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At least 559 records · Page 31

Correlation of Microstructure and Mechanical Properties of Metal Big Area Additive Manufacturing

Metal Big Area Additive Manufacturing (MBAAM) is a novel wire-arc additive manufacturing method that uses a correction-based approach developed at the Oak Ridge National Laboratory (ORNL). This approach is an integrated software method that minimizes the dynamic nature of welding and compensates for build height. The MBAAM process is used to fabricate simple geometry thin walled specimens, using a C-Mn steel weld wire, to investigate the scatter in mechanical properties and correlate them to the underlying microstructure. The uni-axial tensile tests show isotropic tensile and yield properties with respect to building directions, although some scatter in elongation is observed. Large scatter is observed in the Charpy Impact tests. The microstructure characterization reveals mostly homogenous ferrite grains with some pearlite, except for some changes in morphology and grain size at the interface between the build and the base plate. The measured properties and microstructure are compared with the toughness and strength values reported in the literature, and a hypothesis is developed to rationalize the differences. Overall, the MBAAM process creates stable, isotropic, and weld-like mechanical properties in the deposit, while achieving a precise geometry obtained through a real-time feedback sensing, closed loop control system.

36 MATERIALS SCIENCE↗

Microcomputed X-Ray Tomographic Imaging and Image Processing for Microstructural Characterization of Explosives

Microstructural characterization of composite high explosives (HEs) has become increasingly important over the last several decades in association with the development of high fidelity mesoscale modeling and an improved understanding of ignition and detonation processes. HE microstructure influences not only typical material properties (e.g., thermal, mechanical) but also reactive behavior (e.g., shock sensitivity, detonation wave shape). A detailed nondestructive 3D examination of the microstructure has generally been limited to custom-engineered samples or surrogates due to poor contrast between the composite constituents. Highly loaded (>90 wt%) HE composites such as plastic-bonded explosives (PBX) are especially difficult. Here, we present efforts to improve measurement quality by using single and dual-energy microcomputed X-ray tomography and state-of-the-art image processing techniques to study a broad set of HE materials. Some materials, such as PBX 9502, exhibit suitable contrast and resolution for an automatic segmentation of the HE from the polymer binder and the voids. Other composite HEs had varying levels of success in segmentation. Post-processing techniques that used commercially available algorithms to improve the segmentation quality of PBX 9501 as well as zero-density defects such as cracks and voids could be easily segmented for all samples. Aspects of the materials that lend themselves well to this type of measurement are discussed.

36 MATERIALS SCIENCE↗

Effect of Initial Microstructure on the Toughness of Coarse-Grained Heat-Affected Zone in a Microalloyed Steel

Toughness of the coarse-grained-heat-affected-zone (CGHAZ) strongly depends on the prior austenite grain size. The prior austenite grain size is affected not only by chemical composition, thermal cycle, and dissolution of second-phase particles, but also by the initial microstructure. The effect of base metal microstructure (ferrite/pearlite obtained by air cooling and martensite obtained by water-quenching) on Charpy impact toughness of the CGHAZ has been investigated for different heat inputs for high-heat input welding of a microalloyed steel. A welding thermal cycle with a heat input of 100 kJ/cm and 400 kJ/cm were simulated on the MMS-300 system. Despite a similar microstructure in the CGHAZ of both the base metals, the average Charpy impact energy for the air-cooled base metal was found to be higher than the water-quenched base metal. Through thermo-kinetic simulations, it was found that a higher enrichment of Mn/C at the ferrite/austenite transformation interface of the CGHAZ of water-quenched base metal resulted in stabilizing austenite at a lower A1 temperature, which resulted in a coarser austenite grain size and eventually lowering the toughness of the CGHAZ.

