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DOE OSTI2019

Microstructural Characterization and Simulation of High Temperature Inelastic Deformation and Fracture of Al-Li 2070

A combined experimental and simulation investigation is carried out to characterize the high temperature deformation behavior of a recently developed Al-Li alloy, AA2070, over a temperature range including typical forging temperatures. Focus is placed on providing explanations for the temperature-dependent plastic and fracture behavior observed for this material using macroscale tensile tests, microscale imaging and analysis, and physics-based micromechanical modeling. It is shown that AA2070 experiences non-monotonic elongation to failure with a rise in temperature. Detailed fractography and microstructural analysis, including dynamic recrystallization analysis, provide insight into this interesting and practically useful behavior. In addition, a validated crystal plasticity model is called upon to explain the unique texture observed in the necked region of the ductile tensile specimen. The insights provided by this investigation will allow improved design of high temperature forming operations for AA2070 and similar alloys which can extend the application of third generation Al-Li alloys.

36 MATERIALS SCIENCE↗

NASA NTRS2012

Modeling of Damage Initiation and Progression in a SiC/SiC Woven Ceramic Matrix Composite

The goal of an ongoing project at NASA Glenn is to investigate the effects of the complex microstructure of a woven ceramic matrix composite and its variability on the effective properties and the durability of the material. Detailed analysis of these complex microstructures may provide clues for the material scientists who `design the material? or to structural analysts and designers who `design with the material? regarding damage initiation and damage propagation. A model material system, specifically a five-harness satin weave architecture CVI SiC/SiC composite composed of Sylramic-iBN fibers and a SiC matrix, has been analyzed. Specimens of the material were serially sectioned and polished to capture the detailed images of fiber tows, matrix and porosity. Open source analysis tools were used to isolate various constituents and finite elements models were then generated from simplified models of those images. Detailed finite element analyses were performed that examine how the variability in the local microstructure affected the macroscopic behavior as well as the local damage initiation and progression. Results indicate that the locations where damage initiated and propagated is linked to specific microstructural features.

Mital, Subodh K.↗

DOE OSTI2020

Microstructure reconstruction of battery polymer separators by fusing 2D and 3D image data for transport property analysis

A new approach to generate high-fidelity 3D microstructure reconstructions by leveraging resolution and sample volume characteristics from 2D and 3D microscopy methods is presented here. This approach is employed to model the microstructure of a highly orthotropic polypropylene separator used in lithium-ion batteries, which have challenging multi-scale features of fibrils (<100 nm) and lamellae (>100 nm) to resolve in 3D. Phase contrast nano X-ray computed tomographic data are used to reconstruct the lamellae phase, while 2D scanning electron microscopy data are used to characterize sub-100 nm microstructure features such as the thin fibrils that are beyond the effective resolution of X-ray computed tomography. Fibril geometries are reconstructed stochastically based on the 2D higher resolution data, and integrated with the lamellae geometries in 3D space. Transport property analyses are performed to investigate the bias of microstructure models without considering the fibrils. A sensitivity study is also conducted to facilitate understanding of the relationship between microstructure characteristics and transport properties.

25 ENERGY STORAGE↗

DOE OSTI2022

Simulation-guided analysis of resonant soft X-ray scattering for determining the microstructure of triblock copolymers

Resonant soft X-ray scattering (RSoXS) probes structure with chemical sensitivity that is useful for determining the morphology of multiblock copolymers. However, the hyperspectral scattering data produced by this technique can be challenging to interpret. Here, in this study, we use computational scattering simulations to extract the microstructure of a model triblock copolymer from the energy-dependent scattering from RSoXS. An ABC triblock terpolymer formed from poly(4-methylcaprolactone) (P4MCL), poly(2,2,2-trifluoroethylacrylate) (PTFEA), and poly (dodecylacrylate) (PDDA), P4MCL-block-PTFEA-block-PDDA, was synthesized as the model triblock system. Through quantitative evaluation of simulated scattering data from a physics-informed set of candidate structure models against experimental RSoXS data, we find the best agreement with hexagonally packed core–shell cylinders. This result is also consistent with electron-density reconstruction from hard X-ray scattering data evaluated against electron-density maps generated with the same model set. These results demonstrate the utility of simulation-guided scattering analysis to study complex microstructures that are challenging to image by microscopy.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2017

