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At least 91 records · Page 5

Surface Integrity and Oxidation of a Powder Metallurgy Ni-Based Superalloy Treated by Laser Shock Peening

Laser shock peening is a mechanical surface treatment which can induce large compressive residual stresses and microstructural changes in the material by using repetitive shocks from laser pulses. In this work, the surface integrity (surface microstructure, topography, hardness and residual stress) of a laser shock peening treated powder metallurgy Ni-based superalloy was investigated. Laser shock peening treatment introduces large plastic deformation especially at a depth of about 100 μm from the surface, which increases the local hardness. The residual stress from the surface to the interior of the sample was investigated by synchrotron X-ray diffraction. The maximum compressive stress reaches 400 MPa at the surface, while the depth of the compressive stress is about 0.7 mm. Lastly, the oxidation behavior of the treated and untreated samples was evaluated by thermal exposure at 700°C for 312 h. The LSP treatment decreased the thickness of oxide layer, thereby showing improved oxidation resistance.

36 MATERIALS SCIENCE↗

Migration energy barriers and diffusion anisotropy of point defects on tungsten surfaces

We report tungsten is one of the most promising candidates for plasma-facing materials in future fusion devices, owing to its high performance under extreme irradiation conditions. However, irradiation-induced surface morphology varies significantly, depending on the irradiation type, fluence, and flux. Therefore, it is critical to examine the dynamics of point defects on tungsten (W) surfaces to understand how irradiation affects surface morphology. In this study, we employ the Self-Evolving Atomistic Kinetic Monte Carlo (SEAKMC) method to search for potential migration paths of point defects on W (1 0 0), (1 1 0) and (1 1 1) surfaces. The first-principles calculations are then used to accurately determine the migration energy barriers. The obtained paths and barriers are incorporated into a kinetic Monte Carlo (KMC) model to determine trajectories and diffusivities, which are described by diffusion tensors to demonstrate their anisotropic features. Multiple diffusion mechanisms have been identified on different surfaces, with various anisotropy factors. Particularly, point defects on the W (1 1 0) surface have the highest diffusivities, with anisotropy factors independent of temperatures. In comparison, the anisotropy of the W (1 0 0) surface decreases as temperature increases, while the W (1 1 1) surface is isotropic for point defects. This study provides insights into defect transport properties on different surfaces, which are essential for understanding the early stages of irradiation-induced microstructural evolutions and surface morphology of tungsten.

36 MATERIALS SCIENCE↗

Carbon Support Microstructure Impact on High Current Density Transport Resistances in PEMFC Cathode

Cell voltages at high current densities (HCD) of an operating proton-exchange membrane fuel cell (PEMFC) cathode suffer from losses due to the local-O 2 and bulk-H + transport resistances in the catalyst layer. Particularly, the microstructure of high surface area carbon (HSC) support upon which both the platinum catalyst and ionomer are dispersed play a pivotal role in controlling the reactant transport to the active site in the catalyst layer. In this study, we perform a systematic analysis of the underlying microstructure of platinum-cobalt catalyst dispersed on various HSC supports in terms of their surface area and pore-size distribution. The carbon microstructure was found to strongly influence the PtCo nanoparticle dispersion, catalyst layer ionomer distribution and transport losses governing the performance at HCD. Catalyst layer electrochemical diagnostics carried out to quantify local-O 2 transport resistance and bulk-H + transport resistance in the cathode were found to be directly correlated to the micropore (<2 nm) and macropore (>8 nm) surface areas of the carbon support, respectively. Finally, a 1D-performance model has been developed to assimilate our understanding of the catalyst layer microstructure and transport resistances at HCD.