36 MATERIALS SCIENCE↗

Investigation of Microstructures and Tensile Properties of 316L Stainless Steel Fabricated via Laser Powder Bed Fusion

In this study, a thorough investigation of the microstructures and tensile properties of 316L stainless steel fabricated via laser powder bed fusion (L-PBF) was done. 316L stainless steel specimens with two different thicknesses of 1.5 mm and 4.0 mm fabricated under similar conditions were utilized. Microstructural characterization was performed using optical microscopy (OM) and scanning electron microscopy (SEM) equipped with electron backscatter diffraction (EBSD). Melt pools and cellular structures were observed using OM, whereas EBSD was utilized to obtain the grain size, grain boundary characteristics, and crystallographic texture. The 1.5 mm thick sample demonstrated a yield strength (YS) of 538.42 MPa, ultimate tensile strength (UTS) of 606.47 MPa, and elongation to failure of 69.88%, whereas the 4.0 mm thick sample had a YS of 551.21 MPa, UTS of 619.58 MPa, and elongation to failure of 73.66%. These results demonstrated a slight decrease in mechanical properties with decreasing thickness, with a 2.4% reduction in YS, 2.1% reduction in UTS, and 5.8% reduction in elongation to failure. In addition to other microstructural features, the cellular structures were observed to be the major contributors to the high mechanical properties. Using the inverse pole figure (IPF) maps, both thicknesses depicted a crystallographic texture of {001} <101> in their as-built state. However, when subjected to tensile loads, texture transitions to {111} <001> and {111} <011> were observed for the 1.5 mm and 4.0 mm samples, respectively. Additionally, EBSD analysis revealed the pre-existence of high-density dislocation networks and a high fraction of low-angle grain boundaries. Interestingly, twinning was observed, suggesting that the plastic deformation occurred through dislocation gliding and deformation twinning.

316L stainless steel↗

Impact of Powder Variability on the Microstructure and Mechanical Behavior of Selective Laser Melted Alloy 718

Powder-bed additive manufacturing processes use fine powders to build parts layer-by-layer. Alloy 718 powder feedstocks for selective laser melting (SLM) additive manufacturing are produced commercially by both gas and rotary atomization and are available typically in the 10-45 or 15-45 microns size ranges. A comprehensive investigation was conducted to understand the impact of powder variability on the microstructure and mechanical behavior of SLM 718 heat treated to Aerospace Material Specification (AMS) 5664. This study included sixteen virgin powders and three once-recycled powders within the 10-45 and 15-45 microns size ranges that were obtained from seven direct source suppliers and one reseller. Although alike as highly regular spheroids, these powders showed distinct differences in composition (especially Al, C and N contents), particle size distributions, and powder features such as degree of agglomeration, fusion and surface roughness. Compositional differences expectedly had the strongest impact on microstructure. High N and C contents formed TiN-nitrides and/or (Nb,Ti,Mo)-C carbides on the grain boundaries, prevented recrystallization during heat treatment, and resulted in retained (001)-scalloped shaped grains that ranged from 19 to 41 microns in average size. In the absence of this particle pinning, the average grain size of the heat treated SLM 718 ranged from 51 microns to 90 microns. Room temperature tensile and high cycle fatigue (HCF) testing compared as-fabricated (AF) and low stress ground (LSG) surface conditions. Tensile testing revealed consistent behavior between the two surface conditions and amongst the powder lots. The finer grained SLM 718 builds displayed the lowest tensile properties. A SLM 718 build fabricated from a powder with eight times lower C content showed statistically better tensile properties presumably due to enhanced coarsening of (delta)-Ni3Nb precipitates. The specimens from once-recycled powders had slightly higher tensile strengths and slightly higher ductility compared to their virgin equivalents; once-recycling also did not substantially degrade the mean HCF life. The LSG fatigue lives agreed with conventionally manufactured 718 data, while AF lives exhibited a knock-down due to surface roughness. The fatigue lives of AF specimens were statistically equivalent across powder lots except for one and failures typically initiated at stress concentrators associated with SLM surface asperities. Fatigue testing of low stress ground specimens result in both transgranular and within facet crack initiations. More than half of the cracks initiated from these facets for the machined condition; however, these facets appeared to be within grains that were larger-than-average in size. A nitrogen-atomized powder with fine prior particles of TiN-nitrides and M(Ti,Nb,Mo)C carbides from atomization on powder surfaces resulted in the best fatigue performance with segregation of these particles to the SLM 718 grain boundaries leading to higher resistance to early-stage crack propagation. Typically the fine-grained builds with minor phases along the grain boundaries did not perform well in fatigue, whereas a larger-grain build with lower carbon content and coarser delta-Ni3Nb precipitates showed the next best HCF response. Further details of the build microstructure and its impact on tensile and fatigue behavior was considered.

