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At least 91 records · Page 5

New Structural Insight into Interface-Controlled α–σ Phase Transformation in Fe-Cr Alloys

Synchrotron Laue microdiffraction scanning is used for the ex situ study of the body-centered, cubic-to-tetragonal phase transformation that occurs in equiatomic polycrystalline Fe-Cr alloys at temperatures between 550 and 800 °C. Grain orientation and grain strains were scanned with a micron step resolution after annealing at 700 °C for 12 h. Further microstructural details on the early stage of the transformation, and more particularly on the cubic-to-tetragonal phase interface, were achieved. Only the α and ordered σ phases were detected. The crystallographic relationships at the interface between the two phases did not follow the predicted rules; this result is discussed in relation to the measured microstrains.

36 MATERIALS SCIENCE↗

BERT Non-Destructively Probes the Microstructure of Dissimilar Welds [Poster]

Energy-resolved neutron imaging (ERNI) utilizes contrast provided by diffraction. Microstructure with >100µm grains as in cast, annealed or welded materials is difficult to characterize by X-ray or electron-based methods $\Rightarrow$ Well-suited for neutron Bragg-edge radiography. BERT was applied to dissimilar welds of Inconel on steel produced by additive manufacturing. Viewing the sample at time-of-flight/energy/wavelength where a single grain orientation dominates the attenuation allows to map grain orientations. Similarly to electron-backscatter diffraction (EBSD) but on cm length scales and through-thickness. Combined with texture measurements on the HIPPO instrument, identifying major grain orientations, 2D and 3D grain orientation maps are feasible. Results can guide development of thermo-mechanical treatment avoiding or introducing such microstructures, characterize dissimilar welds, interpretation of acoustic signals for quality control, guide destructive examination with X-rays/electrons, or provide data for codes predicting such microstructures.

36 MATERIALS SCIENCE↗

Microstructure and texture evolution of deformed Mg-Zn alloy during recrystallization

Highlights: • The texture intensity in the Mg-Zn alloy relied on the microstructure. • Fine DRXed grains showed a fiber texture distributing between <10.0> and <11.0>. • Coarse DRXed grains mainly exhibited <11.0> fiber texture. • The preferred growth of <11.0> oriented grains resulted in texture evolution. - Abstract: The microstructure and texture evolution of Mg-Zn alloy during recrystallization was investigated by EBSD in the present study. Deformed region, fine DRXed region and coarse DRXed region were obtained in Mg-Zn alloy during deformation. It was found that the texture intensity in DRXed region was weaker compared with the deformed region. The second phase at grain boundaries resulted in the formation of fine DRXed grains with weaker texture compared with the coarse DRXed region. Additionally, a remarkable grain-size driven textural transition from <10.0>–<11.0> texture to <11.0> texture were detected with the growth of DRXed grains. The recrystallized grains with small grain size showed a fiber texture distributing homogeneously between <10.0> and <11.0>, while <11.0> fiber texture was predominant for the large recrystallized grains. It is suggested that <11.0> oriented grains grew faster than other oriented grains, which was ascribed to larger misorientation between <11.0> oriented grains and their neighboring grains.

36 MATERIALS SCIENCE↗

Experimental study of microstructure changes due to low cycle fatigue of a steel nanocrystallised by Surface Mechanical Attrition Treatment (SMAT)

Electron Backscatter Diffraction technique is used to characterize the microstructure of 316L steel generated by Surface Mechanical Attrition Treatment (SMAT) before and after low cycle fatigue tests. A grain size gradient is generated from the top surface to the interior of the samples after SMAT so that three main regions can be distinguished below the treated surface: (i) the ultra-fine grain area within 5 μm under the top surface with preferably oriented grains, (ii) the intermediate area where the original grains are partially transformed, and (iii) the edge periphery area where the original grains are just mechanically deformed with the presence of plastic slips. Fatigue tests show that cyclic loading does not change the grain orientation spread and does not activate any plastic slip in the ultra-fine grain top surface area induced by SMAT. On the opposite, in the plastically SMAT affected region including the intermediate area and the edge periphery area, new slip systems are activated by low cycle fatigue while the grain orientation spread is increased. These results represent a first very interesting step towards the characterization and understanding of mechanical mechanisms involved during the fatigue of a grain size gradient material. - Highlights: •LCF tests are carried out on specimens processed by SMAT. •EBSD is used to investigate microstructural changes induced by LCF. •A grain size gradient is generated by SMAT from surface to the bulk of the fatigue samples. •New slip systems are activated by LCF and GOS is increased in plastically deformed region. •However, these phenomena are not observed in the top surface ultra-fine grain area.