25 ENERGY STORAGE↗

Developing of nano sized fibrous eutectic silicon in hypereutectic Al–Si alloy by laser remelting

Laser surface melting followed by rapid solidification is an effective means to produce very fine microstructures with desirable surface properties because of the high rates of cooling associated with it. In the present study, the effect of rapid cooling on the silicon particle size, distribution, and morphology of hypereutectic Al–17wt.%Si and Al–20wt.%Si alloys have been investigated. A continuous-wave CO2 laser of wavelength 10.6 μm and a Trumpf Yb-YAG disk laser of wavelength 1.030 μm were used with a beam diameter of 1 mm and scanning speeds ranging from 5 to 100 mm/s. Rapid solidification increased the solubility of silicon in aluminum to approximately 5wt% and induced non-equilibrium hypoeutectic microstructures comprising large volume fractions of primary α-Al dendrites and ultrafine Al–Si eutectic of lamellar morphology. Both α-Al dendrites and the silicon particle sizes were significantly reduced from micron to nanoscale level. The morphology of silicon particles is modified from massive polygonal and plate-like to a mixture of fine fakes with round corners, feathery and fibrous, or a coral-like and thread-like structure. The eutectic silicon size and the interlamellar spacing were reduced to 30 and 10 nm, respectively. Furthermore, most of the silicon crystals in the eutectic region and the aluminum dendrites contained a significant number of twins which were considered as an essential contributor to the mechanism of growth and branching. Microhardness values increased two to threefold due to the refinement of the microstructural constituent.

42 ENGINEERING↗

Dual microscopy to explore enhanced atmospheric ice nucleation on multi-component aerosols

Using an optical microscopy setup adapted to in-situ studies of ice formation at ambient pressure, we examined a specific multicomponent mineral, microcline, with the ultimate aim of gaining a more realistic understanding of ice nucleation in Earth’s atmosphere. We focused on a perthitic feldspar, microcline, to test the hypothesis that co-existence in some feldspars of K-rich and Na-rich phases are contributing to enhanced ice nucleation. On a sample deliberately chosen to contain lamella, a typical perthitic microstructure, and flat surface regions next to each other, we performed a series of ice formation experiments. We found microcline to promote ice formation, causing a large number of ice nucleation events at around - 27°C. The number of ice nuclei decreased from experimental run to experimental run, indicating surface aging upon repeated exposure to humidity. An analysis of 10 experimental runs of identical conditions did not reveal an obvious enhancement of ice formation at the lamellar microstructure. Instead, we find efficient nucleation at various surface sites that produce orientationally aligned ice crystallites with asymmetric shape. Based on this observation we propose that surface steps running along select directions produce microfacets of an orientation that is favorable to enhanced ice nucleation, similar to previously reported for K-rich feldspars.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Atomic force microscopy and scanning electron microscopy characterization of the controlling of surface morphology of epoxy‐amine‐cured spin‐coated films

Abstract Atomic force microscopy (AFM) was successfully used to study spin‐coated, amine‐cured epoxy film microstructure and morphology. The air‐epoxy and epoxy‐substrate interfaces were examined using tapping‐mode height and phase imaging AFM. The impact of relative humidity on the morphology and microstructure of the surfaces was determined. AFM was able to elucidate the changes on the surface as relative humidity during processing increased. It was observed that large nodular formations formed on the epoxy surface expose to the air but not epoxy surface formed on the substrate in addition to varying regions of more or less compliant structures, which was attributed to carbamate formation caused by the amine curing agent reaction with atmospheric CO 2 . Scanning electron microscopy (SEM) was used to further elucidate interface and interphase morphology of spin‐coated epoxies. Experimentation also demonstrated that post‐curing above the glass transition did not change the morphology structure, suggesting surface structures are “locked‐in.” SEM was used to further elucidate how the interface and interphase change with changing environmental conditions at both the air‐epoxy and epoxy‐substrate interface/interphases, including the impact of atmospheric CO 2 on Marangoni cell formation.