laser deposition↗

Microstructural Characterization of Laser Powder Bed Fusion (L-PBF) Additively Manufactured Inconel 718 for Aerospace Application

Alloy 718 (Inconel 718) is used for aerospace applications because of its excellent corrosion resistance and mechanical properties. This alloy is particularly applicable in manufacturing components subjected to high temperatures in rocket engines, aero-engines, and gas turbines. Properties for this alloy when processing on systems from similar and different Laser Powder Bed Fusion (L-PBF) machines provide subtle differences due to process parameters, feedstock, and machine configurations. A series of sixteen L-PBF AM Inconel 718 geometric feature build plates have been evaluated for microstructure using optical microscopy. This study presents the details of the microstructure analysis concerning geometry and different machine platforms. Microstructural investigations of these samples included average grain width measurement for all the X-Y and Y-Z build layers and are accompanied by process parameters and powder characterization. The present work concludes with a discussion on the importance of captured differences among builds to understand the practical limitations among AM platforms.

Additive Manufacturing↗

Effect of Heat Treatment on the Microstructure and Mechanical Properties of Monel K500 Alloy Fabricated Via L-PBF and LP-DED

This study examines and compares the effect of different heat treatments (HT) on the microstructure and mechanical properties of Monel K500 fabricated using laser powder bed fusion (L-PBF) and laser powder directed energy deposition (LP-DED) technologies. The as-fabricated Monel K500 specimens exhibited dendritic microstructure and elemental micro-segregation due to high cooling rates induced during the fabrication process. The applicability of HT proposed in the literature for wrought Monel K500 was investigated for L-PBF and LP-DED using four different HT procedures involving hot isostatic pressing (HIP), solution annealing (SA), and aging. The mechanical properties of test specimens were evaluated using uniaxial tensile testing at room temperature. The microstructural evolution of test specimens during HT was analyzed using a scanning electron microscope. For all HT conditions investigated, L-PBF Monel K500 specimens consistently displayed higher strength and lower ductility compared to the LP-DED counterparts. The HT procedure involving HIP at 1160°C for 3hr at 100 MPa, SA at 1100°C for 15 min, and three step aging at 610°C for 16 hr, 540°C for 6 hr, and 480°C for 8 hr resulted in highest strength for both L-PBF and LP-DED fabricated Monel K500.

Additive manufacturing↗

SOC Microstructural Analyzer

This program was designed to analyze the 3-phase microstructure of the electrodes of a solid oxide fuel cell (SOFC) or electrolysis cell (SOEC), both referred to in combination as a solid oxide cell (SOC). It is agnostic to the exact system, so it could be repurposed to analyze any 3-phase microstructure. This tool directly analyzes segmented voxel-based data that has been segmented into phase IDs (1,2,3). The voxels will be analyzed directly for: - tortuosity factors - triple phase boundaries - 2-phase interfacial areas, using a meshed isosurface - mean diameters of each phase, using an inscribed sphere method - standard deviation of the diameters of each phase, from the same inscribed sphere data - connectivity information Comprehensive information is available in the readme file (within the zipped repository in Markdown language, and also available here as a rendered PDF). Please cite this page / DOI, as well as https://doi.org/10.1111/jace.14775, for usage.

