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At least 631 records · Page 35

InSitu SEM Investigation of Microstructural Damage Evolution and Strain Relaxation in a Melt Infiltrated SiC/SiC Composite

With CMC components poised to complete flight certification in turbine engines on commercial aircraft within the near future, there are many efforts within the aerospace community to model the mechanical and environmental degradation of CMCs. Direct observations of damage evolution are needed to support these modeling efforts and provide quantitative measures of damage parameters used in the various models. This study was performed to characterize the damage evolution during tensile loading of a melt infiltrated (MI) silicon carbide reinforced silicon carbide (SiC/SiC) composite. A SiC/SiC tensile coupon was loaded to a maximum global stress of 30 ksi in a tensile fixture within an SEM while observations were made at 5 ksi increments. Both traditional image analysis and DIC (digital image correlation) were used to quantify damage evolution. With the DIC analysis, microscale damage was observed at the fiber-matrix interfaces at stresses as low as 5 ksi. First matrix cracking took place between 20 and 25 ksi, accompanied by an observable relaxation in strain near matrix cracks. Matrix crack opening measurements at the maximum load ranged from 200 nm to 1.5 m. Crack opening along the fiber-matrix interface was also characterized as a function of load and angular position relative to the loading axis. This characterization was funded by NASA GRC and was performed to support NASA GRC modeling of SiC/SiC environmental degradation

testing↗

Microstructure and CPO evolution of dynamically recrystallized olivine during complex deformation conditions: a full-field numerical modeling approach

The rheological properties of mantle rocks are strongly dependent on their crystallographic preferred orientation (CPO). Olivine CPO, defined by the orientation of seismically fast [100] axes parallel to flow direction, is also thought to be a dominant contributor to seismic anisotropy in the Earth's upper mantle. However, the amount of deformation needed to overprint a new CPO on a pre-existing fabric and the impact of the inherited CPOs on the transient microstructure evolution, remain unknown. This study employs a full-field numerical approach (VPFFT-ELLE) to explore the dynamic recrystallization and microstructural evolution of olivine polycrystalline aggregates under complex deformation conditions. We test four combinations of successive pure shear and simple shear boundary conditions. Findings indicate that inherited CPOs influence subsequent deformation in a manner dependent on the kinematic relationship between successive stages. In all cases, a minor strain increment (ε ∼0.3–0.6) is sufficient to erase the previous microstructure and CPO. However, when deformation conditions change dramatically (e.g., stretching direction changes orthogonally), the intensity of the new CPO developed is significantly lower and strain distribution are specially altered. During a transient strain stage, pre-existing microstructures undergo extensive reworking, especially when deformation conditions are changed dramatically, such as switching from simple shear to a pure shear condition with a parallel shortening direction relative to the stretching direction. We estimate the significance of these results in interpreting observations of seismic velocity anisotropy, concluding that P-wave seismic anisotropy is significantly and positively correlated with the evolution of olivine CPO with deformation history. This research underscores the transient nature of microstructural rearrangement in olivine aggregates and the necessity for caution in interpreting seismic anisotropy in regions with complex deformation histories, as inherited CPOs can influence current fabric development and induce deviation to the present deformation conditions.

36 MATERIALS SCIENCE↗

Effect of alloying elements on defect evolution in Ni-20X binary alloys

The effect of alloying elements on radiation-induced microstructural evolution in Ni and Ni-20X (X = Fe, Cr, Mn and Pd) binary alloys was investigated using ion irradiation and cross-sectional transmission electron microscopy. The three-dimensional migration mode is identified to be the dominating migration mechanism for interstitial clusters in these binary alloys, contrary to the one-dimensional mode that dominates in the well-studied dilute alloys. The results reveal that: (1) the average size of defect clusters decreases as the solute atomic volume size factor increases. Smaller void size in Ni-20Cr is attributed to faster vacancy mobility in the near surface region, and weaker vacancy binding energy beyond the irradiation peak than Ni-20Fe. The smaller voids observed in Ni-20Mn and Ni-20Pd beyond the damage peak are due to the stronger Mn/Pd-vacancy binding effect of largely oversized solute atoms. (2) Oversized solutes can act as strong trapping sites for interstitials. The larger the solute atomic volume factor, the stronger the trapping force. This leads to a more significantly sluggish interstitial migration and smaller dislocation loop size. The average dislocation loop size in Ni-20Fe was four times larger than Ni-20Pd (atomic volume factor being 10.6% and 41.3%) but an order of magnitude lower in density. The smaller dislocation loop size in Ni-20Cr is attributed to stronger interstitial binding of Cr-Ni. In conclusion, overall, the alloying effect on defects is more significant in concentrated binary alloys than in dilute binary alloys, due to the concentration difference of alloying atoms and the interstitial dominant migration mechanisms in the main irradiated region.