36 MATERIALS SCIENCE↗

CosTuuM: Polarized Thermal Dust Emission by Magnetically Oriented Spheroidal Grains

We present the new open-source C++-based Python library CosTuuM that can be used to generate infrared absorption and emission coefficients for arbitrary mixtures of spheroidal dust grains that are (partially) aligned with a magnetic field. We outline the algorithms underlying the software, demonstrate the accuracy of our results using benchmarks from literature, and use our tool to investigate some commonly used approximative recipes. We find that the linear polarization fraction for a partially aligned dust grain mixture can be accurately represented by an appropriate linear combination of perfectly aligned grains and grains that are randomly oriented, but that the commonly used picket fence alignment breaks down for short wavelengths. We also find that for a fixed dust grain size, the absorption coefficients and linear polarization fraction for a realistic mixture of grains with various shapes cannot both be accurately represented by a single representative grain with a fixed shape, but that instead an average over an appropriate shape distribution should be used. Insufficient knowledge of an appropriate shape distribution is the main obstacle in obtaining accurate optical properties. CosTuuM is available as a standalone Python library and can be used to generate optical properties to be used in radiative transfer applications.

79 ASTRONOMY AND ASTROPHYSICS↗

Isothermal annealing behaviour of nuclear grade 20Cr-25Ni austenitic stainless steel

Highlights: • At 930 °C recrystallisation of deformed 20/25 Nb steel is completed after 120 s. • Recrystallisation proceeds by strain induced boundary migration. • An increase of cube oriented grains at the expense of S oriented is observed. • The boundary migration induced the precipitation of niobium carbides. • The grain size is limited by the particle dispersion according to Zener pinning. - Abstract: We have performed an in-depth characterisation of the microstructure evolution of 20Cr-25Ni Nb-stabilised austenitic stainless steel during isothermal annealing at 930 °C using scanning and transmission electron microscopy. This steel grade is used as cladding material in advanced gas-cooled fission reactors, due to its resistance to thermal creep and water corrosion. The initial deformed microstructure undergoes recrystallisation via a strain-induced boundary migration mechanism, attaining a fully recrystallised microstructure after 120 s of annealing. The transition from low-to-high grain boundaries has already occurred after 15 s, together with an increase in the cube grain orientation at the expense of the S texture component. After 120 s, the grain boundary migration induces the formation of new fine Nb(C,N) particles, whereas the pre-existing particles become enriched in Ni and Si. The resulting particle population limits the grain growth in the austenitic matrix, based on the Zener pinning model, resulting in relatively small recrystallised austenite grains and a high density of high-angle and special coincidence-lattice-site grain boundaries, together with a large number of particle/matrix interfaces.

36 MATERIALS SCIENCE↗

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↗

Investigation of deformation mechanisms in an advanced FeCrAl alloy using in-situ SEM-EBSD testing

The deformation mechanisms associated with uniaxial tensile testing are observed by conducting tensile experiments of an FeCrAl alloy using scanning electron microscopy (SEM) coupled with electron backscattered diffraction (EBSD). Prior to the deformation, investigated alloy was consisting grain and precipitate size of ~63.0 μm and ~6.7 μm, respectively. The recorded SEM micrographs and EBSD data at increasing levels of strains revealed the complex phenomena of slip bands’ formation in the presence of surface grain morphology evolution and their (001), (110) and (111) crystallographic planes distortions. The grains with orientation (110)||tensile direction (TD) shows higher shape change; however, (001)||TD and (111)||TD oriented grains show higher lattice gradient formation. Extracted information from the EBSD indicates that the crystallographic rotations drive towards specific, fiber-like texture in relation to the loading direction. Postmortem analysis of the recorded microstructure during the tensile deformation explains the phenomena of crack formation in the hard-intermetallic particles before the ultimate tensile strength (UTS). However, after the UTS, pores were identified in the neck that resulted from extensive plastic deformation. In-depth analysis was carried out to identify the cause of cracks and pores formation phenomena during the tensile test.