3D microstructure↗

Tuning Microstructure of Mesophase Pitch Carbon Fiber by Altering the Carbonization Ramp Rate

The microstructure of mesophase pitch carbon fibers (CFs) are tuned by varying ramp rates from 1 to 50 °C min –1 up to 1000 °C to study the effect of ramp rate on CFs’ microstructure, thermal and mechanical properties with the goal of offsetting the cost by decreasing cycle time. The ramp rates represent carbonization times ranging from 16.4 to 1.17 h, not including cool down. Differential scanning calorimetry, thermogravimetric analysis, and derivative thermogravimetry are used to investigate the impact ramp rate has on the thermal properties of mesophase pitch. It is found that lower ramp rates are endothermic in nature with a lower temperature onset and maximum weight loss. Higher ramp rates possess an exothermic nature with higher temperatures resulting in maximal weight loss over a smaller range of temperatures. Mechanical testing shows varying CF strengths and moduli dependent on ramp rate and an optimized process is developed to produce the strongest CF. Furthermore, microstructural characterization revealed that faster ramp rates lead to smaller interplanar spacings and larger crystallites but possessed greater disorder.

36 MATERIALS SCIENCE↗

Optimization of Processing, Microstructure, and Hardness of an Al–Ce–Ni–Mn–Zr Alloy With Laser Additive Manufacturing

Here, this study examines the processing behavior, microstructure, surface roughness, and hardness properties of an aluminum alloy containing 8.2 Ce, 4.5 Ni, 0.5 Mn, and 0.7 Zr (wt%) fabricated using laser powder bed fusion. Sixty samples were produced across a range of laser powers, scan speeds, and hatch spacings to evaluate their effect on porosity, hardness, and microstructural features. Porosity was measured using X-ray computed tomography, while microstructure and surface roughness were characterized by scanning electron (SEM) and laser confocal microscopy. High dense and cracking-free Al–Ni–Ce alloy was successfully manufactured. Porosity showed a U-shaped dependence on energy input, increasing under both insufficient and excessive melting conditions. Hardness increased with cooling rate due to finer cellular structures and solute redistribution. A general statistical model was developed to capture the relationships between processing parameters and material response. Results identify a narrow processing window defined by laser powers between 350 and 370 W, scan speeds from 1400 to 1800 mm/s, and hatch distances between 0.14 and 0.18 mm. Within this window, porosity is minimized (below 0.01%) and hardness is maximized (up to 160 HV), demonstrating that careful control of these parameters enables dense, high strength aluminum components suitable for demanding structural applications.

Aluminum alloys↗

Mechanical Milling – Induced Microstructure Changes in Argyrodite LPSCl Solid-State Electrolyte Critically Affect Electrochemical Stability

Microstructure of argyrodite solid-state electrolyte (SSE) critically affects lithium metal electrodeposition/dissolution. While the stability of unmodified SSE is mediocre, once optimized state-of-the-art electrochemical performance is achieved (symmetric cells, full cells with NMC811) without secondary interlayers or functionalized current collectors. Planetary mechanical milling in wet media (m-xylene) is employed to alter commercial Li 6 PS 5 Cl (LPSCl) powder. Quantitative stereology demonstrates how milling progressively refines grain and pore size/distribution in the SSE compact, increases its density, and geometrically smoothens the SSE-Li interface. Mechanical indentation demonstrates that these changes lead to reduced site-to-site variation in the compact's hardness. Milled microstructures promote uniform early-stage electrodeposition on foil collectors and stabilize solid electrolyte interphase (SEI) reactivity. Analysis of half-cells with bilayer electrolytes demonstrates the importance of microstructure directly contacting current collector, with interface roughness due to pore and grain size distribution being key. For the first time, short-circuiting Li metal dendrite is directly identified, employing 1.5 mm diameter “mini” symmetrical cell and cryogenic focused ion beam (cryo-FIB) electron microscopy. The branching sheet-like dendrite traverses intergranularly, filling the interparticle voids and forming an SEI around it. Importantly, mesoscale modeling reveals the relationship between Li-SSE interface morphology and the onset of electrochemical instability, based on underlying reaction current distribution.

