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At least 91 records · Page 5

Microstructural characterization of limestone exposed to heat with XRD, SEM and TG-DSC

Highlights: • The microstructure of limestone (25 °C–800 °C) was analyzed by XRD, SEM and TG-DSC. • The microstructural properties of the crystal are anisotropic in different crystal plane directions. • Microstructure controls the macroscopic properties of limestone. - Abstract: Limestone is a common rock used in many buildings and found in underground engineering projects. After exposure to heat, for example, the occurrence of fires, the stability of limestone structures is mostly affected, which may have safety repercussions. Therefore, the impact of thermal effects on the microstructure of limestone is investigated in this study, in which 8 groups of limestone samples are exposed to different temperatures (25 °C, 100 °C, 200 °C, 300 °C, 500 °C, 600 °C, 700 °C and 800 °C), after which X-ray diffraction, differential scanning calorimetry and scanning electron microscopy are carried out. The mineral composition and the microstructure of the samples are numerically modeled, in which the diffraction peaks, full width at half maximum, integral breadth, microstrain, average domain size and dislocation density are analyzed. The macroscopic properties obtained from the results in other works in the literature including porosity, compressive strength, damage coefficients and modulus of elasticity are also compared with the parameters above. The changes in the crystal structure of two minerals, calcite and dolomite, are found to be anisotropic in the different crystal plane directions. It is also found that the limestone microstructure affects the macroscopic properties. A temperature between 200 °C to 300 °C is the critical temperature at which both the macroscopic properties and macrostructure demonstrate significant changes.

36 MATERIALS SCIENCE↗

Hot Straining and Quenching and Partitioning of a TRIP-Assisted Steel: Microstructural Characterization and Mechanical Properties

Advanced high strength steels (AHSS), with yield strengths over 300 MPa and tensile strengths exceeding 600 MPa, are becoming more noticeable in vehicle manufacturing. A novel processing route of a TRIP-assisted steel was developed. Characterization and modelling techniques were used to establish correlations between processing, microstructure and mechanical properties. Quenching and partitioning (Q&P) and a novel process of hot straining (HS) and Q&P (HSQ&P) treatments have been applied to a TRIP-assisted steel in a Gleeble ®3S50 thermo-mechanical simulator. The heat treatments involved intercritical annealing at 800 oC and a two-step Q&P heat treatment with a partitioning time of 100 s at 400 oC. The effects of high-temperature isothermal deformation on the carbon enrichment of austenite, carbide formation and the strain-induced transformation to ferrite (SIT) mechanism were investigated. Carbon partitioning from supersaturated martensite into austenite and carbide precipitation were confirmed by means of atom probe tomography (APT). Austenite carbon enrichment was clearly observed in all specimens, and in the HSQ&P samples it was slightly greater than in Q&P, suggesting an additional carbon partitioning to austenite from ferrite formed by the SIT phenomenon. By APT, the carbon accumulation at austenite/martensite interface was clearly observed. The newly developed combined process is promising as the transformation induced plasticity can contribute to the formability and energy absorption, contributing to fill the gap of the third generation of high-strength steels.

Ariza, Edwan Anderson↗

Microstructural Characterization of Pure Tin Produced by the Drop-on-Demand Technique of Liquid Metal Jetting

The microstructure–property relationship of a pure tin part built using the drop-on-demand technique of liquid metal jetting, a cost–effective alternative to selective laser-melting or sintering techniques, was determined. Here, the microstructure of the as-built tin is observed to have minimal stored strain, low dislocation density, few to no voids, and the presence of only the β-tin phase; concurrently, mechanical properties are shown to be identical to the traditionally manufactured tin.