36 MATERIALS SCIENCE↗

Process-Structure Linkages Using a Data Science Approach: Application to Simulated Additive Manufacturing Data

A novel data science workflow is developed and demonstrated to extract process-structure linkages (i.e., reduced-order model) for microstructure evolution problems when the final microstructure depends on (simulation or experimental) processing parameters. Our workflow consists of four main steps: data pre-processing, microstructure quantification, dimensionality reduction, and extraction/validation of process-structure linkages. These methods that can be employed within each step vary based on the type and amount of available data. In this paper, this data-driven workflow is applied to a set of synthetic additive manufacturing microstructures obtained using the Potts-kinetic Monte Carlo (kMC) approach. Additive manufacturing techniques inherently produce complex microstructures that can vary significantly with processing conditions. Using the developed workflow, a low-dimensional data-driven model was established to correlate process parameters with the predicted final microstructure. In addition, the modular workflows developed and presented in this work facilitate easy dissemination and curation by the broader community.

36 MATERIALS SCIENCE↗

TEM investigations on lath martensite substructure in quenched Fe-0.2C alloys

Highlights: • Twin can be lath martensite substructure in low-carbon steels. • Detwinning behavior occurs in an auto-tempering process during quenching. • Detwinning may result in the formation of twinned laths. • Detwinning may result in the laths with dislocation-like contrast as substructure. - Abstract: Lath martensite in low-carbon steels is the main microstructural feature in the quenched state, and dislocations have been generally recognized as the substructure of lath martensite. However, the effects of quenching conditions on the quenched substructure have not yet been fully understood. In the present work, a Fe-0.2C (wt%) alloy was selected for detailed investigations on the microstructural evolution at various austenitizing temperatures. Microstructural characterization was carried out by using a conventional transmission electron microscope (TEM). The substructure of lath martensite was found to vary with austenitizing temperature. In the 1200 °C-water-quenched (WQ) samples, twinned laths (two specific variants having a {112}<111>-type twin relationship) and a twinned region (laths with the twin structure as their substructure) can be observed. Almost all lath martensite with a high density of fine twins as its substructure can be obtained in the 1300 °C-WQ samples. The twins gradually disappear or detwinning-occurs during TEM observations carried out with in situ heating. A further increase in temperature results in the formation of twinned laths and then lath with dislocation-like contrasts or lines appears as the substructure. These results suggested that a completely twin structure can be the initial substructure of lath martensite, and lath with dislocation-like contrasts or lines as its substructure is most likely the auto-tempering result of twinning.

36 MATERIALS SCIENCE↗

Microstructure and microhardness of wire-based laser metal deposited AA5087 using an Ytterbium fibre laser

Highlights: • Heat conduction strongly affects the microstructural development. • Heat conduction conditions changes with increasing part height. • Anisotropic microstructural development affects the microhardness of the part. • Anisotropic mechanical properties along the structure are assumed. - Abstract: Wire-based additive manufacturing has been increasingly investigated in recent years. Although it is possible nowadays to manufacture structures that are free from inner defects such as porosity and cracks using wire and arc additive manufacturing, there is still a lack of knowledge regarding wire-based laser metal deposition of aluminium and its alloys. In order to be able to produce locally tailored part properties, it is necessary to understand the process parameter to material property relationships. Using laser energy sources, it becomes possible to analyse in detail the heat input and to observe occurring microstructural evolutions. This work includes a microstructural and mechanical characterization of an AA5087 wall structure. Detailed analyses of the chemical composition, texture, and microhardness of the structure have been performed. The microstructure contains different grain orientations as well as grain shapes and sizes along the structure, resulting in locally different material properties. The results have been analysed and discussed in reference to fundamental theories such as the Hall–Petch and Orowan mechanisms.