25 ENERGY STORAGE↗

A Comprehensive Experimental Study on Microstructure‐Graded Graphite Anodes for Enhancing Fast‐Charging Capability of Lithium‐Ion Batteries

Lithium‐ion batteries with high gravimetric capacity density and improved cycle life performance under fast‐charging conditions are crucial for widespread electric vehicle (EV) adoption. This study investigates how designing graphite anode microstructure, specifically porosity, and particle‐size gradients, improves lithium‐ion (Li + ) transport during fast‐charging conditions. Three‐layered graphite anodes with varying porosity (24%, 36%, 46%) and particle size gradients (3, 5, 10 μm) were compared to a conventional single‐layered electrode in half‐cell configurations. At room temperature and high discharge rate (2C), both gradient structures showed significantly enhanced capacity retention (80% and 67% vs. 50%) compared to the conventional electrode, highlighting the effectiveness of microstructure engineering for fast charging. The study also investigated the temperature's impact on cycle life. After 200 cycles at 2°C and 45°C, all gradient structures demonstrated superior capacity retention (≈80%) compared to the conventional electrode (35%), suggesting the gradients mitigate degradation rate at high temperatures. Electrochemical impedance spectroscopy confirmed superior Li+ diffusion and lower resistivity in gradient electrodes. Simulations explored the influence of gradient profiles on reaction kinetics across the electrode thickness. Overall, this research demonstrates that the fast‐charging capability of graphite electrodes can be greatly enhanced by engineering the electrode microstructure, thereby making EV technology more accessible and appealing.

Ahmadi, Soma↗

An anisotropic viscoplasticity model for shale based on layered microstructure homogenization

Viscoplastic deformation of shale is frequently observed in many subsurface applications. Many studies have suggested that this viscoplastic behavior is anisotropic—specifically, transversely isotropic—and closely linked to the layered composite structure at the microscale. In this work, we develop a two-scale constitutive model for shale in which anisotropic viscoplastic behavior naturally emerges from semianalytical homogenization of a bilayer microstructure. The microstructure is modeled as a composite of soft layers, representing a ductile matrix formed by clay and organics, and hard layers, corresponding to a brittle matrix composed of stiff minerals. This layered microstructure renders the macroscopic behavior anisotropic, even when the individual layers are modeled with isotropic constitutive laws. Using a common correlation between clay and organic content and magnitude of creep, we apply a viscoplastic modified Cam-Clay plasticity model to the soft layers, while treating the hard layers as a linear elastic material to minimize the number of calibration parameters. We then describe the implementation of the proposed model in a standard material update subroutine. The model is validated with laboratory creep data on samples from three gas shale formations. We also demonstrate the computational behavior of the proposed model through simulation of time-dependent borehole closure in a shale formation with different bedding plane directions.

58 GEOSCIENCES↗

Microstructure‐Dependent Sodium Storage Mechanisms in Hard Carbon Anodes

Sustainable energy storage is essential to support the transition to renewables and meet the increasing demand for energy. Sodium‐ion batteries (NIBs) are attractive for grid‐scale energy storage due to the abundance and low cost of sodium, sustainability of other battery components, and electrochemical performance. Hard carbon (HC) is a leading anode material for NIBs, but its complex microstructure complicates the understanding of sodium storage mechanisms. Using X‐ray total scattering and density functional theory calculations, this study clarifies how HC's microstructural variations influence sodium storage across the slope (high potential) and plateau (low potential) regions of the potential capacity curve. In the slope region, sodium initially adsorbs at high‐binding energy defect sites and subsequently intercalates between graphene layers, adsorbing at low‐binding energy defect sites, correlating with different slopes observed during initial sodiation. Initial irreversibility arises from sodium trapping at surface defects and solid electrolyte interface formation. In the plateau region, sodium simultaneously intercalates and fills pores, influenced by pore size, interlayer spacing, and defect concentration. HCs with larger pore sizes form larger sodium clusters. In conclusion, the proposed mechanism underscores the role of microstructure engineering in enhancing HC performance and advancing NIBs for grid‐scale energy storage.