36 MATERIALS SCIENCE↗

Microstructural characterization of sulfur-doped Bi{sub 2}Te{sub 3} crystals

In this study, the detailed microstructure of sulfur-doped Bi{sub 2}Te{sub 3} and the distribution of sulfur dopants were investigated using X-ray diffraction (XRD) and transmission electron microscopy (TEM). XRD result indicates that the interplanar distances of Bi{sub 2}Te{sub 3} are shortened after introducing sulfur dopants. HRTEM reveals that the unit cell lengths along [001, 100] are decreased as a result of the substitution of Te by smaller S atoms on the anion lattice. XRD and HRTEM analysis suggest that the distortion of the crystal lattice in Bi{sub 2}Te{sub 3} is induced by doping sulfur. High annular angler dark field scanning electron microscopy (HAADF-STEM) image shows obvious contrast variations in the Te atomic columns, indicating that Te sites were unevenly substituted by S dopants. Te columns with least contrast intensity correspond to the preferential occupation sites of S atoms. The replacement of Te atoms by S can be attributed to the evaporated sulfur powder in the gas reaction procedure. The present work is not only contributed to obtain a better understanding of the distribution of sulfur dopants introduced by gas reaction, but also can help explore the structural-property relationship of sulfur-doped Bi{sub 2}Te{sub 3}. - Highlights: • Sulfur-doped Bi{sub 2}Te{sub 3} was synthesized through modified Bridgeman method. • The introduction of S dopants results in shortening the lattice spacing of Bi{sub 2}Te{sub 3}. • HRTEM analysis indicates that S was doped through substituting Te atoms instead of incorporating interstitially. • HAADF-STEM analysis shows that Te columns with least intensity correspond to the preferential occupation sites of S.

36 MATERIALS SCIENCE↗

Microstructural Characterization of AGR-2 TRISO-coated Particle Buffer, IPyC, and Buffer-IPyC Interfaces

Investigating the microstructural, mechanical, and chemical behaviors of Tristructural Isotropic (TRISO) fuel particles is vital for its qualification and use in advanced reactors. Central to the study of TRISO particles is understanding the silicon carbide (SiC) layer's ability to confine fission products, with failure mechanisms linked to chemical degradation following mechanical degradation of the buffer and IPyC layers. Research has been done to quantify the micro-tensile properties of the buffer, inner pyrolytic carbon (IPyC), and buffer-IPyC interlayer regions and their interactions within both irradiated and un-irradiated TRISO particles. Techniques such as atom probe tomography (APT) and transmission electron microscopy (TEM) have also been deployed to examine microstructural defects and fission product distribution in detail. The goal is to understand layer delamination, establish connections between microstructure and mechanical attributes, and inform computational predictions of fuel performance. This work may help refine predictive models of TRISO fuel behavior and facilitating its certification for use in advanced reactors.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Microstructural Characterizations of Two High Fluence Baffle-Former Bolts Retrieved from a Westinghouse Two-loop Downflow Type PWR

As one of the pressurized water reactor (PWR) internal components, baffle-former bolts (BFBs) are subjected to significant mechanical stress and neutron irradiation from the reactor core during the plant operation. Over the long operation period, these conditions lead to potential degradation and reduced load-carrying capacity of the bolts. In support of evaluating long-term operational performance of materials used in core internal components, the Oak Ridge National Laboratory (ORNL), through the Department of Energy (DOE), Office of Nuclear Energy, Light Water Reactor Sustainability (LWRS) Program, Materials Research Pathway (MRP), has harvested two high fluence BFBs from a commercial Westinghouse two-loop downflow type PWR. The two bolts of interest, i.e. bolts # 4412 and 4416, were withdrawn from service in 2011 as part of a preventative replacement plan. No identification of cracking or potential damage was found for these bolts during their removal in 2011. However, the bolts required a lower torque for removal from the baffle structure than the original torque specified during installation. Irradiation damage levels in the bolts range from 15 to 41 displacements per atom. The goal of this project is to perform detailed microstructural and mechanical property characterization of BFBs following in-service exposures. The information from these bolts will be integral to the LWRS program initiatives in evaluating end of life microstructure and properties. Furthermore, valuable data will be obtained that can be incorporated into model predictions of long term irradiation behavior and compared to results obtained from experimental reactor conditions

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

3D Microstructural Characterization of Uranium Oxide as a Surrogate Nuclear Fuel: Effect of Oxygen Stoichiometry on Grain Boundary Distributions

The initial microstructure of an oxide fuel can play a key role in its performance. At low burn-ups, the diffusion of fission products can depend strongly on grain size and grain boundary (GB) characteristics, which in turn depend on processing conditions and oxygen stoichiometry. Serial sectioning techniques using Focused Ion Beam were developed to obtain Electron Backscatter Diffraction (EBSD) data for depleted UO2 pellets that were processed to obtain 3 different oxygen stoichiometries. The EBSD data were used to create 3D microstructure reconstructions and to gather statistical information on the grain and GB crystallography, with emphasis on identifying the character (twist, tilt, mixed) for GBs that meet the Coincident Site Lattice (CSL) criterion as well as GBs with the most common misorientation angles. Data on dihedral angles at triple points were also collected. The results were compared across different samples to understand effects of oxygen content on microstructure evolution.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Microstructural Characterization of Irradiated U0.7ZrH1.6 Using Ultrasonic Techniques

