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At least 163 records · Page 9

7 Innovations in high-rate composite manufacturing: integrating additive manufacturing with compression molding process

Advanced composites play a pivotal role in modern engineering, offering exceptional strength-to-weight ratios and tailored properties, essential for various industries. High-rate composite manufacturing techniques have rapid production capabilities, which are essential for meeting the demands of industries requiring cost-saving, efficiency, and quick turnaround times. This chapter explores the Additive Manufacturing- Compression Molding (AM-CM) system developed by Oak Ridge National Laboratory (ORNL) for advanced composites manufacturing. The AM-CM system integrates additive manufacturing with compression molding, facilitating the production of polymer composite parts with superior mechanical properties and meticulously controlled microstructures. This innovative system not only ensures precise material deposition but also operates as a fast composite manufacturing process, enhancing productivity and performance, which are needed attributes across industrial applications. Through comprehensive mechanical testing and microstructural analysis, AM-CM promotes remarkable fiber alignment and reduced porosity in composite parts compared to alternative thermoplastic high-rate composite manufacturing methods. Furthermore, AM-CM enables overmolding reinforcement using continuous carbon fiber and supports selective reinforcement through customizable toolpaths. It also facilitates the production of hybrid materials to achieve tailored mechanical properties. Future advancements in AM-CM technology aim to enhance process efficiency, broaden material versatility, and improve part performance. This involves exploring novel materials, advancing process monitoring, implementing automation technologies, and integrating artificial intelligence (AI) and machine learning (ML) for predictive modeling and real-time optimization in composite manufacturing. These developments will establish the AM-CM system as a transformative technology in composite manufacturing, driving innovation across industries.

Hassen, Ahmed [ORNL] (ORCID:0000000328521222)

Impacts of Biomass Feedstock Pre-Processing on Heat and Mass Transfer During Pyrolysis Using X-Ray Computed Tomography and Multiscale Modeling

Knowledge of the transport properties of biomass particles such as porosity, tortuosity, and permeability is paramount for high-fidelity modeling of biomass pyrolysis due to the heat and mass transfer limitations imposed by particle microstructure. X-ray computed tomography (XCT) is a non-destructive imaging method that enables full 3D reconstructions of the biomass particle microstructure with high resolution, permitting direct calculation of porosity, tortuosity, and permeability from real particle geometries. In this study, XCT imaging revealed the 3D microstructures of particles and chars from pyrolytic conversion of cylindrically cut or milled/pelletized loblolly pine samples. The porosity, tortuosity, and permeability were calculated directly from the XCT geometries via open-source microstructural analysis tool MATBOX+TauFactor (https://github.com/NREL/MATBOX_Microstructure_analysis_toolbox) and computational fluid dynamics (CFD) simulations using our solver, Mesoflow (https://github.com/NREL/mesoflow). These properties were used in a reactor scale model developed in COMSOL of the single particle reactor at NREL to investigate the impact of feedstock pre-processing on biomass conversion during pyrolysis with rigorous experimental validation.

biomass

Development of Innovative Non-Concentrated Alloy (NCA) Fuel Cladding for Advanced Nuclear Reactors

As the nuclear energy sector advances toward next-generation reactors, the need for high-performance fuel cladding materials has become increasingly urgent. Traditional alloys like zirconium and stainless steel are reaching their performance limits under higher temperatures, more corrosive coolants, and extended irradiation. This report presents the development of a new class of fuel cladding materials based on Non-Concentrated Alloys (NCAs) ? multi-element systems designed to deliver enhanced mechanical strength, corrosion resistance, and radiation tolerance. Through a combination of computational modeling (Computer Coupling of Phase Diagrams and Thermochemistry: CALPHAD), simulation-guided alloy selection, and experimental fabrication via arc melting and spark plasma sintering (SPS), three strategic alloy design paths were explored: (1) FeCrAl-based NCAs, (2) refractory-lean neutron-efficient alloys, and (3) equimolar high-entropy compositions. Microstructural analysis confirmed the formation of stable body-centered cubic BCC_A2 phases, while mechanical testing demonstrated hardness values significantly exceeding those of conventional cladding materials. The results highlight the tunability of NCA systems and their potential for balancing strength and ductility ? a critical consideration for in-reactor performance. Looking forward, future work will focus on thermomechanical optimization, CALPHAD refinement, and benchmarking against industry standards to enable scalable deployment. This work not only advances the science of nuclear materials but also supports broader goals in nuclear safety, performance, and nuclear energy innovation.