36 MATERIALS SCIENCE↗

Phase-field framework with constraints and its applications to ductile fracture in polycrystals and fatigue

Abstract Modeling of ductile fracture in polycrystalline structures is challenging, since it requires integrated modeling of cracks, crystal plasticity, and grains. Here we extend the typical phase-field framework to the situations with constraints on the order parameters, and formulate two types of phase-field models on ductile fracture. The Type-I model incorporates three sets of order parameters, which describe the distributions of cracks, plastic strain, and grains, respectively. Crystal plasticity is employed within grain interiors accommodated by J 2 plasticity at grain boundaries. The applications of the Type-I model to single crystals and bicrystals demonstrate the influences of grain orientations and grain boundaries on crack growth. In the Type-II model, J 2 plasticity is assumed for the whole system and grain structures are neglected. Taking advantage of the efficiency of the fast Fourier transform, our Type-II model is employed to study low cycle fatigue. Crack closure and striation-like patterning of plastic strain are observed in the simulations. Crack growth rate is analyzed as a function of the J -integral, and the simulated fatigue life as a function of plastic strain agrees with the Coffin–Manson relation without a priori assumption.

36 MATERIALS SCIENCE↗

PIND: High spatial resolution by pinhole neutron diffraction

Here, a pinhole neutron diffraction (PIND) technique was developed to enable improving the spatial resolution down to 250 μm. Instead of the conventional engineering diffraction method which integrates all the diffraction signals on the detector plane, the PIND setup utilizes the diffraction pattern of each pixel on 2D detectors. The proposed PIND arrangement enables improving the spatial resolution of time-of-flight instruments and allows solving problems involving steep gradients of strain or texture. The phase content and preferential orientation of grains inside samples can be spatially resolved in 2D/3D. Further, PIND retains the capability of in-situ non-destructive neutron diffraction mapping of lattice strain and grain orientation under external stimuli such as temperature and force.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

NSUF Report EBSD analyses on metallic fuel samples: Tips and improvements in sample preparation

EBSD (Electron Backscatter Diffraction) is an analytic technique used to evaluate the microstructure of a specimen. It can be used to evaluate interesting crystallographic data ranging from grains size to grain orientation, from grain boundaries to stresses. Moreover, in the field of nuclear materials EBSD can aid in estimating properties important for reactor performance, such as dislocation and residual strain [1]. EBSD patterns are generated by focusing a stationary electron gun on the specimen and detecting the backscatter electrons that satisfy Bragg conditions, and thus are diffracted by the crystal planes forming the so called Kikuchi bands. These bands correspond to each of the lattice diffracting crystal planes and are detected on a phosphor screen via a low-light CCD camera [2]. The patterns are generated within a small interaction volume located at a depth of less than 50-100 nm. Because of this, the data quality is extremely sensitive to the integrity of the crystallographic lattice order at the surface of the sample and thus to sample preparation and to oxidation [3]. While conventional sample preparation methods are widely used in materials science, they often do not lead to quality electron backscatter patterns needed for the characterization of nuclear materials [4]. This has been related by many authors to the challenges associated with handling radiological specimens, their rapid oxidation, and artifacts in such samples (e.g. high number of defects, precipitates and/or porosities) [4-8]. EBSD, however, can be an invaluable technique to evaluate microstructural evolution during fabrication and after irradiation at the required mesoscale for model and simulation. It also provides important information on grain structure necessary to understand irradiation effect, such as grain subdivision. Thus, it is of paramount importance to further the application of this technique to nuclear materials and especially irradiated fuels.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Graphite Characterization: Baseline Variability Analysis Report