In recent years, there has been an increased level of effort to understand the changes in microstructure that occur due to irradiation of nuclear fuel. The primary driver for this increased effort is the potential for designing new fuels that are safer and more reliable, in turn enabling new and improved reactor technologies. Much of the data on microstructural change in irradiated fuels is generated through a host of post irradiation examination techniques such as optical microscopy (OM), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) to determine grain structure, porosity, crack geometry, etc. in irradiated fuels. Such “traditional” examination techniques were recently used to characterize a novel new fuel consisting of U0.17ZrH1.6 pellets bonded to zircaloy-2 cladded with lead-bismuth eutectic before and after irradiation. However, alternative methods such as ultrasonic inspection can provide an opportunity for nondestructively assessing microstructure in both in-pile and post-irradiation examinations. In this paper, we briefly describe initial results of ultrasonic examination of the U0.17ZrH1.6 pellets (unirradiated and irradiated), in a post-irradiation examination study. Data indicate some correlation with microstructural changes due to irradiation; however, it is not clear what the specific microstructural changes are that are influencing the ultrasonic measurements. Interestingly, specimens with nominally identical burnup show differences in ultrasonic signatures, indicating apparent microstructural differences between these specimens. A summary of the experimental study, preliminary data and findings are presented in this short paper. Additional details of the analysis will be included in the presentation.

Microstructure evaluation↗

An Integrated High-Speed Microstructural Characterization Method Using Simultaneous XRD, Stereo-DIC, and PCI

High-speed characterization of the deformation mechanisms in polycrystalline metals requires the quantification of full strain fields and local microstructural evolutions simultaneously. In this paper, we present a novel experimental method to integrate phase-contrast imaging (PCI), stereographic digital image correlation (stereo-DIC), and full-ring X-ray diffraction (XRD) to allow for the simultaneous characterization of polycrystalline metals at 1MHz or higher. A Kolsky bar was integrated into the synchrotron X-ray source in Sector 32 ID-B at the Advance Photon Source (APS) at Argonne National Laboratory. When the sample is dynamically loaded, the diagnostic methods of full-ring XRD, PCI, and stereo-DIC are properly synchronized to record the deformation behavior at both continuum and microstructural scales as a function of the loading history. An advanced high-strength steel (AHSS) is used as a model material to demonstrate the capabilities of this new experimental method.

36 MATERIALS SCIENCE↗

Microstructural Characterization of Enhanced Conductivity Aluminum Alloys (Abstract)

In this project, Pacific Northwest National Laboratory (PNNL) will perform multimodal imaging to determine the microstructural features of enhanced conductivity aluminum alloys manufactured by NanoAL LLC. In particular, we will perform imaging to identify the basis of the strengthening mechanisms in the custom AA6X alloys provided by NanoAL LLC. These activities will be performed as part of a voucher service provided by the PNNL for the CABLE Manufacturing Prize stewarded by DOE Advanced Manufacturing Office. This 6-month effort will be executed predominantly at PNNL with a budget of $50,000.

36 MATERIALS SCIENCE↗

Microstructural Characterization and Electrochemical Behavior of AA2014 Al-Cu-Mg-Si Alloy of Various Tempers

AA2014 Al-Cu-Mg-Si alloy is subjected to aging heat treatment, and microstructural features and electrochemical behavior of the AA2014 Al-Cu-Mg-Si alloy of various tempers have been characterized. Hardness measurement of the alloy of different tempers showed typical age hardening behavior. X-ray diffraction and transmission electron microscopy studies revealed the presence of characteristic phases. Differential scanning calorimetry study displayed the sequence of solid-state precipitation and dissolution reactions in the AA2014 alloy of various tempers. Electrochemical behavior was assessed by measurement of variation of open-circuit voltage with time, potentiodynamic polarization and potentiodynamic cyclic polarization of the AA2014 alloy of various tempers in 3.5 wt.% NaCl solution at near neural (pH ~ 7) and at alkaline (pH 12) conditions. Potentiodynamic polarization studies of different tempers in 3.5 wt.% NaCl solution at pH ~ 7 showed that the corrosion potential (E{sub corr}) value has shifted toward more negative (active) direction with increasing aging time. The cyclic polarization in 3.5 wt.% NaCl solution at pH ~ 7 displayed active–passive behavior and also showed a large hysteresis loop indicating high pit growth damage.