Shenk, Timothy M.↗

ZrN Phase Formation, Hardening and Nitrogen Diffusion Kinetics in Plasma Nitrided Zircaloy-4

Plasma nitridation was conducted to modify the surfaces of Zircaloy-4. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Raman analysis were used to characterize microstructures and phases. Surface indentation and cross-sectional indentation were performed to evaluate mechanical property changes. Nitridation forms a thin layer of ZrN phase, followed by a much deeper layer affected by nitrogen diffusion. The ZrN phase is confirmed by both TEM and Raman characterization. The Raman peaks of ZrN phase show a temperature dependence. The intensity increases with increasing nitridation temperatures, reaches a maximum at 700 °C, and then decreases at higher temperatures. The ZrN layer appears as continuous small columnar grains. The surface polycrystalline ZrN phase is harder than the bulk by a factor of ~8, and the nitrogen diffusion layer is harder by a factor of ~2–5. The activation energy of nitrogen diffusion was measured to be 2.88 eV. The thickness of the nitrogen-hardened layer is controllable by changing the nitridation temperature and duration.

36 MATERIALS SCIENCE↗

Surface fluctuating hydrodynamics methods for the drift-diffusion dynamics of particles and microstructures within curved fluid interfaces

Here we introduce fluctuating hydrodynamics approaches on surfaces for capturing the drift-diffusion dynamics of particles and microstructures immersed within curved fluid interfaces of spherical shape. We take into account the interfacial hydrodynamic coupling, traction coupling with the surrounding bulk fluid, and thermal fluctuations. For fluid-structure interactions, we introduce Immersed Boundary Methods (IBM) and related Stochastic Eulerian-Lagrangian Methods (SELM) for curved surfaces. We use these approaches to investigate the statistics of surface fluctuating hydrodynamics and microstructures. For velocity autocorrelations, we find characteristic power-law scalings $τ^{-1}, τ^{-2}$, and plateaus can emerge. This depends on the physical regime associated with the geometry, surface viscosity, and bulk viscosity. This differs from the characteristic $τ^{-3/2}$ scaling for bulk three dimensional fluids. We develop theory explaining these observed power-laws associated with time-scales for dissipation within the fluid interface and coupling to the surrounding fluid. We then use our introduced methods to investigate a few example systems and roles of hydrodynamic coupling and thermal fluctuations including for the kinetics of passive particles and active microswimmers in curved fluid interfaces.

97 MATHEMATICS AND COMPUTING↗

Optimization of WAAM Process to Produce AUSC Components with Increased Service Life

Additive manufacturing has the potential to revolutionize industrial hardware and unlock efficiency gains through the fabrication of geometries and architectures not possible by conventional processing. Wire Arc Additive manufacturing (WAAM) process is a class of directed energy deposition process enabling higher build rate and allowing custom wire feedstock allowing spatial variation of microstructure. The larger spot size and lower speed creates a larger melt pool, reducing residual stress and often time creating directional/columnar microstructure for Ni-superalloy. The use of flexible platform provides freedom in deposition strategy, which can accommodate complex substrates, including feature addition onto existing structures, non-flat layers, and repair methods. However, the certification of the final component needs to match the strength requirement. Hence, the quality of the component produced is stringently monitored to avoid buildup of residual stress, cracks, porosity and to reduce detrimental segregated phases commonly observed during alloy solidification. Simulation plays a huge role in predicting the melt pool dimension and can be used to optimize the process parameter. Similar development is also required to perform physics-based modeling of microstructural development in WAAM that can predict the microstructural features during solidification and can be used to optimize the process more effectively. To move toward this goal, Raytheon Technologies Research Center together with Siemens worked to create a set of computational tools to control the process parameters, enable on-line measurements and acquisition with feedback to the optimized process parameters, and eventually track material evolution through each step of the additive process. Computational fluid dynamics is used for accurate prediction and calibration of the thermal field during WAAM process. and phase field models for microstructure evolution as a function of processing parameters to establish a connection between additive parameters and the final microstructure. Here we report cellular automata (CA) model development to predict the dendritic microstructure evolution with surface and bulk nuclei for single track and multiple layers. The CA model was developed to account for secondary element addition and predict segregation, local melting, and latent heat release as well as prediction of Euler angles from orientation information and validated against experiments. This framework was utilized to tailor spatially-varying composition in a part by appropriately controlling the microstructure evolution during the additive process. Functionally graded Haynes 282 alloy with high Cr content at the surface was tested for oxidation and mechanical properties. An advanced physics-based reaction-diffusion model predicting the simultaneous creation of chromium oxide and alumina is developed and validated to extend life expectancy of the WAAM manufactured high temperature part. A machine-learning data-driven framework establishing the process-structure relationship from a dataset of real microstructure images and corresponding process history data has been developed and implemented in the NX Siemens design system. The digital twin configuration along with the tool path generation enabled prediction of WAAM component buildup time and the techno-economic analysis provided a favorable option for all 4 cases with 15-40% cost reduction.