36 MATERIALS SCIENCE↗

Exploring the Microstructure-Property Relationship of Mg-Al-Mn alloys enhanced via Friction Stir Processing

Friction Stir Processing (FSP) is a solid-state thermomechanical processing technique that enables local grain refinement, densification, and homogenization of microstructure in metallic components. Here, FSP is applied to thin sheets of high-pressure die cast AM60 to address the porosity and heterogeneities inherent to the casting process. In this work, microstructure characterization is correlated to improvements in the static mechanical properties of the Mg-Al-Mn alloy system at various FSP processing conditions. Notably, there is a significant increase in the ductility and ultimate tensile stress of system following FSP. The dominant deformation mechanisms for the as-cast material and the FSP material are investigated. Finally, the fatigue life improvement is correlated to microstructure modifications that may lead to distinct behavior in crack initiation and crack propagation for the as-cast and FSP material.

Garcia, David↗

U-net architected deep material network training with microstructure local field information

The Deep Material Network (DMN) has recently emerged as a powerful reduced-order modeling framework for simulating the mechanical response of heterogeneous materials such as composites. Unlike most data-driven approaches that directly learn a material’s response under prescribed loading, the DMN acts as a homogenization operator, learning the kinematic constraints and mechanical interactions of the underlying microstructure. However, traditional DMN training relies exclusively on homogenized effective properties derived from Direct Numerical Simulations (DNS), discarding the rich local field data that govern microstructural interactions. In this work, we extend the DMN framework to incorporate such local field information into the offline training process. Utilizing a U-Net architecture, we augment the DMN training objective to include the first and second statistical moments of the local stress fields obtained from linear DNS. This ensures that the learned network topology not only fits the effective stiffness but also accurately reflects the internal local stress and strain partitioning of the microstructure. The results confirm that supervising the localization process during training yields a superior surrogate model, reducing local prediction errors by an order of magnitude and significantly improving generalization to unseen nonlinear constitutive behaviors compared to traditional DMNs.

36 MATERIALS SCIENCE↗

Understanding the Impact of Fuel on Surfactant Microstructure of Firefighting Foam

Abstract Aqueous film-forming foam is being phased out due to the environmental impacts of fluorinated surfactants contained in the firefighting foams. To develop an environmentally friendly firefighting foam, it is important to understand the factors controlling the firefighting performance of surfactants. Fuel transport through foam has been considered as a dominant mechanism for foam collapse. Therefore, the impact of fuels (heptane, octane and trimethylbenzene (TMB)) on surfactant microstructure was studied for three different types of surfactants (Capstone, Glucopon, and siloxane) that have applications in firefighting foam. Multiple techniques were used to identify the microstructure and interfacial properties of surfactants with and without exposure to liquid fuel. The ignition time of fuel vapor through foam and solubility of fuel through liquid surfactant solution were measured as well. This work shows fuel solubility has an impact on the surfactant microstructure and interfacial properties. In addition, fuel solubility and vapor pressure affect the ignition time of fuel vapors.

Engineering↗

Fatigue crack growth resistance of a mesoscale composite microstructure Haynes 282 fabricated via electron beam melting additive manufacturing

Materials synthesis via additive manufacturing gives unprecedented control over the solidified microstructure. While a number of studies have demonstrated the ability to produce spatially varying microstructures, little work exists to understand the behavior of such “composite” materials. In this work, we utilized electron beam melting to process Ni-based superalloy Haynes 282 and produce compact tension samples with a spatially varying mesoscale structure. Fatigue crack growth experiments reveal that the crack growth rate is dependent on the degree of microstructural heterogeneity. This work demonstrates that the crack growth resistance can be tailored within a component using electron beam melting additive manufacturing.

36 MATERIALS SCIENCE↗