Effect of stress evolution on microstructural behavior in U-Mo/Al dispersion fuel [Effect of stress on microstructural evolution in U-Mo/Al dispersion fuel]

U-Mo/Al dispersion fuel irradiated to high burnup at high power (high fission rate) exhibited microstructural changes such as deformation of the fuel particles, pore growth, and rupture of the Al matrix. The driving force for these microstructural changes was meat swelling caused by a combination of fuel particle swelling and interaction layer growth. Five miniplates with well-recorded fabrication data and irradiation conditions were selected, and their PIE data was analyzed. ABAQUS finite element analysis (FEA) was utilized to simulate the microstructural evolution of the plates. Using the simulation results shear stress, effective stress and hydrostatic stress exerted on both the fuel particles and the Al matrix were determined. The effects of fabrication and irradiation variables on stress-induced microstructural evolutions, such as pore growth in the interaction layers and Al matrix rupture, were investigated. The observed microstructural changes were consistent with the calculated stress distribution in the meat.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2018

X-ray computed tomography of microstructure evolution during matrix impregnation and curing in unidirectional fiber beds

Microstructural evolution during axial impregnation and subsequent curing of a preceramic polymer in unidirectional ceramic fiber beds is studied using X-ray computed tomography. The principal goal is to identify connections between void locations, void sizes, local fiber bed porosity, fiber movement, and impregnation conditions. The degree of saturation after impregnation is found to increase with instantaneous capillary number. But, because of the need to create pathways for gas escape during curing, fiber beds with high saturation after impregnation show the largest reductions in saturation during curing. Notwithstanding, saturation after curing increases with instantaneous capillary number. Voids tend to form in the largest channels between fibers, where the local fiber bed porosity is high, during both impregnation and curing. Here, void formation is typically accompanied by fiber movement that increases both the local fiber bed porosity near voids and the overall non-uniformity in the fiber bed, as measured by local porosity entropy.

(A - Material) fibers↗

DOE OSTI2013

Retained austenite thermal stability in a nanostructured bainitic steel

The unique microstructure of nanostructured bainite consists of very slender bainitic ferrite plates and high carbon retained austenite films. As a consequence, the reported properties are opening a wide range of different commercial uses. However, bainitic transformation follows the T{sub 0} criteria, i.e. the incomplete reaction phenomena, which means that the microstructure is not thermodynamically stable because the bainitic transformation stops well before austenite reaches an equilibrium carbon level. This article aims to study the different microstructural changes taking place when nanostructured bainite is destabilized by austempering for times well in excess of that strictly necessary to end the transformation. Results indicate that while bainitic ferrite seems unaware of the extended heat treatment, retained austenite exhibits a more receptive behavior to it. - Highlights: • Nanostructured bainitic steel is not thermodynamically stable. • Extensive austempering in these microstructures has not been reported before. • Precipitation of cementite particles is unavoidable at longer austempering times. • TEM, FEG-SEM and XRD analysis were used for microstructural characterization.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Effect of TiO{sub 2} additives to the sintering of Y{sub 2}O{sub 3}

The effect of sintering additive on the microstructure development of yttrium oxide was investigated. Different combinations of yttrium oxide with TiO{sub 2} were used as x-ray diffraction, differential thermal analysis (DTA) were sintering additive. The investigated and microstructure of resulting compacts were characterized by, using scanning electron microscopy, porosity and sintering density for all compacting samples sintered at different sintering temperature under static air.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Quantitative description of microstructure defects in hexagonal boron nitrides using X-ray diffraction analysis

