alloys. This study aimed to investigate the mechanisms of ICIC by coculturing macrophages with lymphocytes. We hypothesized that macrophages would be able to alter the surface oxide layer of CoCrMo and titanium alloy (Ti6Al4V) disks, with greater oxide layer damage occurring in groups with a coculture compared to a macrophage monoculture and in groups with inflammatory activators compared to nonactivated groups. MethodsMurine macrophages were cultured on American Society for Testing and Materials F1537 CoCrMo and F136 Ti6Al4V disks for 30 days and activated with interferon gamma and lipopolysaccharide. Interferon gamma and lipopolysaccharide were added to the culture medium to simulate local inflammation. Macrophages were either cultured alone or in a coculture with T helper lymphocytes. After the 30-day experiment, scanning electron microscopy was used to examine the disk surfaces, and oxide levels were found using energy dispersive x-ray spectroscopy. ResultsPitting features consistent with previous reports of ICIC were found on disks cultured with cells. Both CoCrMo and Ti6Al4V disks had significantly lower oxide levels in all groups with cells compared to control groups with no cells (P < .01). Additionally, CoCrMo disks had significantly lower oxide levels when cultured with activated macrophages and lymphocytes compared to nonactivated macrophages alone (P < .001), activated macrophages alone (P < .01), and nonactivated macrophages and lymphocytes (P < .05). No differences in the oxide levels were found among the Ti6Al4V groups. ConclusionsThis study demonstrates the ability of macrophages to alter the surface chemistry of commonly used orthopaedic alloys. We found that the addition of lymphocytes and a simulated local inflammatory response may contribute to the ICIC of CoCrMo implants.

The negative effect of V content on high temperature oxidation resistance of austenitic stainless steels at 850 °C

The effect of V on the high-temperature oxidation performance of austenitic stainless steel has been investigated by the constant-temperature oxidation weight gain approach, while the morphology, composition and elemental distribution of the oxide film are further analyzed by scanning electron microscopy and energy dispersive spectrum, transmission electron microscope and X-ray powder diffractometer as well as X-ray photoelectron spectroscopy, revealing the mechanism of the effect of V on the high-temperature oxidation performance of austenitic stainless steel. As a result, the addition of V has a significant adverse effect on the oxidation resistance of steel. Noteworthy, vanadium pentoxide generated during the oxidation process increases the internal stress of the surface oxide layer, reduces the integrity of the oxide layer and promotes oxygen penetration into the matrix. Simultaneously, the Z-phase formed at the grain boundaries of the matrix inhibits the diffusion of Cr ions, resulting in the inability to form an effective protective layer of Cr2O3 oxidation on the surface.

Controlling splat boundary network evolution towards the development of strong and ductile cold sprayed refractory metals: The role of powder characteristics

Feedstock powder characteristics such as composition (specific alloying elements and concentrations and impurity levels), microstructure, thickness/composition of surface oxide layers, and particle size distribution play a crucial role in determining the overall mechanical properties of cold sprayed deposits. Herein, we report on two deposits consolidated via cold spray processing from differently-sourced batches of nominally identical elemental refractory powders under identical spraying conditions, which exhibit bending strength and ductility values that differ by more than a factor of two – and with the weakest sample displaying negligible effective ductility. Through chemical, microstructural and micromechanical characterization of both the feedstock powders and cold sprayed deposits, we consider the possible influences of feedstock characteristics on the mechanical performance of cold spray consolidated deposits. It is shown that while differences in interstitial oxygen and hydrogen content may result in differences in the intrinsic yield characteristics of the feedstock material, both feedstocks maintain the ductile behavior required to induce good metallurgical bonding upon impact of optimally sized powder particles. We conclude that the deposits formed from the two feedstock powders are indistinguishable and exhibit high ductility when characterized locally within the relatively undeformed bulk of a single particle or splat. However, the two sprayed deposits show low ductility or brittle behavior when loaded in tension across intersplat boundary domains comprising material that has undergone extensive deformation. In addition, one feedstock incorporates a broader particle size distribution, with a long tail of larger-than-optimal particles. These larger particles are accelerated below the critical impact velocity, resulting in observed imperfect metallurgical bonding at splat interfaces and higher porosity at such intersplat boundaries. This result, combined with the overall differences in the morphology of the intersplat boundary network between the two deposits, explains the difference in macroscopic mechanical behavior. We conclude that accurate control of the powder feedstock particle size distribution is essential for optimizing the mechanical integrity of cold sprayed refractory elements and alloys.

Functionalized interfacial cover design toward pure silicon anode for high power density lithium–ion capacitor

A lithium–ion capacitor, comprising a capacitor–type cathode and battery–type anode, exhibits high power and energy density; however, the integration of different charge storage mechanisms in one cell naturally leads to a kinetic mismatch between the two electrodes, reducing the power density and cycle stability. To solve this problem, high–capacity anode materials with thinner electrodes are required. Silicon, with its high specific capacity, is considered a promising anode material with high energy and power density; however, pure Si anodes undergo rapid capacity fading and exhibit increased internal resistance owing to volume changes during cycling. In this study, both sides of the electrode are covered with functional layers consisting of functionalized herringbone–type carbon nanofibers to protect the Si electrode from degradation. The polar functional groups on the nanofibers weakly interact with the native oxide layer of the Si surface and the carboxyl groups of the binder, ensuring stable contact between electrode materials over repeated cycles. Moreover, the conductive functional cover promotes uniform lithium ion fluxes, aiding the formation of a stable solid electrolyte interphase layer. This study investigates the effects of this strategy on pure Si electrodes by surface morphology analysis, assessment of chemical interactions, and electrochemical testing. This approach has the potential to overcome the degradation of Si electrodes and significantly improve the power and energy density of lithium–ion capacitors.