33 ADVANCED PROPULSION SYSTEMS↗

Surface and subsurface characterization of laser-interference structured Ti6Al4V

Ti6Al4V specimens were exposed to high-energy laser pulses of 1.24 J/cm 2 fluences per pulse using a two-beam optical configuration to attain laser-interference. In addition to the formation of periodic surface textures by laser-interference, scanning electron microscope (SEM) images demonstrated several microstructural changes on the surface processed. Moreover, the surface and subsurface of Ti6Al4V specimens were characterized for the as-received and laser-interference processed conditions using x-ray photoelectron spectroscopy (XPS) and electron energy dispersive spectroscopy (EDS). The XPS data showed that this laser technique is effective at removal of surface contaminants for Ti6Al4V. The XPS analysis also revealed the formation of an oxy-nitride layer on the laser treated material. Finally, the microstructure analysis indicates that grain refinement, dendrite and twin structures were found near the surface due to laser processing.

36 MATERIALS SCIENCE↗

Effects of varying gelatin coating concentrations on RANKL induced osteoclastogenesis

Here, we assessed the effects of varying concentrations of gelatin coating on Receptor Activator of Nuclear Factor κ-B Ligand (RANKL)-induced RAW264.7 murine macrophage differentiation into osteoclast (OC) via osteoclastogenesis. The microstructures of coating surfaces with different concentrations of gelatin were examined by scanning electron microscopy and atomic force microscopy. Increased gelatin coating concentrations led to decreased gel rigidity but increased surface adhesion force attenuated OC differentiation and the decreased actin ring formation in RANKL-induced osteoclastogenesis. The decreased actin ring formation is associated with decreased lysosomal-associated membrane protein 1 (LAMP1) activity and bone resorption in the differentiated OCs with different gelatin coating concentrations as compared to the cells differentiated without gelatin coatings. In addition, increasing concentrations of gelatin coating attenuated the medium TGF-β1 protein levels and the expression levels of TGF-β and type-I (R1) and type-II (R2) TGF-β receptors in OCs, suggesting the gelatin-induced suppression of TGF-β signaling for the regulation of RNAKL-induced OC differentiation. Taken together, these findings showed that changes in gelatin coating concentrations, which were associated with altered gel thickness and substrate rigidity, might attenuate TGF-β signaling events to modulate OC differentiation and concomitant actin ring formation and bone matrix resorption in RANKL-induced osteoclastogenesis.

60 APPLIED LIFE SCIENCES↗

Optimization of stochastic feature properties in laser powder bed fusion

Process parameter selection in laser powder bed fusion (LPBF) controls the as-printed dimensional tolerances, pore formation, surface quality and microstructure of printed metallic structures. Measuring the stochastic mechanical performance for a wide range of process parameters is cumbersome both in time and cost. As such, in this study, we overcome these hurdles by using high-throughput tensile (HTT) testing of over 250 dogbone samples to examine process-driven performance of strut-like small features, ~1 mm 2 in austenitic stainless steel (316 L). The output mechanical properties, porosity, surface roughness and dimensional accuracy were mapped across the printable range of laser powers and scan speeds using a continuous wave laser LPBF machine. Tradeoffs between ductility and strength are shown across the process space and their implications are discussed. While volumetric energy density deposited onto a substrate to create a melt-pool can be a useful metric for determining bulk properties, it was not found to directly correlate with output small feature performance.