36 MATERIALS SCIENCE↗

On the exceptionally high ductility of Mg–2Zn-0.3Ca-0.2Ce-0.1Mn alloy

A newly developed Mg–2Zn-0.3Ca-0.2Ce-0.1Mn (in weight %, ZXEM2000) wrought alloy exhibits an exceptionally high tensile ductility (29% ± 1.4% tensile elongation) along the rolling direction at room temperature. In this work, we investigated the fundamental plastic deformation mechanisms that can contribute to the high ductility of ZXEM2000. Scanning electron microscopy and transmission electron microscopy were carried out at selected strain levels to characterize the microstructural evolution. Compared with the deformed microstructures from the hot-rolled pure Mg and Mg–3Al–1Zn alloy at similar conditions, our results revealed that the high ductility of ZXEM2000 could be attributed to four key factors: weaker texture, fine grain size, reduced twinning, and increased cross-slip frequency of < c +a > dislocation. Furthermore, these direct observations offer a key insight into improving ductility of magnesium alloys for future alloy design and development.

36 MATERIALS SCIENCE↗

Microstructural characterization of dendritic evolution using two-point statistics

Characterizing large four-dimensional materials datasets is difficult due to the presence of complex mi- crostructures and time-varying length scales. We showcase the use of two-point statistics as an efficient and un-biased way of extracting materials parameters from an Al-Cu alloy during solidification. The evo- lution of dendrite primary arm thickness, average secondary arm spacing, and average tip-to-tip spacing were tracked using two-point Pearson auto-correlations of scaled mean curvatures. Insights into compet- itive side-branching are also reported. We show both visually and quantitatively that most length scales change rapidly during early stages of dendritic growth, but slow as diffusion fields of dendrites overlap.

Aluminum alloys↗

Microstructure and texture evolution of friction stir lap welded dissimilar multi-aluminum stack

Here this work investigates the microstructural evolution of a dissimilar multiple-aluminum alloy stack (AA7055, AA7055, AA6022) produced by friction stir lap welding (FSLW). A through-thickness analyses of grain orientation map, grain size and distribution, strain distribution, and texture evolution by electron backscattered diffraction-based characterization technique were performed. Two different welding parameters (combination of tool rotation and traverse speed) were used to study the effects of the welding parameters on these microstructural characteristics. The study shows that higher welding speed and higher rotation speed of the FSLW tool yield finer grains. FSLW resulted in shear texture formation in the weld regions due to high welding speeds. This texture development in the nugget zone is consistent with shear deformation, and (111) pole figures show ideal shear texture components. The Stir Zone (SZ) exhibits shear texture (A/A ̅ and B/B ̅ components), consistent with other shear-assisted processes. Recrystallization mechanisms observed are CDRX in SZ and DDRX in TMAZ (Thermo-Mechanically Affected Zone). Interface analysis reveals the presence of oxide layers between different aluminum sheets, affecting joint mechanical performance. The mechanical property of the lap welded joints was presented in terms of microhardness distribution across the weld cross section. Slightly higher hardness in higher speed welding setup was observed throughout the SZ and AA6022 layer, indicating greater grain refinement and uniform grain structure distribution.

36 MATERIALS SCIENCE↗

Microstructural and compositional evolutions in $γ$-LiAlO 2 pellets during ion irradiation at an elevated temperature

This study reports on the microstructural, phasic and compositional evolutions of γ-LiAlO 2 during ion irradiation. Polycrystalline γ-LiAlO 2 pellets were irradiated sequentially with He + and D 2 + ions to the same combined fluences of up to 3 × 10 17 (He + +D + )/cm 2 at 773 K. The irradiated pellets were characterized using scanning transmission electron microscopy and atom probe tomography. Surface amorphization likely due to radiolysis and planar defects as a possible precursor for formation of precipitates are created at 5 × 10 16 (He + +D + )/cm 2 , followed by the formation of nano-sized precipitates and fractures at higher doses. Spinel-like precipitates of non-stoichiometric LiAl 5 O 8 and gas-filled cavities are observed to grow with increasing dose. Faceted precipitates and rounded cavities appear at 2 × 10 17 (He + +D + )/cm 2 . With further increasing ion fluence to 3 × 10 17 (He + +D + )/cm 2 , amorphization of the precipitates takes place and micron-sized fractures appear. Surface exfoliation could occur at an extremely high ion fluence. There are compositional changes in the γ-LiAlO 2 pellets during the microstructural evolution. In the precipitate and amorphized regions, Li concentrations decrease to ~7 and 3.7 at.% from 25 at.% in γ-LiAlO 2 , respectively. This study reveals a full-cycle microstructural evolution with corresponding compositional changes in γ-LiAlO 2 pellets during ion irradiation at 773 K. In conclusion, the data could help model, assess, and predict the material performance during neutron irradiation in reactors.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