A routine for simultaneous quantification of turbostratic disorder, amount of puckering and the dislocation and stacking fault density in hexagonal materials was proposed and tested on boron nitride powder samples that were synthesised using different methods. The routine allows the individual microstructure defects to be recognised according to their effect on the anisotropy of the X-ray diffraction line broadening. For quantification of the microstructure defects, the total line broadening is regarded as a linear combination of the contributions from the particular defects. The total line broadening is obtained from the line profile fitting. As testing material, graphitic boron nitride (h-BN) was employed in the form of hot-isostatically pressed h-BN, pyrolytic h-BN or a h-BN, which was chemically vapour deposited at a low temperature. The kind of the dominant microstructure defects determined from the broadening of the X-ray diffraction lines was verified by high resolution transmission electron microscopy. Their amount was attempted to be verified by alternative methods. - Highlights: • Reliable method for quantification of microstructure defects in BN was suggested. • The method is based on the analysis of anisotropic XRD line broadening. • This XRD line broadening is unique and characteristic of the respective defect. • Thus, the quantification of coexistent microstructure defects is possible. • The method was tested on hexagonal BN, which was produced by different techniques.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Effect of powder layer thickness on the microstructural development of additively manufactured SS316

By Increasing the powder layer thickness we could increase material deposition rates and reduce build times during laser powder bed fusion (LPBF). However, increasing the powder layer thickness could also negatively affect the local melting and subsequent microstructure of the printed material. This study systematically investigated, for the first time, the defect evolution and microstructural changes of LPBF stainless steel 316 (SS316) processed by using various powder layer thicknesses of 40, 80, and 120 μm while also varying the laser dwell time for the pulsed laser. Through image analysis, the pore density was found to increase with increasing powder layer thickness, particularly when the dwell time was too high or too low. The maximum achievable density (>99%) was found over a wide processing window when using the smallest powder layer thickness of 40 μm between dwell times of 60 and 100 μs. Increasing the powder layer thicknesses to 80 and 120 μm resulted in maximum densities of 98.7 and 96.8%, respectively, but the window for acceptable laser dwell times that could achieve these densities narrowed considerably. A microstructural analysis of the melt pools was performed to measure the melt pool depths and widths, both of which increased with increasing dwell time. However, increasing the powder layer thickness did not affect the melt pool depth and only minorly affected the width. A sub-grain cellular structure distinguished the melt pool boundaries. The cell size increased with increasing dwell time and decreasing powder layer thickness. Moreover, the cell size was used to calculate a cooling rate that had a magnitude of 10 7 K/s and increased with increasing powder layer thickness.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Assessment of MARMOT Grain Growth Model

This report assesses the MARMOT grain growth model by comparing modeling predictions with experimental results from thermal annealing. The purpose here is threefold: (1) to demonstrate the validation approach of using thermal annealing experiments with non-destructive characterization, (2) to test the reconstruction capability and computation efficiency in MOOSE, and (3) to validate the grain growth model and the associated parameters that are implemented in MARMOT for UO 2 . To assure a rigorous comparison, the 2D and 3D initial experimental microstructures of UO 2 samples were characterized using non-destructive Synchrotron x-ray. The same samples were then annealed at 2273K for grain growth, and their initial microstructures were used as initial conditions for simulated annealing at the same temperature using MARMOT. After annealing, the final experimental microstructures were characterized again to compare with the results from simulations. So far, comparison between modeling and experiments has been done for 2D microstructures, and 3D comparison is underway. The preliminary results demonstrated the usefulness of the non-destructive characterization method for MARMOT grain growth model validation. A detailed analysis of the 3D microstructures is in progress to fully validate the current model in MARMOT.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2015

Study of microstructure and silicon segregation in cast iron using color etching and electron microprobe analysis

An investigation on silicon segregation of lamellar, compacted and nodular graphite iron was carried out by applying a selective, immersion color etching and a modified electron microprobe to study the microstructure. The color etched micrographs of the investigated cast irons by revealing the austenite phase have provided data about the chronology and mechanism of microstructure formation. Moreover, electron microprobe has provided two dimensional segregation maps of silicon. A good agreement was found between the segregation profile of silicon in the color etched microstructure and the silicon maps achieved by electron microprobe analysis. However, quantitative silicon investigation was found to be more accurate than color etching results to study the size of the eutectic colonies. - Highlights: • Sensitivity of a color etchant to silicon segregation is quantitatively demonstrated. • Si segregation measurement by EMPA approved the results achieved by color etching. • Color etched micrographs provided data about solidification mechanism in cast irons. • Austenite grain boundaries were identified by measuring the local Si concentration.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Microstructure, strengthening mechanisms and hot deformation behavior of an oxide-dispersion strengthened UFG Al6063 alloy