316 L stainless steel↗

Surface Film Formation on Al-V Alloys with Far-From-Equilibrium Microstructure

Nanocrystalline supersaturated Al-V alloys produced by high-energy ball milling have been reported to exhibit enhanced corrosion resistance and mechanical properties compared to commercial Al alloys. Corrosion of passive alloys such as Al-V alloy relies on the characteristics of the surface film, which is studied using scanning/transmission electron microscopy and time-of-flight secondary ion mass spectrometry. The effect of microstructure and composition on the surface film has been investigated after different immersion periods (30 min, 2 h, and 1 day) in 0.1 M NaCl. The surface film was complex and composed of oxidized Al and V. The heterogeneous surface film was observed due to the presence of secondary phases and initiation of localized corrosion. The void formation was observed beneath the surface film that would potentially cause pitting corrosion. The generation of nano-sized voids was dependent on grain orientation. Compared to pure Al, the chloride penetration is suppressed in Al-V alloys. The effect of composition and microstructure on surface film formation and attendant corrosion behavior is discussed herein.

36 MATERIALS SCIENCE↗

Microscale drivers and mechanisms of fracture in post-processed additively manufactured Ti–6Al– 4 V

Herein, we focus on understanding the microstructure-fracture correlations in a Ti–6Al– 4 V alloy additively manufactured via electron beam melting (EBM) and subjected to various post-process heat-treatments. Specifically, the as fabricated material is subjected to a sub-transus heat-treatment followed by air-cooling and a super-transus heat-treatment followed by either air- or furnace-cooling. Next, a series of in-situ single edge notch tension (SENT) tests are carried out under a high-resolution digital optical microscope. The panoramic high-resolution images captured during the in-situ tests are then used to characterize the planar deformation on the specimen surface using microstructure-based digital image correlation (DIC). Additionally, the results of the in-situ SENT tests together with DIC and post-mortem fractographic analyses provided us with a better understanding of the microstructure-fracture correlations in these materials. Our results show that the fracture mechanism of the as fabricated and sub-transus heat-treated materials is essentially the same, while the changes in the microstructure following the super-transus heat-treatments significantly affects the fracture mechanism. In this case, several microcracks of hundreds of microns in length first nucleate away from the deformed notch following extreme plastic deformation at discrete locations. Furthermore, the location of these microcracks in the super-transus heat-treated materials is extremely sensitive to the details of the underlying microstructure.

36 MATERIALS SCIENCE↗

High-Sensitivity Low-Energy Ion Spectroscopy with Sub-Nanometer Depth Resolution Reveals Oxidation Resistance of MoS 2 Increases with Film Density and Shear-Induced Nanostructural Modifications of the Surface

For decades, density has been attributed as a critical aspect of the structure of sputter-deposited nanocrystalline molybdenum disulfide (MoS 2 ) coatings impacting oxidation resistance and wear resistance. Despite its importance, there are few examples in the literature that explicitly investigate the relationship between the density and oxidation behaviors of MoS 2 coatings. Aging and oxidation are primary considerations for the use of MoS 2 coatings in aerospace applications as they inevitably experience prolonged storage in water and oxygen-rich environments prior to use. Oxidation that is either limited to the first few nanometers or through the bulk of the coating can result in seizure due to high initial coefficients of friction or component failure from excessive wear. High-sensitivity low-energy ion spectroscopy (HS-LEIS) and Rutherford backscattering spectrometry (RBS) are both used to understand the extent of oxidation throughout the first ~10 nanometers of the surface of pure sputtered nanocrystalline MoS 2 coatings after high-temperature aging and how it is impacted by the density of coatings as measured by RBS. Results show that low-density coatings (ρ = 3.55 g/cm 3 ) exhibit a more columnar microstructure and voiding, which act as pathways for oxidative species to penetrate and interact with edge sites, causing severe surface and subsurface oxidation. Furthermore, HS-LEIS of surfaces sheared prior to oxidation reveals that the oxidation resistance of low-density MoS 2 coatings can be significantly improved by shear-induced reorientation of the surface microstructure to a basal orientation and elimination of pathways for oxygen into the bulk through compaction of surface and subsurface voids.