Microstructure and hardness evolution induced by annealing of ion irradiated LiTaO 3

We report the evolution of the microstructure and mechanical properties of low-energy heavy-ion-irradiated LiTaO 3 crystals annealed at various temperatures was investigated by transmission electron microscopy (TEM) observations and nanoindentation tests to extend the applications of irradiated LiTaO 3 crystals. Before annealing, randomly distributed voids formed in an approximately 200 nm thick region at the end of the ion irradiation range, which was attributed to preferential absorption of interstitials by the amorphous-crystalline interface. After annealing, a new directional diffusion path of defects was identified, resulting in a void string. Furthermore, void string diffusion to the free surface was also found during the annealing temperature increase process, which offers a potential application in designing custom sized-thickness exfoliation at the nanoscale. Meanwhile, two competing processes were identified during the annealing process: epitaxial recrystallization from the amorphous-crystalline interface and grain nucleation process in the amorphous region, which formed phases different from the matrix crystal structure, resulting in an interaction between them. Furthermore, the hardness of irradiated samples was also found to be affected by the annealing process; in particular, a hardness decrease induced by the interstitial Fe ions in the recrystallized region was also confirmed, which can improve the processability of samples for further application.

36 MATERIALS SCIENCE↗

Development of Nano-Modified Concrete for Next Generation of Storage Systems

The goal of the research was to develop a superior concrete for the long-term storage of used nuclear fuel by engineering concrete at the nanoscale through the incorporation of nano-sized and nano-structured particles based on enhanced reactivity (not fiber reinforcement). The specific objectives were to determine for nano-modified concrete: 1. The effects of environmental weathering (i.e., wet/dry and ingress of reactive species such as chloride and sulfate from the marine environment or other sources) and exposure to radiation and thermal environments on the structural stability and microstructural evolution of the material; 2. How microstructural and morphological changes from environmental weathering and thermal and radiation damage affect the long-term, macroscale performance of the material; and, 3. Identify formulation envelopes for nanoparticle content and combinations to achieve superior concrete criteria for dry storage systems by integrating and extending existing predictive modeling approaches that couple reactive transport and thermo- chemo- and radiation induced damage. The major findings of this work are summarized as follows. The results are being processed and compiled in manuscripts for peer-reviewed publication. Due to the late access to the gamma irradiation facility, material characterization is continuing. Dispersion/agglomeration of nanoparticles in cement pastes. The dispersion/agglomeration of nanoparticles (NPs) of SiO 2 , TiO 2 , Al 2 O 3 , Fe 2 O 3 , and clay (bentonite and halloysite) in water, with and without polycarboxylate-based high range water reducer (P-HRWR), and in the environment of hydrating cement have been investigated. The intrinsic particle characteristics, surface charge, pH, monovalent and divalent ion concentrations in solution, and modes of interaction of the NPs with P-HRWR influenced the NP behavior in solution.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

FFTF HT9 Cladding Microstructure Characterization

The sodium-cooled fast reactor (SFR) is a promising candidate for next generation nuclear reactors, operating at extreme conditions which include high temperatures (>500?C core outlet temperature) and significant neutron damage. High-Cr martensitic HT9 steel is an excellent candidate for SFR cladding and duct material due to its compatibility with liquid sodium, good thermal conductivity, resistance to void swelling, and strong creep rupture strength [1-4].However, the harsh in-core environment of SFRs can cause complex microstructural changes and mechanical property degradation in HT-9. Ensuring the safe use of HT9 cladding for metallic fuel requires both a thorough understanding of its mechanical response to microstructure evolution as well as reliable microstructure-sensitive modeling predictions. Microstructure-sensitive modeling of high temperature creep behavior in HT9 cladding for SFR applications currently lack experimental data to model the phenomena accurately. To fill this need, methods to perform microstructural characterization have been developed and performed on HT9.