An ultrafine-grained Al6063/Al{sub 2}O{sub 3} (0.8 vol.%, 25 nm) nanocomposite was prepared via powder metallurgy route through reactive mechanical alloying and hot powder extrusion. Scanning electron microcopy, transmission electron microscopy, and back scattered electron diffraction analysis showed that the grain structure of the nanocomposite is trimodal and composed of nano-size grains (< 0.1 {mu}m), ultrafine grains (0.1-1 {mu}m), and micron-size grains (> 1 {mu}m) with random orientations. Evaluation of the mechanical properties of the nanocomposite based on the strengthening-mechanism models revealed that the yield strength of the ultrafine-grained nanocomposite is mainly controlled by the high-angle grain boundaries rather than nanometric alumina particles. Hot deformation behavior of the material at different temperatures and strain rates was studied by compression test and compared to coarse-grained Al6063 alloy. The activation energy of the hot deformation process for the nanocomposite was determined to be 291 kJ mol{sup -1}, which is about 64% higher than that of the coarse-grained alloy. Detailed microstructural analysis revealed that dynamic recrystallization is responsible for the observed deformation softening in the ultrafine-grained nanocomposite. - Highlights: Black-Right-Pointing-Pointer The strengthening mechanisms of Al6063/Al{sub 2}O{sub 3} nanocomposite were evaluated. Black-Right-Pointing-Pointer Hot deformation behavior of the nanocomposite was studied. Black-Right-Pointing-Pointer The hot deformation activation energy was determined using consecutive models. Black-Right-Pointing-Pointer The restoration mechanisms and microstructural changes are presented.

36 MATERIALS SCIENCE↗

NASA NTRSDate not supplied

Microstructural Constraints on the Formation of Diamond in Ureilites, the Case from the Kenna Meteorite

The origin of diamonds in ureilitic meteorites, a major family of ultramafic achondrites, has long been debated, with various formation mechanisms inferred, including: 1) shock conversion of preexisting graphite due to a hypervelocity impact on the ureilite parent body; 2) vapor deposition during condensation of the solar nebula; or 3) static transformation in the mantle of a large planetesimal (>1000 km in diameter). The Kenna ureilite is a 10.9 kg stone that was found in Kansas in 1972 and is dominantly composed of olivine and pigeonite (68% and 22% modal abundance, respectively), together with minor metal and carbon-rich regions. Within the carbon-rich domains researchers have identified microdiamonds up to ~10 µm in size. Due to the proximity of the extremely hard microdiamonds with soft graphite and moderately hard silicates, achieving an appropriately flat surface for electron backscatter diffraction (EBSD) analysis has proved challenging. We have, therefore, employed a Hitachi ArBlade 5000 broad beam Ar ion milling system to prepare a sample with an adequate surface uniformity. The ion milling dramatically improved indexing of the EBSD patterns and facilitated high-resolution microstructural analysis of the carbon-rich domains. The carbon-bearing regions occur as tabular domains between polygonal olivine and pigeonite, and are composed of aggregates of micrometer-scale diamond with intermediate graphite, oxides and metal grains. Within the microdiamonds, {111} twins are abundant, many of which form ragged lamellae consistent with mechanical twinning. The microdiamond assemblages appear to pseudomorph tabular graphite habits, which together with the abundant deformation twins, supports a shock transformation mechanism for microdiamond formation within the Kenna meteorite. To compliment the EBSD microstructural analyses, coordinated laser Raman, focused ion beam/transmission electron microscopy imaging and diffraction data, and NanoSIMS N and C tomographic isotopic imaging will be collected. These data will provide further constraints on the formation of diamonds within ureilites.