36 - MATERIALS SCIENCE

A Machine Learning Approach to Quantitative Analysis of Enamel Microstructure from Scanning Electron Microscopy Images

Dental enamel, the outermost tissue of mammalian teeth, must withstand a lifetime of wear and cyclic contact. To meet this demand, enamel possesses a combination of high hardness and resistance to fracture, properties that are typically mutually exclusive. The impressive damage tolerance has been attributed largely to decussation of the enamel rods, the principal unit of its microstructure. As such, enamel is inspiring the design of next‐generation structural materials. However, quantitative descriptions of the decussated enamel rod microstructure remain limited due to challenges encountered in applying computed tomography and in acquiring quality images appropriate for traditional digital processing methods. Here, a machine learning segmentation method is applied to images of the enamel obtained using scanning electron microscopy to support quantitative analysis of the microstructure. A pretrained convolutional neural network is used to expand the input training image dataset to allow the training of a random forest classifier, which ultimately segments the image with a very small training set ( n = 3 images). A validation of this segmentation method is presented, in addition to its application to calculate relevant microstructural parameters for images of tooth enamel from selected mammalian species. The methodology applied here is equally applicable to other hard tissues.

36 MATERIALS SCIENCE

Two-Dimensional Nonlinear Finite Element Analysis of CMC Microstructures

Detailed two-dimensional finite element analyses of the cross-sections of a model CVI (chemical vapor infiltrated) SiC/SiC (silicon carbide fiber in a silicon carbide matrix) ceramic matrix composites are performed. High resolution images of the cross-section of this composite material are generated using serial sectioning of the test specimens. These images are then used to develop very detailed finite element models of the cross-sections using the public domain software OOF2 (Object Oriented Analysis of Material Microstructures). Examination of these images shows that these microstructures have significant variability and irregularity. How these variabilities manifest themselves in the variability in effective properties as well as the stress distribution, damage initiation and damage progression is the overall objective of this work. Results indicate that even though the macroscopic stress-strain behavior of various sections analyzed is very similar, each section has a very distinct damage pattern when subjected to in-plane tensile loads and this damage pattern seems to follow the unique architectural and microstructural details of the analyzed sections.

Mital, Subodh K.

Informed unsupervised machine learning analysis of dislocation microstructure from high-resolution differential aperture X-ray structural microscopy data

This study leverages high-resolution differential-aperture X-ray structural microscopy (DAXM) to probe the local dislocation structure in deformed 304L-stainless steel at small strain, by measuring the lattice rotation and deviatoric elastic strain with a sub-micron resolution. For a single grain in a polycrystalline specimen, the measured lattice rotation field over the measured volume exhibited a multimodal distribution while the deviatoric elastic strain showed a single-mode distribution. An unsupervised Cauchy mixture machine learning model was developed to resolve the multimodal distribution of the lattice rotation. By mapping the lattice rotation data associated with each Cauchy peak in the model back onto the measured volume, we identify contiguous regions of the crystal rotated near the average values corresponding to the peaks of the overall rotation distribution. These regions represent the grain subdivision in the microstructure. Finally, the dislocation density tensor was also computed and its norm was laid over the rotation field to detect the subgrain boundaries. This step provided a validation of the Cauchy mixture model for the analysis of the lattice rotation distribution. The current study highlights the integration of advanced X-ray microscopy techniques with data-driven analysis methods to uncover detailed microstructure scales in deformed crystals.

Machine learning; Lattice rotation; High-energy X-

Analysis of Base Metal Microstructures and Mechanical Properties of a Single-Piece, Spin-Formed Forward Pressure Vessel Bulkhead