36 MATERIALS SCIENCE↗

Microstructure and phase evolution in the U-10Zr fuel investigated by in situ TEM heating experiments

The development of U-Zr metallic nuclear fuel for fast spectrum reactors is impacted by a lack of mechanistic understanding of the fuel behavior evolution under thermal irradiation conditions, despite previous works providing substantial fuel performance data. This work uses in-situ transmission electron microscopy heating experiments to study phase and microstructural evolution in several unirradiated U-10Zr specimens during rapid heating ramps (from room temperature to 1000 °C). The starting a-U + bcc-(Zr, U) eutectic microstructure began to decompose above 600 °C. The decomposition initiated from the bcc (U,Zr) phase. Similar results were observed for all specimens even when fabricated by different routes (e.g., cold rolled or annealed). As a result, the impact of observed microstructure and phase evolutions at high temperatures on fuel fabrication and in-pile fuel transient test was also discussed.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Microstructural characterization of the oxidation of nuclear graphite under chronic and accident conditions via XCT and synchrotron XCT

Graphite is a candidate material to moderate fast neutrons and for structural components in the US next-generation graphite-moderated reactors. A graphite core is conceived as a large formation of interconnected bricks that primarily serves as the moderator of fast neutrons, holds instrumentation, fuel elements, control rods, and is a receptacle for molten salts for Molten Salt Reactors (MSRs) designs. During the operation of a graphite-moderated power plant, graphite components might be subjected to chronic oxidation during normal operating conditions or aggressive oxidation as a result of accidental ingress of air that reacts vigorously with the graphite core. Using synchrotron, x-ray computed tomography (XCT), this research systematically characterized microstructural changes that accompanied these two oxidation scenarios. Chronic oxidation was studied by characterizing IG-110, PCEA, and NBG-18 specimens that were gradually oxidized in air at a low temperature (520°C). The accidental ingress of air into the graphite reactor was simulated by subjecting the grades mentioned above to high-temperature oxidation at approximately 750°C. This research is the first, in situ, systematic characterization of nuclear graphite microstructural evolution that can be associated with the two possible oxidation scenarios and provide insight into related repercussions. The results show that the microstructure and pore connectivity influence the rate of oxidation and evolution of the microstructure under the two oxidation regimes. These results are crucial to understanding which grades are more resilient to each type of oxidation and documenting the damage created in the graphite.

Arregui Mena, Jose'↗

HPC for Optimizing Process Parameters to Control Material Evolution in Seamless Induction Hardening of Wind Turbine Main Shaft Bearings

Work proposed in this project focused on understanding the effect of martensitic transformation in the steel on the potential for cracking during seamless induction hardening (SIH) as a function of process conditions to allow the process to optimally scale up. Large-scale, three-dimensional phase-field simulations of martensitic transformation were performed using MEUMAPPS-SS (Microstructure Evolution Using Massively Parallel Phase-field Simulations – Solid State) code developed at Oak Ridge National Laboratory. The simulations were guided by location-specific thermal history generated by experimental measurements of time-temperature history generated at The Timken Company. The simulations were able to capture the morphological evolution of the martensite variants in an Fe-1.0C-1.5Cr steel based on the Nishiyama-Wasserman (NW) orientation relationship. The simulations were also able to quantify the stress-state at the interface between impinging martensite variants. The simulations indicated that the magnitude of the various stress and strain components were dependent on the sizes of the impinging plates with a reduction in these quantities with reduced plate size in agreement with experimental findings. The results obtained from the simulations will be used to guide the optimization of the alloy thermal conditions to eliminate quench cracking during SIH of bearing steels.

99 GENERAL AND MISCELLANEOUS↗

Detailed Analysis of RUS Insertion Experiment and Scoping Studies for Performing Next Experiment using an Enriched Fuel Sample

Microstructure evolution due to irradiation in a nuclear reactor can have a dramatic effect on material properties. A better understanding of this evolution is necessary for developing improved nuclear fuels and materials. The ability to measure such changes in real time is extremely challenging due to high temperatures, high radiation fields, and limited access of the reactor environment. Through carefully designed experiments, measurement of elastic properties can be tied directly to microstructure. We present an instrument that has been developed to monitor in-pile changes in grain microstructure. The measurement approach involves optically exciting and detecting flexural waves in a thin cantilever beam. An instrument capsule based on this technique was fabricated and underwent an irradiation test in the TREAT reactor in May 2019. Analyses of the test results are presented in this report. Scoping studies on the expected impact of radiation on similar tests are also presented.

36 MATERIALS SCIENCE↗