The Idaho National INL’s Baseline Material Property program provides many measurements of different material properties on a variety of nuclear graphite grades being investigated for irradiation-induced changes in material properties. The baseline material properties provide an unirradiated reference for comparison with measurements of those properties after irradiation. This study describes how uncertainty, or variance, in estimates of important material properties, like compressive strength, may depend on sample size, sample distribution and parameter estimation methods. Compressive strength data from two large collections of specimens from a billet of PCEA graphite (sample size = 230) and a billet of IG-110 graphite (sample size = 48) are used to illustrate these dependencies. The grades of graphite used represent approximate end members in terms of relative variability in strength measurements. Monte Carlo simulation and bootstrapping methods were used to examine variance in Weibull-parameter estimates as a function of sample size. Results were consistent with what previous statistical analyses have shown about the relationship between sample size and width of the confidence interval for maximum likelihood (ML) estimated parameters when samples are repeatedly drawn from a Weibull distribution. As a function of sample size, the precision of the modulus estimate increases faster than that of the characteristic strength. The modulus maximum likelihood estimates (MLEs) are biased for low sample sizes. The American Society for Testing and Materials document ASTM D7846-16 provides equations that describe the dependence of the variance of parameter MLEs on sample size. Using the same methodology, we show that the polynomials provided for variance dependence on sample size are inaccurate for sample sizes greater than ~120. We provide approximations to that relationship that illustrate relative constancy for sample size > ~10, in the logspace relationship of the modulus variance and the log transformed characteristic strength variance. Bootstrapping provided a means of comparing Weibull parameters obtained using ASME’s guidance for specimen collection to those obtained using different weighting in a case where strength is related to position in a billet and to grain orientation and a single distribution is used to characterize the billet. ASME specifies that samples be collected with equal representation in all locations and grain orientations. Parameter values obtained using ASME’s method were different from those obtained using random sampling of the complete data sets, and this was particularly true for the PCEA data. In addition, while the ASME approach yielded more conservative parameters for the PCEA data, the opposite was true for the IG-110 data. The difference observed for the PCEA data set likely reflects the larger number of against-grain specimens collected, which had generally higher strength than the with-grain specimens. This emphasizes the importance of the dependence of strength on location or grain orientation and suggests that it may be prudent to weight specimen collection toward the weaker subgroups if a conservative estimate as desired, as the equal weighting method recommended by ASME would will not always provide the most conservative Weibull parameters. Because spatial correlations commonly exist in certain grades of graphite, future work may involve developing a methodology for parameter inference that relaxes the assumption of independent specimens. ASTM and ASME codes recommend different parameter estimation methods and models of the Weibull distribution in different situations. Descriptions of the effects on parameter estimates for the example billets used in this study provide an example of how the method may affect the parameter estimate, and how—in this case—that compares to differences due to other factors, such as sample size and dependence on grain orientation or sample location.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Micromechanical Behavior of Solid-Solution-Strengthened Mg-1wt.%Al Alloy Investigated by In-Situ Neutron Diffraction

In-situ neutron-diffraction experiments were employed to investigate the micromechanical behavior of solid-solution-strengthened Mg-1wt.%Al alloy. Two starting textures were used: 1) as-extruded then solutionized texture, T1, in which the basal poles of most grains are tilted around 70~85 from the extrusion axis, and 2) a reoriented texture, T2, in which the basal poles of most grains are tilted around 10~20 from the extrusion axis. Lattice strains and diffraction peak intensity variations were measured in situ during loading-unloading cycles in uniaxial tension. Twinning activities and stress states for various grain orientations were revealed. The results show that the soft grain orientations, favorably oriented for either extension twinning or basal slip, exhibit the stress relaxation, resulting in the compressive residual strain after unloading. On the other hand, the hard grain orientations, unfavorably oriented for both extension twinning and basal slip, carry more applied load, leading to much higher lattice strains during loading followed by tensile residual strains upon unloading.