In 2012, a pathfinder forward pressure vessel bulkhead (FPVBH) for the Orion Multi-Purpose Crew Vehicle (MPCV) was fabricated using aluminum (Al) alloy 2219. The demonstration article was offered as a replacement for the baseline configuration, which at that time was a multi-piece welded construction using aluminum-lithium (Al-Li) alloy 2195. In 2014, the NASA Engineering and Safety Center (NESC) funded a Phase I effort to explore spin-forming as a manufacturing method to produce a complex-shaped, single-piece FPVBH for the crew module (CM) [1]. The primary focus of the NESC effort was to expand spin-forming technology to the fabrication of an Al-Li 2195 FPVBH. As a result, limited testing and analysis was performed on the original Al 2219 article. In this study, a sufficiently large plate of Al 2219 was not available for the fabrication of a FPVBH. Therefore, the forming blank comprised two plates (from different lots) butt welded together using a single friction stir weld. The welded forming blank was then spin formed into the FPVBH configuration and heat treated to the T62 temper. Mechanical property testing of the spin-formed 2219-T62 FPVBH revealed that the tensile properties were comparable to the Metallic Material Properties Development and Standardization (MMPDS) A-basis allowable for Al 2219-T6 wrought products. However, post-spin forming application of the standard heat treatment produced large, recrystallized grains in the material. The response varied within the two plates; one plate lot exhibited nearly complete recrystallization, while the other lot contained bands of recrystallization. Although no reduction in tensile properties was observed due to these microstructural variations, a more detailed investigation was recommended to better understand the effect of spin forming on the recrystallization mechanism and the impact on other material properties. The current study examined the microstructure and mechanical properties of the fully processed Al 2219-T62 FPVBH with emphasis on comparing differences between the two plates. Testing was limited to the cone region of the FPVBH. The two specific tasks in this study were: a) Characterization of the microstructure and mechanical properties in the two plates used in the FPVBH. b) Isolation of the impact of each step in the thermo-mechanical processing (TMP) sequence of the FPVBH on recrystallization and grain growth. Mechanical property testing sampled regions containing both large, recrystallized and small, unrecrystallized grains. Tensile strengths and elongations were equivalent in both regions and exceeded MMPDS A-basis allowables. Fracture toughness was equivalent in both regions and fracture morphology was typical of aluminum alloys. The fatigue precrack region of the fracture toughness specimens appeared more faceted in the recrystallized plate. This suggests that property testing that is more sensitive to grain size, such as fatigue crack growth rate and stress corrosion cracking, may be warranted. Alcoa reviewed the production records for the two plate lots and confirmed that composition of both plates was within the allowable range for Al 2219 and that plate processing steps were all performed within production limits. However, the Fe content was notably higher in the fully recrystallized plate, resulting in a greater volume fraction of large Fe-bearing inclusions and Al-Cu constituent particles. Alcoa did not provide details regarding plate processing variables for the two plate lots. It was surmised that deformation by hot rolling was the most accurate TMP simulation of commercial spin forming within a laboratory setting. Both hot rolling and spin forming comprise combinations of shear and compressive deformation. The through-thickness strain caused by hot rolling is symmetrical about the mid-plane, as the rollers contact both sides of the material. Shear strains are maximum at the inner and outer surfaces and trend toward zero at the mid-thickness. In contrast, spin forming utilizes a single roller on the outer surface, producing a gradient in shear stress through the thickness. Shear strains in spin-formed material are highest at the outer surface due to direct contact with the roller, and trend toward zero at the inner surface. Consequently, there will undoubtedly be some discrepancies in the mechanical response of hot-rolled and spin-formed products in the through-thickness direction. Interrupted TMP simulations were performed on remnant plate from the FPVBH forming blank in order to isolate the effects of a post-weld anneal, spin-forming deformation/thermal cycling, and solution heat treatment (SHT) on development of the recrystallized microstructures. Analysis confirmed that large, recrystallized grains formed exclusively during SHT and only after a certain deformation level was exceeded. Remnant plate from both lots that received thermal processing only did not exhibit recrystallization but exhibited fully recrystallized microstructures when processed by hot rolling. This indicates that (1) the level of deformation exceeded the critical level for recrystallization in both plates and (2) that the level of deformation during hot rolling was greater than that which accumulated during spin forming of the FPVBH. Comparison of the hot-rolled plate with the spin-formed material showed that the recrystallized grain size was larger in the FPVBH, providing further evidence that deformation levels were lower in the FPVBH. The most plausible explanation for the differing degrees of recrystallization in the two plates is particle stimulated nucleation (PSN) at the Fe-bearing inclusions and large Al-Cu constituent particles. In the plate with higher solute content, the greater volume fraction of these particles reduces the deformation level required to promote recrystallization. During spin forming the critical deformation level was likely exceeded for the higher Fe content plate resulting in a fully recrystallized microstructure. The lower Fe content plate developed a microstructure that exhibited bands of recrystallization due to the combination of a non-uniform distribution of particles and deformation. The critical deformation required for recrystallization was likely only exceeded during spin forming in regions of higher particle content. While there were differences in Fe content between these lots of Al 2219 plate, the composition of both was within defined alloy limits and Alcoa reported no anomalies during plate production. The observed differences in recrystallization after spin forming may reflect the inherent variability between these two lots of plate. The spin-forming vendor, Spincraft, reported that similar variations in recrystallized microstructures have been observed during examination of multiple spin-forming trials of a different 2xxx series aluminum alloy. Hence, tighter chemical specification limits on impurity levels in Al 2219 plate may help ensure uniform, predictable microstructures. Finally, the tensile and fracture toughness properties were not affected by the microstructural variations noted.