36 MATERIALS SCIENCE↗

Microstructural Characterization, Mechanical Properties, and Corrosion Resistance of Dental Co-Cr-Mo-W Alloys Manufactured by Selective Laser Melting

In this paper, the microstructure, mechanical properties, and corrosion resistance of the dental Co-Cr-Mo-W alloys fabricated by selective laser melting (SLM) were systematically investigated and correlated. The microstructure of the SLM group (SG) specimens is composed of extremely fine columnar crystals, exhibiting supersaturated and homogeneous character. The matrix mainly consists of face-centered-cubic (FCC) cobalt solid solutions, and minimal hexagonal-close-packed (HCP) cobalt solid solutions. Mechanical test results showed that the 0.2% yield strength of SG was 775 ± 7 MPa, and the ultimate tensile strength was 1118 ± 25 MPa. The elongation of SG was 8.28 ± 0.4%, and the microhardness of SG was 476 ± 10 HV. All of these values largely exceeded the cast group (CG) specimens. The high strength is attributed to their fine columnar crystals and supersaturated matrices. The fewer content from the HCP phase and a lack of intermetallic compounds or eutectic contribute to the high ductility. Furthermore, a higher E{sub corr}, lower I{sub corr} were acquired for better corrosion resistance compared to cast specimens, due to even less composition segregation and more microstructural homogeneity.

36 MATERIALS SCIENCE↗

High-Throughput Ion Irradiation and Microstructural Characterization of Multi-Principal-Element Alloys

Multi-principal-element alloys (MPEAs) have garnered interest in the nuclear community for their apparent resistance to microstructural damage under irradiation. While both experimentation and simulation have demonstrated reduced hardening and void swelling in MPEAs, the relationship between composition and irradiation response is still poorly understood since a rich experimental database for MPEAs does not yet exist. In this work, to accelerate the generation of experimental irradiation-response data for MPEAs, high-throughput synthesis, irradiation, and characterization techniques have been employed. Specifically, additive manufacturing has been used to produce arrays of various MPEAs (1-cm2 coupons), which have been subsequently irradiated using 4-MeV Ni2+ ions to a peak damage of 200 dpa at 500 °C. Hardening and void swelling have been assessed using nanoindentation and trenching via plasma focused ion beam (PFIB), respectively. Trends in the experimental data relating hardening and void swelling behavior to composition have been analyzed using different machine learning approaches.

36 MATERIALS SCIENCE↗

Microstructural characterization of weld joints of 9Cr reduced activation ferritic martensitic steel fabricated by different joining methods

This paper presents a detailed electron microscopy study on the microstructure of various regions of weldment fabricated by three welding methods namely tungsten inert gas welding, electron beam welding and laser beam welding in an indigenously developed 9Cr reduced activation ferritic/martensitic steel. Electron back scatter diffraction studies showed a random micro-texture in all the three welds. Microstructural changes during thermal exposures were studied and corroborated with hardness and optimized conditions for the post weld heat treatment have been identified for this steel. Hollomon–Jaffe parameter has been used to estimate the extent of tempering. The activation energy for the tempering process has been evaluated and found to be corresponding to interstitial diffusion of carbon in ferrite matrix. The type and microchemistry of secondary phases in different regions of the weldment have been identified by analytical transmission electron microscopy. - Highlights: • Comparison of microstructural parameters in TIG, electron beam and laser welds of RAFM steel • EBSD studies to illustrate the absence of preferred orientation and identification of prior austenite grain size using phase identification map • Optimization of PWHT conditions for indigenous RAFM steel • Study of kinetics of tempering and estimation of apparent activation energy of the process.