Lee, Sooyeol↗

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↗

In-situ synchrotron micro-diffraction study of surface, interface, grain structure, and strain/stress evolution during Sn whisker/hillock formation

We have performed X-ray synchrotron micro-diffraction measurements to study the processes controlling the formation of hillocks and whiskers in Sn layers on Cu. The studies were done in real-time on Sn layers that were electro-deposited immediately before the X-ray measurements were started. This enabled a region of the sample to be monitored from the as-deposited state until after a hillock feature formed. In addition to measuring the grain orientation and deviatoric strain (via Laue diffraction), the X-ray fluorescence was monitored to quantify the evolution of the Sn surface morphology and the formation of intermetallic compound (IMC) at the Sn-Cu interface. The results capture the simultaneous growth of the feature and the corresponding film stress, grain orientation, and IMC formation. The observations are compared with proposed mechanisms for whisker/hillock growth and nucleation.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Organic solvent vapor sensitive methylammonium lead trihalide film formation for efficient hybrid perovskite solar cells

In this study, the anisotropic electronic properties of the perovskite crystals originating from their non-cubic crystal structures can potentially give rise to the grain orientation correlated photovoltaic device performance. Here we report that an organic solvent vapor atmosphere introduced during the spin-coating and formation of perovskite films changes the orientation and size of perovskite grains. It was found that slightly larger but much more oriented methylammonium lead trihalide (CH 3 NH 3 PbI 3 ) grains could be obtained under 1,2-dichlorobenzene (DCB) and dimethyl sulfoxide (DMSO) vapor atmospheres. The devices with more oriented grains outperformed regular devices with more random grains by a 50 mV larger open circuit voltage as well as a slightly increased fill factor. The device efficiency enhancement can be attributed to the longer charge recombination lifetime resulting from the reduced trap density and oriented grains. This result is important in providing guidelines for comparing the results from various groups because organic solvent vapors are generally present in a sealed glovebox for perovskite solar cell fabrication.

14 SOLAR ENERGY↗

Development of crystallographic-orientation-dependent internal strains around a fatigue-crack tip during overloading and underloading

In-situ neutron diffraction was employed to directly measure the crystallographic-orientation-dependent (i.e. hkl) internal strains as a function of distance from the crack tip on the pre-cracked Hastelloy C-2000 compact-tension specimen. Both in-plane (IP) and through-thickness (TT) strain evolutions for various grain orientations were examined during tensile overloading and compressive underloading cycles. After overloading, underloading and their combination loadings were applied and unloaded, the significantly different (hkl) residual strain profiles were obtained in the vicinity of the crack tip. The load responses of the (200) grain orientation in both the IP and TT directions were more significant than those of any other orientations. It is suggested that the different orientation-dependent strain distributions around the crack tip are caused by the combined effects of elastic and plastic anisotropy of each (hkl) reflection upon loading and the subsequent development of residual stresses generated near the crack tip during unloading as a result of the plastic deformation. - Highlights: ► (hkl) strains are examined in situ using neutron diffraction. ► Distinct strain responses are developed around the crack tip under loading. ► The strain response of the (200) grain orientation is more significant. ► Possible mechanisms for the orientation-dependent strain responses are provided.

36 MATERIALS SCIENCE↗

Electron microscopy of an aluminum layer grown on the vicinal surface of a gallium arsenide substrate

A thin Al layer grown by molecular-beam epitaxy on a misoriented GaAs (100) substrate is studied by transmission electron microscopy. Electron diffraction data and bright-field, dark-field, and high-resolution images show that, in the layer, there are Al grains of three types of crystallographic orientation: Al (100), Al (110), and Al (110)R. The specific structural features of the interfaces between the differently oriented grains and substrate are studied by digital processing of the high-resolution images. From quantitative analysis of the dark-field images, the relative content and sizes of the differently oriented grains are determined. It is found that atomic steps at the substrate surface cause an increase in the fraction and sizes of Al (110)R grains and a decrease in the fraction of Al (100) grains, compared to the corresponding fractions and sizes in the layer grown on a singular substrate surface.

36 MATERIALS SCIENCE↗