single-piece

Two-Dimensional Nonlinear Finite Element Analysis of CMC Microstructures

A research program has been developed to quantify the effects of the microstructure of a woven ceramic matrix composite and its variability on the effective properties and response of the material. In order to characterize and quantify the variations in the microstructure of a five harness satin weave, chemical vapor infiltrated (CVI) SiC/SiC composite material, specimens were serially sectioned and polished to capture images that detailed the fiber tows, matrix, and porosity. Open source quantitative image analysis tools were then used to isolate the constituents, from which two dimensional finite element models were generated which approximated the actual specimen section geometry. A simplified elastic-plastic model, wherein all stress above yield is redistributed to lower stress regions, is used to approximate the progressive damage behavior for each of the composite constituents. Finite element analyses under in-plane tensile loading were performed to examine how the variability in the local microstructure affected the macroscopic stress-strain response of the material as well as the local initiation and progression of damage. The macroscopic stress-strain response appeared to be minimally affected by the variation in local microstructure, but the locations where damage initiated and propagated appeared to be linked to specific aspects of the local microstructure.

Mital, Subodh K.

Virtual texture analysis to understand microstructure effects on deformation twinning and detwinning behavior in BCC metals

Understanding and predicting deformation twinning contributions to plastic deformation in BCC metals has been a long-standing challenge due to the interplay with dislocation slip and non-Schmid effects that render an asymmetry under tension and compression. This paper uses molecular dynamics simulations to understand the effect of unloading and grain orientation on deformation twinning in a nanocrystalline Fe (nc-Fe) system as a model BCC metal. The nc-Fe system is loaded under uniaxial stress tension and compression to understand the effect of grain orientation (Schmid effects) on deformation twinning behavior and the tension/compression asymmetry (non-Schmid effects). A new virtual texture analysis “VirTex” tool is used to understand the role of grain orientation on the nucleation of twins and their contributions to the observed stress–strain response. For certain grain orientations, the twinnability is observed to be different in tension and compression. In addition, the flow stress accommodation from twins in certain grains is observed to be different in tension and compression and different from that for the grains. Subsequent unloading leads to detwinning in the deformed microstructures, where the extent of detwinning depends on the strain from which the system is unloaded and on the morphology of the twin. Lastly, the simulations are carried out to analyze the role of the Schmid factor on the twinnability and asymmetry in tension and compression.

Kannan, Aadhithyan [University of Connecticut, Sto

Solution of free-boundary problems using finite-element/Newton methods and locally refined grids - Application to analysis of solidification microstructure

A new method is presented for the solution of free-boundary problems using Lagrangian finite element approximations defined on locally refined grids. The formulation allows for direct transition from coarse to fine grids without introducing non-conforming basis functions. The calculation of elemental stiffness matrices and residual vectors are unaffected by changes in the refinement level, which are accounted for in the loading of elemental data to the global stiffness matrix and residual vector. This technique for local mesh refinement is combined with recently developed mapping methods and Newton's method to form an efficient algorithm for the solution of free-boundary problems, as demonstrated here by sample calculations of cellular interfacial microstructure during directional solidification of a binary alloy.

Tsiveriotis, K.