Deterioration effect of creep on fatigue properties in QCr0.8 alloy: Damage mechanism and fatigue-creep life evaluation

The QCr0.8 alloy used in the thrust chamber liner wall of the reusable liquid rocket engine is subjected to high-temperature fatigue and high-temperature creep loading. This work investigates the effect of fatigue-creep interaction (FCI) on the fatigue life of QCr0.8 alloy. Experimental results reveal accelerated cyclic softening and decelerated stress relaxation in the alloy under FCI conditions, attributed to creep deformation and stress amplitude growth. The damage evolution mechanism of FCI is revealed by the results of the energy dispersive spectroscopy (EDS) and scanning electron microscopy (SEM). The decrease in fatigue-creep life of the QCr0.8 alloy is attributed to the fracture of the outer surface oxide layer, as well as the coupling development of creep voids and secondary cracks. Finally, a new fatigue-creep life prediction model has been developed, taking into account the increase in plastic strain energy resulting from stress relaxation and creep deformation behaviors. The study results provide substantial theoretical justification for the utilization of QCr0.8 alloy in the thrust chamber wall of reusable liquid rocket engines.

Microstructure evolution during oxidation of quinary Ti3(AlSiSn)C2 at high temperatures and induced probable performance

Quinary Ti3Al0.6Si0.2Sn0.2C2 and Ti3Al0.5Si0.4Sn0.1C2 solid solution bulks were synthesized via hot-pressing process. High temperature oxidation behaviors were then investigated over a temperature range of 800–1200 °C. The weight gain per surface area and oxidation layer thickness were measured to study the oxidation kinetics. The as-synthesized compounds with varying solid solution ingredients exhibited comparable oxidation kinetics which fitted a parabolic kinetic better with the oxidation duration of 0–20 h, while it appeared to get more complicated after prolonging the oxidation time. The microstructure evolution and phase compositions of the oxide scales during breakaway oxidation were characterized to illuminate the oxidation mechanism. The oxidation layers exhibited a multi-layer structure resulting from the disparities between the diffusion and migration energies of the multi-elements. Anticipated performance induced by high temperature oxidation was further explored through investigation on the crack self-healing and tribological optimization capacities. It was revealed that cracks could be filled by predominant TiO2 and Al2O3 with a high efficiency at 1000 °C during annealing in air. At 800 °C, Ti3Al0.6Si0.2Sn0.2C2 exhibited self-lubricating properties that was attributed to the formation of smoothing tribo-oxide films, as demonstrated by the increasing oxygen content of the friction surface during sliding.

Characteristics and hot corrosion behavior of NiCrAlY metal bonding layers prepared by different processes

The hot corrosion experiments of René N5 alloy coated with three different NiCrAlY metal bonding layers are carried out, that the layers are prepared by different methods (APS, HVAF and MIP). Compared with bare René N5 alloy samples, the hot corrosion resistance of coated samples is improved. It can be attributed to the small internal stress of the surface oxide layer on the coating sample, which is difficult to spall, reducing the degree of hot corrosion reaction. The hot corrosion resistance of NiCrAlY layers is MIP > HVAF > APS, which is positively positively related to the density of layers, because the influence of element diffusion in the process of hot corrosion is effectively slowed down.

Nano-scale corrosion mechanism of T91 steel in static lead-bismuth eutectic: A combined APT, EBSD, and STEM investigation

T91 steel is a candidate material for structural components in lead-bismuth-eutectic (LBE) cooled systems, for example fast reactors and solar power plants [1]. However, the corrosion mechanisms of T91 in LBE remain poorly understood. In this study, we have analysed the static corrosion of T91 in liquid LBE using a range of characterisation techniques at increasingly smaller scales. A unique pattern of liquid metal intrusion was observed that does not appear to correlate with the grain boundary network. Upon closer inspection, electron backscatter diffraction (EBSD) reveals a change in the morphology of grains at the LBE-exposed surface, suggesting a local phase transition. Energy dispersive X-ray (EDX) maps show that Cr is depleted in the T91 material near the LBE interface. Furthermore, we observed the dissolution of all Cr-enriched precipitates in this region. Although the corrosion is conducted in an oxygen deficient environment, both scanning transmission electron microscopy (STEM) and atom probe tomography (APT) reveal a thin surface oxide layer (presumably wüstite) at the LBE-steel interface. Using electron energy loss spectroscopy (EELS) in the STEM, as well as APT, the atomic scale elemental redistribution and 3D morphology of the corrosion interface is investigated. By combining results from these different techniques, several types of oxide phases and structures can be identified. Based on this detailed nano-scale information, we propose potential mechanisms of T91 corrosion in LBE.

Effect of Silver Addition on Microstructure, Phase Composition, Microhardness and Surface Oxide Layer Formation of Al0.5CoCrCu0.5FeNi and Al0.5CoCrCuFeNi High-Entropy Alloys

Effect of Silver Addition on Microstructure, Phase Composition, Microhardness and Surface Oxide Layer Formation of Al0.5CoCrCu0.5FeNi and Al0.5CoCrCuFeNi High-Entropy Alloys