Timmons M Erickson↗

DOE OSTI2019

Characterization of Creep-Fatigue Crack Growth in Alloy 709 and Prediction of Service Lives in Nuclear Reactor Components (Final Report)

This final report summarizes the activities and results that were obtained by the research team working on the project “Characterization of Creep-Fatigue Crack Growth in Alloy 709 and Prediction of Service Lives in Nuclear Reactor Components”, DOE-NEUP Project 15-8623. This project was mainly concerned with the creep-fatigue crack growth characterization of austenitic stainless-steel Fe-20Cr-25Ni (Alloy 709). For this purpose, an array of experimental and computational activities was performed. The main goal of these activities was to describe and predict the crack growth behavior in Alloy 709 under different conditions of applied loading and temperature. Alloy 709 specimens were tested to describe both the uniaxial creep behavior and creep-fatigue crack growth rates at temperatures between 550°C and 700°C. Microstructure and fracture surface analysis was performed using several experimental techniques, and the defining features of crack growth propagation were identified and described. Thermodynamic and diffusion simulations were performed to understand the microstructure evolution of Alloy 709 at elevated temperatures, and to establish an aging schedule relevant for in-service conditions over extended periods. Experimental testing was performed on both as-received and aged Alloy 709 specimens. Two computational methods were developed to predict crack growth rates and remaining lives in specimens loaded under either fatigue of creep-fatigue. The first computational technique was the finite element method, while the second was strip-yield modeling. Both methods relied on the prediction of crack growth rates using the concept of plasticity-induced crack closure. Crack-tip opening loads were computed and used to perform crack growth rate predictions. The computational predictions matched well with the experimental results. The strip-yield model was shown to be an excellent predictive tool not only for crack growth in austenitic SS Alloy 709, but also in 316 SS, martensitic Cr-Mo steels, Ni-based alloys and Al-based alloys. The main conclusion of this study is that Alloy 709 exhibits excellent creep crack growth resistance at temperatures between 550°C and 700°C. In fact, the crack growth resistance of this alloy appears to be higher than that of 316 SS in similar testing conditions. Moreover, when creep loading with hold (dwell) times of 60s or 600s were intercalated every fatigue cycle, the crack growth rates did not change significantly. The conclusion is that the tests performed revealed that the crack growth is insignificant during the creep portion of a loading cycle, as compared with the crack growth during the fatigue portion of the cycle. In general, Alloy 709 shows excellent resistance to creep deformations and creep crack growth up to 700°C.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2021

Influence of geometry on columnar to equiaxed transition during electron beam powder bed fusion of IN718

Correlation between spot-melt scan parameters (linear spot-density aka areal energy density), build geometry, and solidification microstructure evolution (columnar vs equiaxed) in a powder bed fusion technology is investigated. It is shown that to maintain the equiaxed solidification microstructure evolution in electron beam powder bed additive manufacturing (AM), the areal energy density per layer needs to be scaled with respect to the 2D cross-sectional area of the layer being melted. Samples with two different cross-sectional areas (40 × 40 mm and 20 × 20 mm) have been fabricated with varying areal energy densities. For a given square cross-section (20 × 20 mm), increasing the areal energy density (4.8 MJ/sq.m to 14.7 MJ/sq.m) transitioned the solidification microstructure from columnar to equiaxed. The observed microstructure data (Electron Back Scattered Diffraction - EBSD) is quantified by calculating the principal component (PC) score using a spatial statistics methodology. The sample with equiaxed grains is found to have a low PC score while the sample with columnar grain had a high PC score. A semi-analytical model is used to simulate the heat transfer and the local solidification conditions as a function of processing parameters (linear spot-density). The result from the heat transfer model is correlated with previously quantified microstructure data. Space-Time analysis of the melt pattern is done and correlated with the observed microstructure. In addition, from the findings, appropriate parameters have been used to additively manufacture a turbine blade with site-specific or hybrid solidification microstructure (traditional fabrication possible via a patented method of localized cold working and heat treatment).