An evaluation of a coupled microstructural approach for the analysis of functionally graded composites via the finite-element method

A comparison is presented between the predictions of the finite-element analysis and a recently developed higher-order theory for functionally graded materials subjected to a thorough-thickness temperature gradient. In contrast to existing micromechanical theories that utilize classical (i.e., uncoupled) homogenization schemes to calculate micro-level and macro-level stress and displacement fields in materials with uniform or nonuniform fiber spacing (i.e., functionally graded materials), the new theory explicitly couples the microstructural details with the macrostructure of the composite. Previous thermo-elastic analysis has demonstrated that such coupling is necessary when: the temperature gradient is large with respect to the dimension of the reinforcement; the characteristic dimension of the reinforcement is large relative to the global dimensions of the composite and the number of reinforcing fibers or inclusions is small. In these circumstances, the standard micromechanical analyses based on the concept of the representative volume element used to determine average composite properties produce questionable results. The comparison between the predictions of the finite-element method and the higher-order theory presented herein establish the theory's accuracy in predicting thermal and stress fields within composites with a finite number of fibers in the thickness direction subjected to a thorough-thickness thermal gradient.

Pindera, Marek-Jerzy

Characterization of the microstructure of yttrium hydride under proton irradiation

High moderation per unit volume solid moderator materials like yttrium hydride (YH x ) are necessary for compact nuclear microreactors. However, the phase stability and hydrogen transport processes of YH x under high-temperature irradiation are largely unknown. Proton irradiation was conducted on YH x at 300 °C and 580 °C to 0.2 dpa using 1 MeV or 2 MeV protons in a high-vacuum environment. The hydrogen concentration was determined before and after irradiation using elastic recoil detection analysis, and microstructural evolution was examined via post-irradiation scanning transmission electron microscopy and Raman spectroscopy. Dislocation loops and cavities were observed in all conditions; their distribution was correlated with the bombarding proton energy and ion irradiation temperature. This work revealed that hydrogen retention is proportional to the formation of traps for hydrogen gas atoms and identified pathways for hydrogen release. The relative contributions of bulk or fast diffusion paths, such as grain boundaries, delamination boundaries, and stacking faults are discussed; the primary mechanisms of hydrogen loss are likely based on diffusion, ruling out artefacts of the experimental design. In conclusion, the study suggests proton irradiation may be a strong surrogate to study hydrogen transport in hydride moderator materials under irradiation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH

Multiscale Modeling for the Analysis for Grain-Scale Fracture Within Aluminum Microstructures

Multiscale modeling methods for the analysis of metallic microstructures are discussed. Both molecular dynamics and the finite element method are used to analyze crack propagation and stress distribution in a nanoscale aluminum bicrystal model subjected to hydrostatic loading. Quantitative similarity is observed between the results from the two very different analysis methods. A bilinear traction-displacement relationship that may be embedded into cohesive zone finite elements is extracted from the nanoscale molecular dynamics results.

Glaessgen, Edward H.

Comparative Analysis of Austenitized Steel Microstructures Due to Induction and Conventional Heating in High Magnetic Field

While magnetic field-assisted processing shows promise in improving alloys’ mechanical properties, insufficient descriptions of heating methods hinder development of tailored processing pathways. This study investigates how induction and conventional heating affect microstructures of near-eutectoid Fe–C steel with and without 9 T magnetic field. Conventionally heated samples in field showed more austenite grain growth compared to inductively heated counterparts. Annealing twin frequency increased under field, with twin density increases not fully explained by larger grain sizes.

Hurley, Megan [University of Florida, Gainesville]

Hydrogen induced fracture characteristics of single crystal nickel-based superalloys

A stereoscopic method for use with x ray energy dispersive spectroscopy of rough surfaces was adapted and applied to the fracture surfaces single crystals of PWA 1480E to permit rapid orientation determinations of small cleavage planes. The method uses a mathematical treatment of stereo pair photomicrographs to measure the angle between the electron beam and the surface normal. One reference crystal orientation corresponding to the electron beam direction (crystal growth direction) is required to perform this trace analysis. The microstructure of PWA 1480E was characterized before fracture analysis was performed. The fracture behavior of single crystals of the PWA 1480E nickel-based superalloy was studied. The hydrogen-induced fracture behavior of single crystals of the PWA 1480E nickel-based superalloy was also studied. In order to understand the temperature dependence of hydrogen-induced embrittlement, notched single crystals with three different crystal growth orientations near zone axes (100), (110), and (111) were tensile tested at 871 C (1600 F) in both helium and hydrogen atmospheres at 34 MPa. Results and conclusions are given.

Chen, Po-Shou