36 MATERIALS SCIENCE↗

Fatigue Testing and Characterization of Pre-hydrided Zircaloy-4 Cladding Tubes

The solubility of hydrogen in Zircaloy-4 (Zry-4) at the cladding operating temperature is near 100 wt. ppm. Above this solubility limit, excess hydrogen precipitates as δ-hydride platelets in the cladding material. Because of the effect of the thermal gradient across the cladding thickness on the migration and precipitation of hydrogen, hydride rims are often observed at the cladding outer surface; under excessive corrosion conditions hydride blisters are possible. It is well known that the fatigue of metal alloys, especially high cycle fatigue, is sensitive to the status of surface including the microstructure, roughness, and residual stress. Thus, the question considered herein, is whether excessive hydrogen pickup modifies the microstructure such that it has a degradation effect on the fatigue performance of cladding during operation. This report describes the evaluation of fatigue performance of a pre-hydrided Zry-4 cladding. A commercial Zry-4 was polished and pre-hydrided to 800 ppm and 1300 ppm H contents. The fatigue testing was conducted under strain control at 5 Hz with fully-reversed bending by using a cyclic integrated reversible bending fatigue tester (CIRFT). Six specimens with 1300 ppm and one specimen with 800 ppm were tested. Significant variation in test results were observed. While two of the 1300 ppm specimens failed with less than 1 ×10 5 cycles (at 0.32% and 0.41%), the four other samples did not fail over the strain amplitude range of 0.25% to 0.38%. Interestingly, the fracture initiation site of the failed samples was on the outside diameter (OD) surface rather than on the inside diameter (ID) surface as is typical for the as-polished cladding. This suggested a degrading effect of the hydriding process. Subsequently, three of the unfailed specimens were then further tested at ~0.43% to observe where failure initiation occurred. Significant variation was also observed in these three specimens. One specimen failed at ~9000 cycles while the two others failed at 43000 and 1.06 ×10 5 cycles. The performance here correlated to the location of failure initiation; failure initiated on the OD in the sample that failed after 9000 cycles while it initiated on the ID in the sample that failed after 43000 and 1.06 ×10 5 cycles. Flat features at the OD initiation sites suggest a brittle hydride feature on the surface of those samples was the cause of the degradation in fatigue performance, though the overall hydrogen levels in all samples was similar. A summary of all the observations is provided below: • The un-failed specimens with 1300 ppm H were cycled to failure with a higher amplitude near 0.43%. In addition, the fatigue-treated specimen tended to have a longer fatigue at the same induced amplitude. • Fractography revealed a mixed failure mode for the pre-hydrided specimen. Particularly, the specimen with fracture initiation site (FIS) located on the outer diameter surface of tube tended to have a shorter fatigue life than that of FIS on the inner diameter surface. • Etched cross section was shown to have hydride platelets aligned with tube longitudinal axis as expected, and the density of hydrides is at the similar level as in literature data. Meanwhile, a LECO procedure was applied for hydrogen concentration measurement, which showed the measured hydrogen contents are close to the nominal value. • With the polished cladding tube as baseline, O’Donnell-Lager (O-L) analysis showed that a decrease of about 50% in reduction-of-area (RA) would be needed for the O-L fitting to the fatigue data of 1300 ppm cladding. The suggestion for the next steps is provided.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Extent of interlocking and metallurgical bonding in friction riveting of aluminum alloy to steel

In this study, the joining of 6061-T6 aluminum alloy and DP590 steel using a M42 steel rivet via friction riveting technique is investigated. The surface morphology and microstructure characterization reveal the formation of an anchor zone that imparts mechanical interlock as well as the formation of metallurgical bonds at the interface of aluminum and steel. A combination of interlocking and bonding results in the achievement of a high load-carrying capacity of 5.7 kN during lap shear testing at room temperature. A finite element-based computational model was developed which accurately predicted the lap shear response of the joint. The model revealed that the metallurgical bond formed during fric-riveting adds 39% peak load strength to the joint. An extensive microstructural investigation, post-lap-shear fractography, and the modeling results, together provided insights on the joint failure mechanism. In conclusion, this study highlights that friction riveting is a promising method for aluminum-to-steel dissimilar joining, which is important for lighweighing automotive vehicles for energy efficiency.

36 MATERIALS SCIENCE↗