36 MATERIALS SCIENCE↗

Microstructural characterization of Charpy-impact-tested nanostructured bainite

In this work, a possible cause of the extraordinary low impact toughness of nanostructured bainite has been investigated. The microstructure of nanostructured bainite consisted chiefly of carbide-free bainitic ferrite with retained austenite films. X-ray diffractometry (XRD) measurement indicated that no retained austenite existed in the fractured surface of the Charpy-impact-tested specimens. Fractographs showed that cracks propagated mainly along bainitic ferrite platelet boundaries. The change in microstructure after impact loading was verified by transmission electron microscopy (TEM) observations, confirming that retained austenite was completely transformed to strain-induced martensite during the Charpy impact test. However, the zone affected by strained-induced martensite was found to be extremely shallow, only to a depth of several micrometers from the fracture surface. It is appropriately concluded that upon impact, as the crack forms and propagates, strain-induced martensitic transformation immediately occurs ahead of the advancing crack tip. The successive martensitic transformation profoundly facilitates the crack propagation, resulting in the extremely low impact toughness of nanostructured bainite. Retained austenite, in contrast to its well-known beneficial role, has a deteriorating effect on toughness during the course of Charpy impact. - Highlights: • The microstructure of nanostructured bainite consisted of nano-sized bainitic ferrite subunits with retained austenite films. • Special sample preparations for SEM, XRD and TEM were made, and the strain-affected structures have been explored. • Retained austenite films were found to transform into martensite after impact loading, as evidenced by XRD and TEM results. • The zone of strain-induced martensite was found to extend to only several micrometers from the fracture surface. • The poor Charpy impact toughness is associated with the fracture of martensite at a high strain rate during impact loading.

36 MATERIALS SCIENCE↗

Microstructure Characterization and Modeling for Improved Electrode Design

This presentation describes research work led by NREL with team members from Argonne National Laboratory and Texas A&M University in microstructure analysis, modeling and validation under DOE's Computer-Aided Engineering of Batteries (CAEBAT) program. The goal of the project is to close the gaps between CAEBAT models and materials research by creating predictive models that can be used for electrode design.

33 ADVANCED PROPULSION SYSTEMS↗

Microstructure characterization of SiC nanowires as reinforcements in composites

SiC nanowires have been rarely investigated or explored along their axial direction by transmission electron microscopy (TEM). Here we report the investigation of the cross-section microstructure of SiC nanowires by embedding them into Al matrix. Morphology of SiC nanowires was cylindrical with smooth surface or bamboo shape. Cubic (3C-SiC) and hexagonal structure (2H-SiC) phases were detected by X-ray diffraction (XRD) analysis. High density stacking faults were observed in both the cylindrical and bamboo shaped nanowires which were perpendicular to their axial direction. Selected area electron diffraction (SAED) patterns of the cylindrical and bamboo shaped SiC nanowires both in the perpendicular and parallel direction to the axial direction were equivalent in the structure. After calculation and remodeling, it has been found that the SAED patterns were composed of two sets of diffraction patterns, corresponding to 2H-SiC and 3C-SiC, respectively. Therefore, it could be concluded that the SiC nanowires are composed of a large number of small fragments that are formed by hybrid 3C-SiC and 2H-SiC structures. - Graphical abstract: Display Omitted - Highlights: • Cross-section microstructure of SiC nanowires was observed in Al composite. • Cylindrical with smooth surface or bamboo shape SiC nanowires were found. • The cylindrical and bamboo shaped SiC nanowires were equivalent in structure. • Structure of SiC nanowires was remodeled. • SiC nanowires are composed of hybrid 3C-SiC and 2H-SiC structures.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Microstructural characterization of nuclear graphite: from the microscale to the nanoscale

Multiple reactor designs use graphite as a moderator of the nuclear reactions and as structural support. During the lifetime of the reactor, multiple aging factors such as neutron irradiation, oxidation, and temperature along with others induce changes in the microstructure and crystal lattice of graphite components. The pore morphology and crystal structure of some phases in graphite can be used to trace the evolution of irradiation defects and mechanical properties of graphite. We present a combination of results from several microscopy techniques to investigate the differences between nuclear graphite grades and the effects of neutron irradiation and oxidation at multiple length scales. This multiscale approach is needed to understand the microstructural variations caused by the raw materials and manufacturing processes as well as how the different phases of graphite are affected by the reactor environment. The results provide insight into the oxidation- and radiation-induced changes of graphite and create a robust baseline of microstructure information that can be used for the selection of materials for the next generation of nuclear power stations. Moreover, the experiments conducted in this work provide an overview of the advantages and limitations of the most common techniques used to characterize nuclear graphite and how these techniques might be applied to study other carbon-based materials used in the nuclear industry.

Arregui Mena, Jose'↗