36 MATERIALS SCIENCE↗

NASA NTRS2003

Characterization of Al-Cu-Mg-Ag Alloy RX226-T8 Plate

Aluminum-copper-magnesium-silver (Al-Cu-Mg-Ag) alloys that were developed for thermal stability also offer attractive ambient temperature strength-toughness combinations, and therefore, can be considered for a broad range of airframe structural applications. The current study evaluated Al-Cu-Mg-Ag alloy RX226-T8 in plate gages and compared performance with sheet gage alloys of similar composition. Uniaxial tensile properties, plane strain initiation fracture toughness, and plane stress tearing resistance of RX226-T8 were examined at ambient temperature as a function of orientation and thickness location in the plate. Properties were measured near the surface and at the mid-plane of the plate. Tensile strengths were essentially isotropic, with variations in yield and ultimate tensile strengths of less than 2% as a function of orientation and through-thickness location. However, ductility varied by more than 15% with orientation. Fracture toughness was generally higher at the mid-plane and greater for the L-T orientation, although the differences were small near the surface of the plate. Metallurgical analysis indicated that the microstructure was primarily recrystallized with weak texture and was uniform through the plate with the exception of a fine-grained layer near the surface of the plate. Scanning electron microscope analysis revealed Al-Cu-Mg second phase particles which varied in composition and were primarily located on grain boundaries parallel to the rolling direction. Fractography of toughness specimens for both plate locations and orientations revealed that fracture occurred predominantly by transgranular microvoid coalescence. Introduction High-strength, low-density Al-Cu-Mg-Ag alloys were initially developed to replace conventional 2000 (Al-Cu-Mg) and 7000 (Al-Zn-Cu-Mg) series aluminum alloys for aircraft structural applications [1]. During the High Speed Civil Transport (HSCT) program, improvements in thermal stability were demonstrated for candidate aircraft wing and fuselage skin materials through the addition of silver to Al-Cu-Mg alloys based on Al 2519 chemistry [2]. Thermal stability of the resulting Al-Cu-Mg-Ag alloys, C415-T8 and C416-T8, was due to co-precipitation of the thermally stable . (AlCu) and ' (Al2Cu) strengthening phases [1-4]. The strength and toughness behavior was investigated for these alloys produced as 0.090-inch thick rolled sheet in the T8 condition and after various thermal exposures. The mechanical properties were shown to be competitive with conventional aircraft alloys, 2519-T8 and 2618-T8 [2]. During the Integral Airframe Structure (IAS) program, advanced aluminum alloys were examined for use in an integrally stiffened airframe structure where the skin and stiffeners would be machined from plate and extruded frames would be mechanically attached (see Figure 1) [5]. Advantages of integrally stiffened structure include reduced part count, and reduced assembly times compared to conventional built-up airframe structure. The near-surface properties of a thick plate are of significance for a machined integrally stiffened airframe structure since this represents the skin location. Properties measured at the mid-plane of the plate are more representative of the stiffener web. RX226 was developed to exploit strength-toughness improvements and thermal stability benefits of Al-Cu-Mg-Ag alloys in plate gages. This study evaluated the microstructure and properties of three gages of plate produced in the T8 condition.

Lach, Cynthia L.↗

DOE OSTI2016

Analysis of irradiated U-7wt%Mo dispersion fuel microstructures using automated image processing

The High Performance Research Reactor Fuel Development (HPPRFD) program is responsible for developing low enriched uranium (LEU) fuel substitutes for high performance reactors fueled with highly enriched uranium (HEU) that have not yet been converted to LEU. The uranium-molybdenum (U-Mo) fuel system was selected for this effort. In this study, fission gas pore segmentation was performed on U-7wt%Mo dispersion fuel samples at three separate fission densities using an automated image processing interface developed in MATLAB. Pore size distributions were attained that showed both expected and unexpected fission gas behavior. In general, it proved challenging to identify any dominant trends when comparing fission bubble data across samples from different fuel plates due to varying compositions and fabrication techniques. Here, the results exhibited fair agreement with the fission density vs. porosity correlation developed by the Russian reactor conversion program.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